SI 40
Parts 136 to 149
Revised as of July 1,2004
Protection of Environment
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PV.
40
Parts 136 to 149
Revised as of July 1, 2004
Protection of
Environment
Containing a codification of documents
of general applicability and future effect
As of July 1, 2004
With Ancillaries
Published by
Office of the Federal Register
National Archives and Records
Administration
A Special Edition of the Federal Register
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Table of Contents
Page
Explanation v
Title 40:
Chapter I—Environmental Protection Agency (Continued) 3
Finding- Aids:
Material Approved for Incorporation by Reference 845
Table of CPB Titles and Chapters 867
Alphabetical List of Agencies Appearing in the CFR 885
List of CFR Sections Affected 895
111
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Cite this Code: CFR
To cite the regulations in
this volume use title,
part and section num-
ber. Thus, 40 CFR 136.1
refers to title 40, part
136, section 1.
iv
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Explanation
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REPUBLICATION OF MATERIAL
vi
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RAYMOND A. MOSLEY,
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July 1, 2004.
Vll
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THIS TITLE
Title 40—PROTECTION OF ENVIRONMENT is composed of thirty volumes. The parts
in these volumes are arranged in the following order: parts 1-49, parts 50-51, part
52 (52,01-52,1018), part 52 (52.1019-End), parts 53-59, part 60 (60.1-End), part 60 (Ap-
pendices), parts 61-62, part 63 (63.1-63.599), part 63 (63.600-1-63.1199), part 63 (63.1200-
63.1439), part 63 (63.1440-63.8830), part 63 (63.8980-End) parts 64-71, parts 72-80, parts
81-85, part 86 (86.1-86.59i-99) part 86 (86.600-1-End), parts 87-99, parts 100-135, parts
136-149, parts 150-189, parts 190-259, parts 260-265, parts 266-299, parts 300-399, parts
400-424, parts 425-699, parts 700-789, and part 790 to End. The contents of these
volumes represent all current regulations codified under this title of the CPE
as of July 1, 2004.
Chapter I—Environmental Protection Agency appears in all thirty volumes.
An alphabetical Listing of Pesticide Chemicals Index appears in parts 150-189.
Regulations issued by the Council on Environmental Quality appear in the vol-
ume containing part 790 to End. The OMB control numbers for title 40 appear
in § 9.1 of this chapter.
For this volume, Cheryl E. Sirofehuek was Chief Editor. The Code of Federal
Regulations publication program is under the direction of Prances D. McDonald,
assisted by Alomha S. Morris.
IX
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Title 40—Protection of
Environment
(This "book contains parts 136 to 149)
Part
CHAPTER I—Environmental Protection Agency (Continued) 136
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CHAPTER I—ENVIRONMENTAL PROTECTION
AGENCY (CONTINUED)
EDITORIAL NOTE: Nomenclature changes to chapter I appear at 65 PR 47324, 47325, Aug. 2,
2000, and at 66 PR 34375, 34376, June 28, 2001.
SUBCHAPTBB D—WATER PROGBAMS (CONTINUED)
Port Page
136 Guidelines establishing test procedures for the
analysis of pollutants 5
140 Marine sanitation device standard 339
141 National primary drinking water regulations 343
142 National primary drinking water regulations im-
plementation .,,,.,. 561
143 National secondary drinking water regulations 616
144 Underground injection control program 618
145 State UIC program requirements 685
146 Underground injection control program: Criteria
and standards 698
147 State underground injection control programs 728
148 Hazardous waste injection restrictions ., 829
149 Sole source aquifers 838
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SUBCHAPTER D—WATER PROGRAMS (CONTINUED)
PART 136—GUIDELINES ESTAB-
LISHING TEST PROCEDURES FOR
THE ANALYSIS OF POLLUTANTS
Sec,
136.1 Applicability.
136.2 Definitions.
136.3 Identification of test procedures.
136.4 Application for alternate test proce-
dures.
136.5 Approval of alternate test procedures.
APPENDIX A TO PART 136—METHODS FOR OR-
GANIC CHEMICAL ANALYSIS OF MUNICIPAL
AND INDUSTRIAL WASTEWATBB
APPENDIX B TO PART 136—DEFINITION AND
PROCEDURE FOR THE DETERMINATION OF
THE METHOD DETECTION LIMIT—REVISION
1,11
APPENDIX C TO PART 136—INDUCTIVELY COU-
PLED PLASMA—ATOMIC EMISSION SPIC-
TROMETRIC METHOD FOR TRACE ELEMENT
ANALYSIS OF WATER AND WASTES METHOD
200.7
APPENDIX D TO PART 136—PRECISION AND RE-
COVERY STATEMENTS FOR METHODS FOB
MEASURING METALS
AUTHORITY: Sees. 301, 304(h), 307 and 501(a),
Pub. L. 98-217, 91 Stat. 1566, et seq. (33 U.S.C.
1251, et seq.) (the Federal Water Pollution
Control Act Amendments of 1972 as amended
by the Clean Water Act of 1977).
§ 136.1 Applicability.
The procedures prescribed herein
shall, except as noted in §136.5, be used
to perform the measurements indicated
whenever the waste constituent speci-
fied is required to be measured for:
(a) An application submitted to the
Administrator, or to a State having an
approved NPDES program for a permit
under section 402 of the Clean Water
Act of 1977, as amended (CWA), and/or
to reports required to be submitted
under NPDES permits or other re-
quests for quantitative or qualitative
effluent data under parts 122 to 125 of
title 40, and,
(b) Reports required to be submitted
by discharges under the NPDES estab-
lished by parts 124 and 125 of this chap-
ter, and,
(c) Certifications issued by States
pursuant to section 401 of the CWA, as
amended.
[38 FR 28758, Oct. 16, 1973, as amended at 49
PR 43250, Oct. 26,1984]
§138.2 Definitions.
As used in this part, the term:
(a) Act means the Clean Water Act of
1977, Pub. L, 95-217, 91 Stat. 1566, et seq,
(33 U.S.C. 1251 et seg.) (The Federal
Water Pollution Control Act Amend-
ments of 1972 as amended by the Clean
Water Act of 1977).
(b) Administrator means the Adminis-
trator of the U.S. Environmental Pro-
tection Agency.
(c) Regional Administrator means one
of the EPA Regional Administrators.
(d) Director means the Director of the
State Agency authorized to carry out
an approved National Pollutant Dis-
charge Elimination System Program
under section 402 of the Act.
(e) National Pollutant Discharge Elimi-
nation System (NPDES) means the na-
tional system for the issuance of per-
mits under section 402 of the Act and
includes any State or interstate pro-
gram which has been approved by the
Administrator, in whole or in part,
pursuant to section 402 of the Act,
(f) Detection limit means the minimum
concentration of an analyte (sub-
stance) that can be measured and re-
ported with a 99% confidence that the
analyte concentration is greater than
zero as determined by the procedure
set forth at appendix B of this part.
[38 PE 28758, Oct. 16, 1973, as amended at 49
FR 43250, Oct. 28, 1984]
§ 136.3 Identification of test proce-
dures.
(a) Parameters or pollutants, for
which methods are approved, are listed
together with test procedure descrip-
tions and references in Tables IA, IB,
1C, ID, IE, and IP. The full text of the
referenced test procedures are incor-
porated by reference into Tables IA, IB,
1C, ID, IE, and IF. The incorporation by
reference of these documents, as speci-
fied in paragraph (b) of this section,
was approved by the Director of the
Federal Register in accordance with 5
U.S.C. 552(a) and 1 CFR part 51. Copies
of the documents may be obtained from
the sources listed in paragraph (b) of
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§136.3
40 CFR Ch. I (7-1-04 Edition)
this section. Information regarding ob-
taining these documents can be ob-
tained from the EPA Office of Water
Statistics and Analytical Support
Branch at 202-566-1000. Documents may
be inspected at EPA's Water Docket,
EPA West, 1301 Constitution Avenue,
NW., Boom B135, Washington, DC
(Telephone: 202-566-2426); or at the Na-
tional Archives and Records Adminis-
tration (NARA). For information on
the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal register/
code of_Jederal_regulations/
ibr locations.html. These test proce-
dures are incorporated as they exist on
the day of approval and a notice of
anys change in these test procedures
will be published in the FEDERAL REG-
ISTER. The discharge parameter values
for which reports are required must be
determined by one of the standard ana-
lytical test procedures incorporated by
reference and described in Tables IA,
IB, 1C, IE, and IP, or by any alternate
test procedure which has been approved
by the Administrator under the provi-
sions of paragraph (d) of this section
and §§136.4 and 136.5. Under certain cir-
cumstances (paragraph (b) or (c) of this
section or 40 CPR 401.13) other test pro-
cedures may be more advantageous
when such other test procedures have
been previously approved by the Re-
gional Administrator of the Region in
which the discharge will occur, and
providing the Director of the State in
which such discharge will occur does
not object to the use of such alternate
test procedure.
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TABLE IA—LIST OF APPROVED BIOLOGICAL METHODS
Parameter and units
Bacteria:
1. Coliform (fecal), num-
ber per 100 mL.
2. Coliform (fecal) in
presence of chlorine,
number per 100 mL.
3. ColHorm (total), num-
ber per 100 mL.
4. Colrform (total), in
presence of chlorine,
number per 100 mL.
100 mL3».
S. Fecal streptococci,
number per 100 mL.
per 100 mL.
Protozoa:
Aquatic Toxfcity:
10. Toxfcity, acute, fresh
water organisms,
LC50, percent effluent.
Method1
Most Probable Number (MPN), 5
tube 3 dilution, or
Membrane fitter (MF)2, single
step,
MPN, 5 tube, 3 dilution, or
MF, single step6 .
MPN, 5 tubs, 3 dilution, or
MPN, 5 lube, 3 dilution, or
MF8 with enrichment
MPN 7*15, multiple tube
multiple tube/multiple well
MF»*7-8-9 two step, or
single step
MPN, 5 tube, 3 dilution,
MFZ or .
MPN '• » multiple tuba
MF «>•*•»•» two step .
Fittration/l MS/FA
Fitlration/IMS/FA
Ceriodaphnte dubia acute
EPA
p. 1323
p. 1243
p. 1323
p. 1243
p. 1143
p. 1083
p. 1143
p. 111'
1 103.1 »
1603*1
1604 *z
p. 1393
p. 1363
p. 143*
1106.1*4
160025
p. 1433
162226
1623Z7
162327
2002.0 M
Standard methods 18th,
19th, 20th Ed.
9221C E"
9222D"
9221CE-"
9222D*
9221B4
9222B*
9221 B*
9222(B+B.5c)"
9221B.1/9221F*''2'"
9223B4-13
9Z2ZB/9222G*-19
9213D"
9230B4, 9230C4
9230B4
9230C4
ASTM
D5392-9310
D6S03-9910
D5259-9210
AOAC
991. 1511
B-0055-
85s
uses
B-0050-
85s
B-0025-
8S5
Other
Colilert®13-17
Colilert-IS®"'1*17
mColiBue 24 "
Enterotort®".23
<
3
f
I
o
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TABLE IA—LIST OF APPROVED BIOLOGICAL METHODS—Continued
Parameter and units
1 1 . Toxicrty, acute, estu-
arine and marine or-
ganisms of the Atlan-
tic Ocean and Gulf of
Mexico, LC50, per-
cent effluent.
12. Toxicity, chronic,
fresh water orga-
nisms, NOEC or IC25,
percent effluent.
1 3. Toxicity, chronic, es-
tuarine and marine or-
ganisms of the Atlan-
tic Ocean and Gulf of
Mexico, NOEC or
IC25, percent effluent.
Method1
Daphnia pup/ex and Daphnia
magna acute.
Fathead Minnow, Pimephales
promelas, and Bannerfin shin-
er, Cyprinella teedsi, acute.
Rainbow Trout, Oncorhynchus
mykiss, and brook trout,
Salvelinus fontinalis, acute.
Mysid, Mysidopsis bahia, acute ..
Sheepshead Minnow,
Cyprinodon variegatus, acute.
Silverside, Menidia beryllina,
Menidia menidia, and Menidia
peninsulae. acute.
Fathead minnow, Pimephales
promelas, larvalsurvival and
growth.
Fathead minnow, Pimephales
promelas, embryo-larval sur-
vival and teratogenicity.
Daphnia, Ceriodaphnia dubia,
survival and reproduction.
Green alga, Selenastrum
capricomutum, growth.
Sheepshead minnow,
Cyprinodon variegafusjarval
survival and growth.
Sheepshead minnow,
Cyprinodon
variegarus, embryo-larval sur-
vival and teratogenicity.
Inland silverside, Menidia
beryllina, larval survival and
growth.
Mysid, Mysidopsis bahia, sur-
vival, growth.and fecundity.
EPA
2021 .029
2000.029
2019.029
2007.0 29
2004.0 29
2006.0 29
1000.0 3°
1001.0 3°
1 002.0 3°
1003.0 3°
1004.031
1005.03'
1006.03'
1007.03'
Standard methods 18th,
19th, 20th Ed.
ASTM
AOAC
USGS
Other
ur>
0*
o
•n
JO
O
p-
i
i
m
O.
§
-------
Sea urchin, Arbaoia punctulata,
fertilization.
08,0 3'
Notes to Table IA:
1 The method must be specified when results are reported.
2A 0.45 ^im membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractabtes which could interfere with their
growth.
3USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency,
Cincinnati, Ohio. EPA/600/8~78/017.
"APHA. 1998, 1995, 1992. Standard Methods for the Examination of Water and Wastewater. American Public Hearth Association. 20th, 19th, and 18th Editions. Amer. Publ. Hlth. Assoc.,
Washington, D.C.
5US6S. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods tor Collection and Analysis of Aquatic Biological
and Microbiological Samples, U.S. Geological Survey, U.S. Department of Interior, Beston, Virginia.
6 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.
7 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character,
consistency, and anticipated organism density of the water sample.
"When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncolrform bacteria, or samples that may contain organisms stressed by
chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.
9To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely
tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines,
10ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. American Society for Testing and Materials. 100 Barr Harbor Drive,
West Conshohocken, PA 19428.
11AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists International. 481 North Frederick Ave-
nue, Suite 500, Gaithersburg, Maryland 20877-2417.
12The multiple-tube fermentation test is used in 9221 B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and
LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total conform using lactose broth is less than 10 per-
cent. No requirement exists to run the completed phase on 10 percent of all total coiHorm-positive tubes on a seasonal basis.
13These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme (3-glucuronidase produced by E CD//.
14 After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incu-
bation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 ug/mL of MUG may be used.
15Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using muitipie-tube procedures, employ an appropriate tube and dilution configuration of the sample as
needed and report the Most Probable Number (MPN). Samples tested with ColilerW may be enumerated with the multiple-well procedures, Quantl-Tray® or Quanti-Tray« 2000, and the
MPN calculated from the table provided by the manufacturer.
1BColllert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 aC rather than the 24 h
required for the CoiilerW test and is recommended for marine water samples,
17 Descriptions of the ColilertS, Colilert-18», Quanti-Tray*. and Quanti-Tray«/2000 may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.
18 A description of the mColiBlue24" test. Total Coiiforms and E. coll, Is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
19Sub}ect total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
20 USEPA. 2002. Method 1103.1: Escherichia coli (E. call) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia call Agar (mTEC). U.S. Environmental Protection
Agency, Office of Water, Washington D.C. EPA-821-R-02-020.
21USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar ( modified mTEC). U.S. Environ-
mental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-023.
22 Preparation and use of Ml agar with a standard membrane filter procedure is set forth in the article, Brenner et ai. 1993, "New Medium for the Simultaneous Detection of Total Coliform
and Escherichia coli in Water," Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604: Total Coliforms and Escherichia coli (E. col/} In Water by Membrane Filtration by
Using a Simultaneous Detection technique (Ml Medium). U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA 821-R-02-Q24.
23A description of the Enterolert* test may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.
24USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental Protection Agency, Office
of Water, Washington DC. EPA-821-R-Q2-021.
25 USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-p-D-Glucostde Agar (mEI). U.S. Environmental Protection Agency, Of-
fice of Water, Washington, DC. EPA-821-FM12-022.
26 Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, imrnunofluorescence assay to determine concentrations, and confirmation
through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium, USEPA. 2001. Method 1622: Cryptosporidium in Water by Fittration/IMS/FA.
U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821-H-G1-026.
^Method 1623 uses filtration, concentration, irnmunomagnetrc separation of oocysts and cysts from captured material, immunofluorescence assay to determine concentrations, and con-
firmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of dyptosporicXum and Giardla oocysts and cysts. USEPA. 2001. Method
1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821-R-01-G25.
2e Recommended for enumeration of target organism in ambient water only.
tOi
-------
S9USEPA. October 2002. Methods for Measuring the Acute Toxlcity of Effluents and Receiving Waters to Freshwater and Marine Organisms, Fifth Edition. U.S. Environmental Protection
Agency, Office of Water, Washington DC. EPA/821/R-02/012.
soysEPA, October 2002. Short-term Methods for Estimating the Chronic Toxicity ol Effluents and Receiving Waters to Freshwater Organisms. Fourth Edition, U.S. Environmental Protec-
tion Agency, Office of Water, Washington DC. EPA/821/R-02/013.
31USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. Third Edition. U.S. Environmental
Protection Agency, Office of Water, Washington DC. EPA/821/R-02/014.
TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES
Parameter, units and
method
1 . Acidity, as CaCOj, mg/L:
Electrometrlc endpoint or
phenolphthalein endpoint.
2. Alkalinity, as CaCOj, mg/L:
Electrometric of Colorimetric
titratton to pH 4.5, manual
or automatic.
3. Aluminium— Total,4 mgyL; Diges-
tion 4 followed by:
AA direct aspiration **
AA furnace
Inductively Coupled Plasma/
Atomic Emission Spec-
trometryflCP/AES)*.
Direct Current Plasma
(DCP)3".
Cotorimetric (Eriochrome
cyanine R).
4. Ammonia (as N^, mg/L:
Manual, distillation (at pH
9.5) o followed by.
Tttration
Electrode
Automated phenate, or
5. Antimony-Total,* mg/L; Digestion4
followed by:
AA direct aspiration38
ICP/AES36 .. .
6. Arsenic-Total" mg/L:
Reference (method number or page)
EPA'-"
3051
3101
310.2.
202 1
2022
200 75
3502
3502
3S02
3503
350.1
204.1
2042
200 ?5
Standard Methods [Edi-
tion(s)]
2310 B(4a) [18th, 19th,
20th].
23208118th, 19th, 20th] ...
3111 D [18th 19th] . ..
3113B[181h, 19th].
3120 B [18th, 19th, 20th] ...
3500-AI B [20th] and
3500-AI D [18th, 19th],
4500-NH, B (18th, 19th,
20th],
4S)0-NH1C[18th]
4500-NHj C [19th, 20th]
and 4500-NK, E [16th].
4500-NH3DorE[19th,
20th] and 4500-NH3 F or
G [18th].
4500-NH3 G [19th, 20th)
and 4500-NH, H [18th].
3111 B [18th, 19th]
3113 B[18m 19th]
3120 B [18th, 19th, 20th] ...
ASTM
D1067-92
D1 067-92
D4190-94
D1426-98(A)
D1428-98(B).
uses*
1-1020-85
1-2030-85
1-1030-85
I-2030-85
1-3051-85
M471-9750
1-3520-85
1-4523-85
Other
973.4S3
Mote 34.
973.49 3
97S.493
Note 7,
o
^
I
-------
Digestion* followed by
AA fumade
ICP/AES * or
Colorimelric (SDDC)
7. Barium-Total," mg/L; Digestion4
followed by:
ICP/AES 14
DCP14
8, Beryllium-Total," mg/L; Digestion'1
followed by;
AA direct aspiration „,...,.
ICP/AES ,
DCP or
9. Biochemical oxygen demand
(BODs), mg/L:
10, Borons-Total, mg/L:
ICP/AES or
DCP
11. Bromide, mg/L:
12. Cadmium— Total," mg/L; Diges-
tion "followed by:
ICP/AES36 , ,
DCP*
13. Calcium— Total,* mg/L; Diges-
tion* followed by:
ICP/AES ,..
DCP or
Titrimetric (EDTA)
14. Carbonaceous biochemical oxy-
gen demand (CBOD 3), mg/L«:
with nitrification inhibitor.
(COD), mg/L; Titrimetric
or
206.5
2063
206,2
20075
206.4
206 1
2082 . . .
200 7s
210,1
2102
200.7s
405 1
212.3
20075
320 1
213 1
2132
200.7s
215 1
200,7s
2152
410 1
410.2
3114 B4d [18th 19fh]
3113B (18th 19th]
3120 B [18th 19th 20th]
3500-As B [20th] and
3500-As C [18th, 19th).
3111 D [18th 19th]
31 13 B [18th, 19th]
3120 B [18th 19th 20th]
3111 D[18th, 19thJ
31 13 B [18th 19Bi] . .
3120 B [18th, 19th, 2«hJ ..
3500-Be D [Iflth, 19th] .. .
5210 B [18th 19th 20th]
4500-B B [18th, 19th, 20th]
3120 B (18th 19th 20th] ..
3111 B or C [18th 19th)
31 13 B [18th 19th]
3120 B [18th, 19th, 20th] ...
3500-Cd D [18th IStti]
3111 6 [18th 19th]
3120 B (18th, 19th, 20th] ..
3500-Ca B [20lh] and
3500-Ca D [18th, 19th].
5210 B [18th, 19th, 20th].
5220 C [18th, 19«h, 20th] .
02972-97(8)
D2972-97JCJ
D2972-97(A)
D4382-95
D3645-93<88)jA)
D3645-93(88)(B)
D41 90-94
D41 90-94
D1246-95(C)
D3557-95 (A or B)
D3557-95JD)
04190-94
D3557-95(C).
D51 1-93(B)
D511-93(A)
D1252-95(A)
J-30S2-85
(-4063-88 4*
I-3060-S5
I-3084-85
1-3095-%
1-4471 -97 so
1-1578-78"
1-3112-85
(-4471-97 so
1-1125-85
1-3135-85 or 1-3136-85
M1 38-89 51
I-1472-8S or 1-4471-975°
1-3152-85
|_447t_97so
I-3560-85
N3562-85
Note 34.
Note 34.
973.44,3p. 17«
Note 34.
p. S44«
974.27,3 p. 37»
Note 34.
Note 34.
9T3.46,3 p. 17 »
-------
TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
Parameter, unils and
method
Spectrophotometric, manual
or automatic.
16. Chloride, mg/L:
Titrimetric (silver nitrate) or
Colorimetric, manual or
Automated (Ferricyanide) ...
17. Chlorine — Total residual, mg/L;
Titrimetric:
Back titration ether end-
point15 or.
DPD-FAS
Spectrophotometric, DPD ...
Or Electrode
18. Chromium VI dissolved, mg/L;
0.45 micron filtration followed by:
AA chelation-extraction or ...
Colorimetric
(Diphenylcarbazide).
19. Chromium-Total,4 mg/L; Diges-
tion " followed by:
AA direct aspiration x
AA chelation-extraction
ICP/AES36
DCP36or
Colorimetric
(Diphenylcarbazide).
20. Cobalt— Total," mg/L; Digestion4
followed by:
AA direct aspiration
ICP/AES
Reference (method number or page)
EPA1-"
410.3.
4104
3253
325.1 or 325.2
330.1
3303
330.2
330.4
3305
218.4
218 1
218.3
21B2
2007s
219 1
219.2
200.75
Standard Methods [Edi-
tion(s)]
5220 D [18th, 19th, 20th] ...
4500-CI-B [18th, 19th,
20th].
4500-CI-C [18th, 19th,
20th].
4500-CI-E[18th, 19th,
20th].
4500-CI D [18th, 19th,
20th).
4500-CI B [18th, 19th,
20th].
4500-CI C [18th, 19th,
20th].
4500-CI F [18th, 19th,
20th].
4500-CI G [18th, 19th,
20th].
3111 C [18th 19th]
3500-Cr B [20th] and
3500-CrD[18th, 19th].
3111 B [18th, 19th]
3111 C[18th, 19th].
3113 B [18th 19th]
31 20 B [18th, 19th, 20th],
3500-Cr B [20th] and
3500-Cr D[18th, 19th].
3111 BorC [18th, 19th] ....
3113 B [18th, 19th]
3120 B [18th. 19th. 20thl ...
ASTM
D1252-95(B)
D512-89(B)
D512-89(A)
01253-86(92).
D1687-92(A)
D1687-92(B)
D1687-92(C)
D4190-94
D3558-94(A or B)
D3558-94(C)
USGS2
1-3561-85
1-1183-85
1-1184-85 .
1-1187-85
1-2187-85
1-1232-85
1-1230-85
I-3236-85
I-3233-9346.
I-3239-85
M243-89".
1^4471-9750.
Other
Notes 13, 14.
973.51 3
Note 16.
974.273
Note 34.
p. 379
o
-n
TO
O
-------
DCP
21. Color platinum cobalt units or
dominant wavelength, hue, lumi-
nance purity:
Colorimetric (ADMI), or.
22. Copper— Total," mg/L; Digestion 4
followed by:
AA direct aspiration M
ICP/AES »
DCP36 or
Colorimetric (Neocuproine)
or.
23. Cyanide — Total, mg/L:
MgCI2 followed by..
or.
24. Available Cyanide, mg/L:
MgCI2 followed by
tttrimetric or
Spectrophotometric.
exchange, followed by
amperometry.
25. Fluoride — Total, mg/L:
by.
Electrode, manual or
Colorimetric (SPADNS)
Or Automated complexone
26. Gold — Total,4 mg/L; Digestion4
followed by:
DCP
27. Hardness— Total, as CaCOi, mg/
L:
Automated Colorimetric
110 1
1102
110.3
220.1
2202
200 7 '
3352"
3353"
335 1
340.2
340.1
340.3
231 1
231 2
130.1
2120 E [18th 19th 20th]
2120 B [18th 19th 20th]
2120 C [18th, 19th, 20th].
3111 BorC [18th, 19th] ....
3113 B [18th 19th]
3120 B [18th 19th 20th]
3500-Cu B [20th] and
3500-Cu D [18th, 19th].
3500-Cu C [20th] and
3500-As B [18th, 19th].
4500-CN C [18th, 19th,
20th].
4500-CN D [18th 19th
20th].
4500-CN E [18th 19th
20th].
4500-CN G [18th 191h,
20th].
4500-F B [18th, 19th, 20th]
4500-FC[18th, 19th, 20th]
4500-F D [18th, 19th, 20th]
4500-F E [18th, 19th, 20th]
3111 B [18th 19th]
D41 90-94
D1688-95(A or B)
D1688-95JC)
D41 90-94
D2036-98(A)
D2036-98(A)
D2036-98(B)
D1 179-93(6)
D1179-93(A)
1-1 250-85
1-3270-85 or 1-3271-85 ....
1-4274-8951
1 — 4471— 97 !0
I-3300-85
I-4302-85
I-4327-85
. Note 34.
Note 18.
974.27' p. 37'
Note 34.
Note 19.
p. 22 »
OIA-16774
Note 34.
an
-------
TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
Parameter, units and
method
Trlrimetric (EDTA), or Ca
plus Mg as their carbon-
ates, by inductively cou-
pled plasma or AA direct
aspiration {See Param-
eters 13 and 33).
28. Hydrogen ion (pH), pH units:
Eleetrometrfc measurement,
or.
29. Indium— Total,4 mg/L; Digestion4
to/lowed by:
30. Iron— Total,4 mg/L; Digestion4
followed by:
AA direct aspiration-1*
AA furnace
ICP/AES"
DCPM or
Colorimetric (Phenan-
thrcdine).
31, Kjektehl Nitrogen— Total, {as N),
mfl/L:
Digestion and distillation fol-
lowed by.
Electrode
Semi-automated block digester cd-
orimetric,
Manual or block digestor potentio-
metric.
Block digester, followed by Auto dis-
tillation and Titration, or.
32. Lend— Total,4 mg/L; Digestion"
followed by;
AA direct aspiration3*
Reference (method number or page)
EPA KM
130.2
150.1
235 1
23S.2
236.1
236.2
200.7' . .
3S1.3
351.3
351 3
351.3 ... .
351 1
351 .2 . .
351 4
239.1
Standard Methods [Edi-
tion^)]
2340 B or C [18th, 19th,
20th).
45QQ-H-1- B [18th, 19th,
20th].
3111 B [18th 19th]
3111 B or C [18th, 19th] ....
3113 B[18th, 19th]
3120 B [18th 19th 20th]
3500-Fe B [20th] and
3500-Fe D [18th, 19th).
4500-N,, B or C and
4500-NH, B [18th, 19*.
20th].
4500-NH, C [18th]
4500-NH, C [19th, 20»h]
and 4500-NH, E [18thJ.
3111 BorCnsth. 1«M ....
ASTM
01128-86(92)
01293-84 !90)(A or B)
D1068-96(A or B)
D1068-96(C)
D4190-94 .. .
D 1068-96(0)
03590-fl9(A)
D3590-89(A)
D3590-fl9(A)
03590-69(8)
D3590-89(A)
D3559-96(A or B)
USGS8
1-1338-85
1-1 588-45
1-2587-85
1-3381-85
1_4471 .97 »
M551-?8»
1-4515-91 ".
I-3399-8S
Other
973.52B'
973.41 '
Note 21.
974.27'
Note 34.
Note 22.
973.48 3
Note 39.
Note 40.
Note 41.
974.273
o
Tt
TO
O
E
-------
AA furnace
ICP/AES36
DCP-"
VoNamelry11 or
Colorimetric (Drthizone)
33. Magnesium— Total,4 mg/L; Di-
gestion 4 followed by:
ICP/AES
DCPor
Gravimetric
34, Manganese-Total," mg/L; Diges-
tion" followed by:
AA furnace
ICP/AES36
OCPm or
Colorimetric (Persulfate!, or
(Penodate) .........
35. Mercury — Total,4 mg/L:
Cold vapor manual or
Oxidation, purge and trap,
and cold vapor atomic flu-
orescence spectrometry
(ng/L).
36. Molybdenum— Total", mg/L; Di-
gestion " followed by:
AA furnace
ICP/AES
DCP ..
37. Nickel— Total," mg/L; Digestion4
followed by:
AA direct aspiration ^
AA furnace
ICP/AES36
DCP56, or
38. Nitrate (as N), mg/L:
Colorimetric (Brucine sul-
fate), or Nitrate-nitrite N
minus Nitrite N (See pa-
rameters 39 and 40).
39. Nitrate-nitrite (as N),
mg/L:
Cadmium reduction. Manual
or.
239.2 ..
200 75
242 1
200.7* .. . .
2431
2432 .
2007s
245.1
2452
1631 E*>
2461
246.2 . . .
2007s
2481
24S.2
200 Js
352.1
353.3
31 13 B [18th 19th]
3120 B [18th 19th 20thJ
3500-Pb B [ 20th] and
3500-PbD[18th, 19th).
3111 B(18th 19th]
3120 8 {18th, 19th, 20th] ...
3500-Mg D [18th, 19th]
3111 B(18th 19th]
31 13 B [18th 19th]
3120 B [18th 19th 20th]
3SOO-Mn B [20th] and
3500-Mn D (16lh, 19th].
3112 B [18th, 19th)
3111 D[18th 19th]
31 13 B [18th, 19th)
3120 B [18th 19th 20th]
3111 BorC [18th 19lh] .
3113 B(18lh, 19th]
3120 B [18th 19th 20th]
3500-Ni D[17thl
4500-NOj-E [18th, 19lh,
20th].
D3559-96(D)
04190-94
D3559-96(C)
D511-93(B)
0858-95(A or B)
D858-^95(C)
D4 190-94
D3223-91
01 886-90! A or B)
D1886-90(CS
04190-94
03867-99(6).
M403-89 51
|_4471_97»
|_3447_85
M471-97SO
i-3454-85
1-4471-97 m
(-3462-85
|_3490_85
1-3492-98"'
1-4471 ~@7SQ
1-3499-85
1-4503-89 51
(_4471_97»
Note 34.
974.27'
Note 34.
974.27 3
Note 34
920.203'
Note 23.
977.22 a
•o
5
8
1
Note 34.
Note 34.
973.50,3419D," p. 2B9
-------
TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
un
Parameter, units and
method
Automated, or
Automated hydrazine
40. Nitrite (as N), mg/L;
Spectrophotometric:
41. Oil and grease — Total recover-
able, mg/L:
Gravimetric (extraction)
Oil and grease and non-
polar material, mg/L:
Hexane extractable mate-
rial (HEM): n-Hexane ex-
traction and gravimetry.
Silica gel treated HEM
(SGT-HEM): Silica gel
treatment and gravimetry.
42. Organic carbon— Total (TOC),
mg/L:
Combustion or oxidation
43. Organic nitrogen (as N), mg/L:
Total Kjeldahl N (Parameter
31) minus ammonia N
(Parameter 4).
44. Orthophosphate (as P), mg/L;
Ascorbic acid method:
Manual single reagent
45. Osmium— Total4, mg/L; Diges-
tion "followed by:
AA direct aspiration, or
AA furnace
46. Oxygen, dissolved, mg/L:
Winkler (Azide modification),
or.
Electrode
Reference (method number or page)
EPA '.«
353.2
353 1
354 1
413 1
1664A"2
1664A42.
415.1
365 1
365.2
365.3.
252.1
252.2.
360 2
360.1
Standard Methods [Edi-
tion^)]
4500-NO,-F [18th, 191h,
20th].
4500-NO,-H [18th, 191h,
20th].
4500-NO2-B [18th, 19th,
20th].
5520B[18th, 191h, 20th]38.
5520B[18th, 19th, 20th]38.
5310 B, C, or D [18th, 191h,
20th].
4500-PF[18th, 191h, 20th]
4500-P E[18th, 191h, 20th]
3111 D[18th, 191hJ.
4500-OC[18th, 191h, 20th]
4500-OG [18th, 19th,
201h].
ASTM
D3867-99(A)
D2579-93 (A or B) ....
D515-88(A)
D888-92(A)
D888-92(B)
USGS2
I-4545-85.
I-4540-85.
1-4601-85
I-1575-788
1-1 576-78°.
Other
Note 25.
973.47,3 p. 14 2"
973.563
973.553
973.45B3
&
o
Tl
TO
9
g
m
a
I
-------
47, Palladium—Total," tng/L; Diges-
tion4 followed by:
AA direct aspiration, or
AA furnace
DCP
48, Phenols, rng/L:
Manual distillation26
Followed by:.
Colorimetric
(4AAP) manual,
or.
Automated18
49. Phosphorus (elemental), mg/L:
Gas-liquid chromatography
50. Phosphorus—Totai, mg/L:
Persulfate digestion fol-
lowed by.
Manual or
Automated ascorbic acid re-
duction.
Semi-automated biock
digester.
51. Platinum—Total,* mg/L: Diges-
tion" followed by:
AA direct aspiration
AA furnace
DCP
52. Potassium—Total,4 mg/L: Diges-
tion * followed by:
AA direct aspiration
ICP/AES
Flame photometric, or
253.1 .
253.2 .
420.1 .
420.1 .
420.2.
365.2 ....
365.2 or 385.3 .
365.1 .
365.4 ,
255.1 ..
255.2.
258.1 .
200.7s
Colorimetric
53. Residue—Total, mg/L:
Gravimetric, 103-105*
54. Residue—filterable, mg/L:
Gravimetric, 180°
55. Residue—nonfilterable (TSS),
mg/L:
Gravimetric, 103-105" post
washing of residue.
56. Residue—settleable, mg/L:
Volumetric, (Imhotf cone), or
gravimetric.
57. Residue—Volatile, mg/L:
Gravimetric, 550°
58. Rhodium-Total,'5 mg/L; Diges-
tion4 followed by:
AA direct aspiration, or
180.3 .
160.1 .
180.2.
160.5 .
160.4 .
3111 B[18th, 1ith).
4500-P B, 5 [18th, 19th,
20thJ.
4500-P E [18th, 19th, 20th]
4500-P F [18th, 19th, 80th)
3111 B[18th, 19th).
3111 B[18th, 19th]
3120 B (18th, 19th, 20th].
3500-K B [20th] and 3500-
KD[18th, 19th).
2540 B [18th, 19th, 20th] ...
2540 C [18th, 19th, 20th) ...
2540 D [18th, 19th, 20th) ...
2540 F [18th, 19th, 20th).
D515-88(A)
D515-88(B)
i 3111 B[18th, 19th].
1-4600-85 ...
M610-91 *>
(-3630-85 ,
1-3750-85.
1-1750-85.
1-3765-85.
p. 827"
p. S2810
Note 34.
Note 27.
Note 27.
Note 28.
973.5S3
973.56'
!
I
>
Note 34
973.53'
317 B"
(01
-------
TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
CO
Parameter, units and
method
59, Ruthenium— Tota*,* mg/L; Diges-
tion 4 followed by;
AA direct aspiration, or ..,.„,
60, Selenium— Total,4 mg/L; Diges-
tion 4 followed by:
ICP/AES,36 or ....................
61. Silica*1— Dissolved, mg/L; 0.45
micron filtration followed by:
Colorimetric, Manual or
Automated
(Molybdosilicate), or.
ICP .. .
62. Silver— Total," mg/L: Diges-
tion «» followed by:
AA furnace
ICP/AES
DCP
63. Sodium— Total,4 mg/L; Diges-
tion * followed by:
AA direct aspiration
ICP/AES
DCP or
64, Specific conductance,
micromhos/cm at 25 °C:
Wheatstone bridge
65. Sultate (as SO4), mg/L:
Automated colorimetric (bar-
ium chtoranilate).
66. Sulfide (as S), mg/L:
Trtrimetric (iodine), or
Reference (method number or page)
EPA'."
265.2.
267.1
267.2.
2702
200.7s
370 1
200,7s
272.1
272.2
200.75
273 1
200 7s
1201
375.1.
375 3
3754
376 1
Standard Methods [Edi-
tion(s)]
3111 B[18th, 18th].
3113 BflBth, 19th]
3120 B [18th, 19th, 20th].
3114 B [18th 19th]
4500-SIO2 C [20th] and
4500-Si D [18th, 19th].
3120 B [18th, 19th, 20th) ...
3111 B or C [18th, 19th] ....
3113 B [18th, 19th)
3120 B [18th, 19th. 20th] ...
3111 B [18th 19th]
3120 B [18th 18th 20th]
3500 Na B [20th] and 3500
NaD[18th, 19th).
2510 B [18th, 19th, 20th] ...
4500-SO4-2CorD[18th,
19th, 20th).
4500-S-ZF [19th, 20th] or
4500-S-2E [18th].
ASTM
Q3859-98(B)
D3a59-98(A)
0859-94
D1125~95(A)
0516-90
USGS2
1-4668-88 *'.
1-3667-85.
1-1700-85.
I-2700-85.
1-4471-97 50.
I-3720-85
M724-«9S1
M471-97 so
1-3735-85
1-4471-9750
1-2781-85
I-3840-85.
Other
974.27,3 p. 37«
Note 34.
973.543
Note 34.
973.403
925.543
426C»
tat
w
o
Tl
TO
O
-------
Colorirrtetric (methylene
blue).
67. SutfHe (as SO,), mg/L:
Tftrimslric (todine-todate)
68. Surfactants, mg/L:
blue).
69. Temperature, °C:
70. Thallium— Total," mg/L; Diges-
tion * followed by:
AA direct aspiration
AA fumade
ICP/AES
71. Tin— Total," mg/L; Digestion4 fol-
lowed by:
AA furnace, or ,...,.
ICP/AES
72. Titanium — Total,4 mg/L; Diges-
tion " followed by:
AA direct aspiration
AA furnace
DCP
73. Turbidity, NTU:
74. Vanadium— Total,4 mg/L; Diges-
tion 4 followed by:
AA direct aspiration ..... .......
ICP/AES .. .
DCP or
Cotortmetric (Gallic Acid)
75. Zinc— Total,4 mg/L; Digestion*
followed by:
AA furnace
ICP/AES x
DCP x or
376,2 ,
3771
4251
170 1
279.1 ...
279,2.
2007"
2821
282.2
200.7'.
283 1
283.2.
190 1
286,1
2862
200.7*
280 1
289.2.
200.75
4500-S~2D [18th 19th,
20th].
4500-SCK~JB[18th 19th
20m].
5540 C [1 8th t9th 20th)
2550 B [18th 19th 20th]
3111 B[16lh. 19th].
3120 B (18th 19tti 20m)
31 1 1 B [18th 19thj
31 13 B [18th, 19th|.
31 1 1 D [18th, 19th].
2130 B [18th, 19th 20th] .
3111 D[18th, 19th).
3120 B [18th, 19th, 20th] ..
3500-V B [20th] and 3SOO-
VD(1Oh. 19th|.
3111 BorC [18»i 19fh]
3120 B [18lh, 19lh, 20lh] . .
3500-Zn E [18th, 19th]
3500-Zn B [20th] and
3500-Zn F [18th, 19th].
D2330-68
D1889-94(A)
D3373-93
D41 90-94
D1691-95IA or B)
D4 190-94
I-3850-78"
1-3860-85
W471^9750
(-3900-85
|_4471-97 so
Note 32.
Note 34.
Note 34
974273p 37"
Note 34.
Note 33
Table 1B Notes:
1 "Methods for Chemical Analysis of Water and Wastes," Environmental Protection Agency, Environmental Monitoring Systems Laboratory— Cincinnati (EMSL-CI), EPA-600/4-79-020,
Revised March 1983 and 1979 where applicable.
2 Fishman, M.J., et al. "Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, "U.S. Department of the Interior, Techniques of Water-Resource Investigations of
the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
'-Official Methods of Analysis of the Association of Official Analytical Chemists,' methods manual, 15th ed. (1990).
<0>
-------
4 For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended material and to destroy possible organic-metal <*•
complexes. Two digestion procedures are given in "Methods for Chemical Analysis of Water and Wastes, 1979 and 1983". One (Section 4.1.3), is a vigorous digestion using nitric acid. A —•
less vigorous digestion using nitric and hydrochloric acids (Section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types. x*
Particularly, if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive state. In those situations, the .
vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing large amounts of organic materials may also benefit by this vigorous *•»
digestion, however, vigorous digestion with concentrated nitric acid will convert antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as well as de-
terminations for certain elements such as antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all cases the
method write-up should be consulted for specific instructions and/or cautions.
Note to Table 18 Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the above, the EPA procedure must be
used. Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the referenced procedure for total metals
must be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample solution for total metals) may be omitted for AA (direct aspiration or graphite fur-
nace) and ICP analyses, provided the sample solution to be analyzed meets the following criteria:
a. has a low COD (<20)
b. is visibly transparent with a turbidity measurement of 1 NTU or less
c. is colorless with no perceptible odor, and
d. is of one liquid phase and free of paniculate or suspended matter following acidification.
5 The full text of Method 200.7, "Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes," is given at Appendix C of this Part
136.
6 Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary distillation step is not necessary: however,
manual distillation will be required to resolve any controversies.
7 Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Tech-
nologies, Inc., Elmsford, NY 10523.
8 The approved method is that cited in "Methods for Determination of Inorganic Substances in Water and Fluvial Sediments", USGS TWRI, Book 5, Chapter A1 (1979).
9 American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 25 West 43rd Street, New York, NY 10036.
10"Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency", Supplement to the Fifteenth Edition of Standard Methods for the Examination
of Water and Wastewater (1981).
11 The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
12 Carbonaceous biochemical oxygen demand (CBOD,) must not be confused with the traditional BOD; test method which measures "total BOD". The addition of the nitrification inhibitor
bO is not a procedural option, but must be included to report the CBOD; parameter. A discharger whose permit requires reporting the traditional BOD; may not use a nitrification inhibitor in the
O procedure for reporting the results. Only when a discharger's permit specifically states CBOD; is required can the permittee report data using a nitrification inhibitor.
13OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, PO Box 2980, College Station, TX 77840.
"Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, PO Box 389, Loveland, CO 80537.
15 The back titration method will be used to resolve controversy.
16 Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph
for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 ml 0.00281 N potassium iodate/100 ml solution, re-
spectively.
"The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
'"National Council bf the Paper Industry for Air and Stream Improvement, Inc. Technical Bulletin 253, December 1971. ^
19 Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979. Hach Chemical Company, PO Box 389, Loveland, CO 80537. O
20 After the manual distillation is completed, the autoanalyzer manifolds in EPA Methods 335.3 (cyanide) or 420.2 (phenols) are simplified by connecting the re-sample line directly to the f\
sampler. When using the manifold setup shown in Method 335.3, the buffer 6.2 should be replaced with the buffer 7.6 found in Method 335.2. Li
21 Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Tech- jn
nologies, Inc., Elmsford, NY 10523. _
22Tron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, PO Box 389, Loveland, CO 80537. O
23 Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537. 3"
24 Wershaw, R.L., et al, "Methods for Analysis of Organic Substances in Water," Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972 _
Revised 1987) p. 14. _
25 Nitrogen, Nitrite, Method 8507, Hach Chemical Company, PO Box 389, Loveland, CO 80537. VI
26 Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 * 9 NaOH. I
27 The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted at a pH of 10.0±0.2. The ap- T"
proved methods are given on pp 576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 51OC for the manual Spectrometric A
procedure. E
28R.F. Addison and R.G. Ackman, "Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography," Journal of Chromatography, Vol. 47, No. 3, pp. 421-426, 1970. m
29 Approved methods for the analysis of silver in industrial waste waters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides Q_
such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. =
Therefore, for levels of silver above 1 mg/L, 20 ml of sample should be diluted to 100 ml by adding 40 ml each of 2 M Na2S:Oi and NaOH. Standards should be prepared in the same Q
manner. For levels of silver below 1 mg/L the approved method is satisfactory. 3
aoThe approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition. v
-------
31 EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of total cyanide.
3S Stevens, H.H., Ficke, J.F., and Smoot, G.F., "Water Temperature—Influential Factors, Field Measurement and Data Presentation," Techniques of Water-Resources Investigations of the
U.S. Geological Survey, Book 1, Chapter D1, 1975.
33Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis. 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
M "Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AESQ029," 1986—Revised 1991, Thermo Jarrell Ash
Corporation, 27 Forge Parkway, Franklin, MA 02038,
36 Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC method for arsenic are provided in
Appendix D of this part titled, "Precision and Recovery Statements for Methods for Measuring Metals".
36"Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals", CEM Corporation, PO Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from
the CEM Corporation.
37 When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
^Only use Trichlorotrifluorethane (1,1,2-trichioro-1,2.2-trifluoroethane; CFC-113) extraction solvent when determining Total Recoverable Oil and Grease (analogous to EPA Method
413.1). Only use n-hexane extraction solvent when determining Hexane Extractable Material (analogous to EPA Method 1664A). Use of other extraction solvents is strictly prohibited.
39 Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, Ol Analyticat/ALPKEM, PO Box 9010. College Station, TX
77842.
"°Nitrogen, Total Kjeldahl, Method PA1-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, Ol Analytical/ALPKEM, PO Box 9010, College Station, TX
77842.
41 Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, Ol Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
42 Method 1664, Revision A "n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction
and Gravimetry" EPA-S21-R-98-QQ2, February 1999, Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, Virginia 22161.
^USEPA. 2002. Method 1631, Revision E, "Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry." September 2002. Office of Water, U.S.
Environmental Protection Agency (EPA-B21-R-02-019). The application of clean techniques described in EPA's draft Method 1669: Sampling Ambient Water for Trace Metals at EPA
Water Quality Criteria Levels (EPA-821-R-9S-011) are recommended to preclude contamination at low-level, trace metal determinations.
** Available Cyanide, Method OIA-1677 (Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry), ALPKEM, A Division of Ol Analytical, PO Box 9010. College Station,
TX 77842-9010.
45"Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method", Open File
Report (OFR) 00-170.
•^"Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption
Spectrophotometry", Open File Report (OFR) 93-449.
47 "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry",
Open File Report (QFR) 97-198.
48 "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colori-
metric Finish That Includes Dialysis" Open File Report (OFF)) 92-146,
49 "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Ab-
sorption Spectrometry1' Open File Report (OFRj 98-639.
50 "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical
Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry", Open File Report (QFR) 98-165.
51 "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluviai Sediment", Open File
Report (OFR) 93-125.
TABLE 1C—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS
m
Parameter 1
2. Acenaphthylene
EPA method number2'7
GC | GC/MS
610
610
603
603
610
625 1625B
625, 1625B
624" 1624B
6244, 1624B
625, 1625B
HPLC
610
610
610
Other approved methods
Standard Methods
[Edition(s))
6440 B [18th, 19th,
20thj.
6440 B, 6410 B [18th,
19th, 20th].
6410 B, 6440 B [18th,
19th, 20th].
ASTM
D4657-92
D46S7-92
D4657-92
Other
Note 9, p.27.
Note 9, p.27.
Note 9, p. 27.
5
I
o
1
-------
TABLE 1C—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
an
to
to
Parameter 1
7 Benzidine
10. Benzo(b)fluoranthene
11 Benzo(g, h, i)perylene
1 3 Benzyl chloride
14. Benzyl butyl phthalate
1 5 Bis(2-chloroethoxy) methane
16 Bis(2-chloroethyl) ether
17. Bis(2-ethylhexyl) phthalate
18. Bromodichloromethane
20. Bromomethane
22 Carbon tetrachloride
23 4-Chloro-3-methylphenol
EPA method number 2. v
GC
602
610
610
610
610
610
606
611
611
606
601
601
601
611
601
604
GC/MS
624 1624B
6255 1625B .. .
625, 1625B
625, 1625B
625, 1625B
625, 1625B
625, 1625B
625, 1625B
625, 1625B
625 1625B
625, 1625B
624, 1624B
624 1624B
624, 1624B
625, 1625B
624 1624B
625,16258
HPLC
605 .
610
610
610
610
610
Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th].
6410 B, 6440 B [18th,
19th, 20th].
6410 B, 6440 B [18th,
19th, 20th].
6410 B, 6440 B [181h,
19th, 20th].
6410 B, 6440 B [18th,
19th, 20th].
6410 B, 6440 B [18th,
19th, 20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
6410 B [18th, 19th,
20th].
6200 C [20th] and
6230 B [18th, 19th].
6410 B, 6420 B [18th,
19th, 20th].
ASTM
D4657-92
D4657-92
D4657-92
D4657-92
D4657-92
Other
Note3, p.1.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note3, p 130: Note 6,
p. S102.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 3, p. 130.
Note 9, p. 27.
o
-n
70
O
O
-------
24. Chlorobenzene
25. Chloroethane
26. 2-Chloroethylvinyl ether
27. Chloroform:
28. Chloromethane .
to
CO 30. 2-Chlorophenoi ...
32. Chrysene
36. 1 ,3-Dichlorobenzene
601 602 . .
601
601
601
601
612
604
611
610
610
601
601, 602. 612
601, 602,612
624 1624B ,
624, 1624B
824 1624B
624, 1624B
624, 1624B ....
625 1625B
625 1625B ..
625 1625B
625, 1625B
625 1625B
624 1624B
624 625, 1625B
624, 625, 1625B ..
610
610
6200 B [20th] and
621 OB (18th, 19th],
6200 C [20th] and
6220 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th],.
6200 B [20th] and
6210 B [18th, 19th],
6200 C |20thJ and
6230 B[18th, 19th).
6200 B [20th] and
6210Bl18th, 19th],
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th] and
6210 B[18th, 19th],
6200 C (20th] and
6230 B (18th, 19thj.
6200 B (20th) and
6210 B [18th, 19th]
6200C [20th] and
6230 B [18th, 19th].
6410 B [18th 19th
20th].
6410 B 6420 B [18th
19th, 20th).
6410 B (18th 19th
20th],
6410 B 6440 B [18th
19th, 20th].
6410 B 6440 B [18th
19th, 20th].
6200 B [20th] and
6210 B(18th, 19th]
6200 C [20th] and
6230 B [18th, 19th).
6200 C [20th] and
6220B|1 8th, 19th),
6200 C [20th] and
6230 B [18th, 19th],
6410 B [18th, 19th,
20th].
6200 C (20th] and
6220 B[18th, 19th],
6200 C [20th] and
6230 B (18th, 19th],
6410 B [18th, 19th,
20th].
D4657-92
D4657-92
Note 3 p 130 m
<_
3
»
|r
•o
s
I
Note 3, p 130. §
&
-------
TABLE 1C—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
37. 1 ,4-Dichlorobenzene
38, 3,3-DichforGbenzidine
40. 1 ,1 -Diehloroethane
42 1 1-Dichloroethene ... ..
43, trans-1 ,2-Diehloroethene
48 Diethyl phthalate
EPA method number2 7
GC
601, 602, 612
601
GC/MS
624, 625, 1625B ..
625, 1625B
601 624. 1624B
601
601 ...
601
604
601
601
601
606
624 1624B
624 1624B
624, 1624B
625, 1625B
624, 1624B
624, 1624B
624, 1624B
625 1625B
HPLC
605
Other approved methods
Standard Methods
[Edition(s)]
6200 C [20th] and
6220 B[18th, 19th],
6200 C [20th] and
6230 B [18th, 19th],
6410 B [18th. 19th,
20th}.
6410 B [18th, 19th,
20th].
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
6200 B [20th] and
6210 B [18th, 19thj,
6200 C [20th] and
6230 B [18th, 19th],
6200 B [20th) and
6210 B[18th. 19th],
6200 C [20th] and
6230 B [18th, 19*].
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th],
6410 B, 6420 B [18th,
19th, 20th].
6200 B [20th] and
6210 B [18th, 19th),
8200 C [20th] and
6230 B [18th, 19th).
6200 B [20th] and
6210 B[18th, 19th),
6200 C [20th] and
6230 B [18th, 19th).
6200 B [20th] and
621 OB [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th).
6410 B [18th, 19th,
20th).
ASTM
Other
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Co)
*
f>
"fl
m
O
2
m
Q.
O
-------
to
Ol
49.
50.
51,
52.
53.
54.
55,
56.
57,
60.
61.
62.
63.
65.
68.
67.
68.
69.
70.
71.
72.
73.
75.
76.
77.
2,4-Dimethylphenol ...
Di-n-butyt phthalate
Di-n-octyl phthalate
2,6-Dinitrotoluene
Ethylbenzene ,
123467 8-Heptachloro- dibenzofuran
123478 9-Heptachloro- dibenzofuran
Hexachlorobutadiene
Hexachlorocyclopentadiene
1 ,2,3,6,7,8-Hexacnloro- dibenzofuran
1 ,2,3,7,8,9-Hexachloro- dibenzofuran
2,3,4,6,7,8-Hexachloro- dibenzofuran
1 ,2,3,7,8,9-Hexachloro- dibenzo-p-dioxin
604
606
606
606
604
609
609
602
610
610
612
612
612
616
610
609
601
604
625, 1625B
625 1625B
625, 1625B
625 1625B
625 1625B
625, 16258
625, 1625B
624, 1624B
625 1625B
625 1625B .
1613B
16138
161 38
625 1625B
625, 1625B
5625, 1B25B
1613B
1613B.
1613B.
1613B.
1613B
1613B
1613B.
625 1625B
625 1625B
625 1625B
624 1624B
625, 1625B
610
610
610 .
6410 B 6420 B [18th.
19th, 20th].
6410 B [18th 19th
20th}.
6410 B [18th, 19th,
20thj.
6410 B [18th 19th
20th).
6410 B 6420 B [18th
19th, 20th].
6410 B (18th 19th,
20th].
6410 B [18th, !9th,
20th).
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th],
6410 B 6440 B [18th
19th, 20th],
6410 B 6440 B (18th
19th, 20th].
6410 B [18th 19th
20th],
6410 B [18th, 19th,
2«h],
6410 [18th, 19th, 20th]
6410 B [18th 19th
20th).
6410 B 6440 B [18th
19th, 20th],
6410 B [18th 19th
20th].
6200 C [20th] and
6230 B [18th, 19th],
6420 B 6410 B [18th
19th, 20th].
D4657-92 .
D4657-92 .
Note 9, p. 27.
Note 9, p. 27,
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
] Note 9, p. 27.
j Note3, p, 130, Note 6,
p. S102.
. Note 9, p. 27.
. ! Note 9, p. 27.
i
. Note 9, p, 27.
. Note 9, p. 27.
. Note 9, p. 27.
: Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27.
Note 3, p. 130,
Note 9, p. 27.
I
I
3
B"
-------
TABLE 1C—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter1
78. Naphthalene
80 2-Nitrophenol
81 4-Nitrophenol
82. N-Nitrosodimethylamine . .
87. 2,2'-Oxybis(2-chloropropane) [also known
as bis(2-chloroisopropyl) ether].
88. PCB-1016
89 PCB-1221
90 PCB-1232
91 PCB-1242
92. PCB-1248
93 PCB-1254
94 PCB-1260
95. 1,2,3,7,8-Pentachloro- dibenzofuran
97. 1,2,3,7, 8, -Pentachlorodibenzo-p-dioxin
98. Pentachlorophenol
99. Phenanthrene
100 Phenol
101. Pyrene
EPA method number2-7
GC
610
609
604
604
607
607
607
611
608
608
608
608
608
608
608
604
610
604
610
GC/MS
625, 1625B
625, 1625B
625, 1625B
625 1625B
625=, 1625B
625 1625B
6255, 1625B
1613B.
1613B.
625, 1625B
625
625
625
625
625.
625
625
1613B.
161 3B.
1613B.
625, 1625B
625, 1625B
625, 1625B
625, 1625B
HPLC
610
610
610
Other approved methods
Standard Methods
[Edition(s)]
6440 B, 6410 B [18th,
19th, 20th].
6410 B [18th, 19th,
20th].
6410 B, 6420 B [18th,
19th, 20th].
6410 B, 6420 B [18th,
19th, 20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th],
6410 B [18th, 19th,
20th].
6410 B[18th, 19th,
20th],
6410 B[18th, 19th,
20th].
6410 B[18th, 19th,
20th],
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B, 6630 B [18th,
19th, 20th].
6410 B, 6630 B [18th,
19th, 20th].
641 0 B, 6440 B [18th,
19th, 20th].
6420 B, 6410 B [18th,
19th, 20th].
64408,641 OB
D4675-92 [18th,
19th, 20th].
ASTM
D4657-92
D4657-92
D4675-92
Other
Note 9, p. 27.
Note 9, p. 27.
Note 9, p. 27
Note 9, p. 27
Note 9, p. 27
Note 9, p. 27
Note 9, p. 27
Note 3, p. 43
Note 3, p. 43
Note 3, p. 43
Note 3, p. 43
Note 3, p. 43
Note 3, p. 43
Note3, p. 140; Note 9,
p. 27
Note 9, p. 27
Note 9, p. 27
Note 9, p. 27
an
g
<*>
o
•n
TO
O
O
-------
102. 2,3,7,8-Tetrachloro- dibenzofuran
104 11 2 2-Tetrachloroethane
106 Toluene .
108. 1,1,1-Trichloroethane
112. 2,4,6-Trichlorophenol
1 13 Vinyl chloride
601
601
602
612
601
601
601
601
604
601
1613B.
613 1613B
624 1624B
624 1624B
624, 1624B
625 1625B
624, 1624B
624 1624B
624 1624B
624
625, 1625B
624 1624B
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B[18th, 19th).
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th).
6410 B [18th 19th
20th].
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th).
6200 B [20th] and
6210 B[18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
6420 B, 6410 B [18th,
19th, 20th].
6200 B [20th] and
6210 B [18th, 19th),
6200 C [20th] and
6230 B[18th, 19th).
Note 3 p 130
Note 3, p. 130
Note 3, p. 130; Note 9
p. 27.
Note 3, p. 1 30
Note 9, p. 27.
1.
I
o
s
o
Table 1C notes:
1 All parameters are expressed in micrograms per liter (ng/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/L).
zThe full text of Methods 601-613, 624, 625, 1624B, and 1625B, are given at Appendix A, "Test Procedures for Analysis of Organic Pollutants," of this Part 136. The full text of Method
1613B is incorporated by reference into this Part 136 and is available from the National Technical Information Services as stock number PB95-104774. The standardized test procedure to
be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, "Definition and Procedure for the Determination of the Method Detection Limit," of
this Part 136.
3"Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater," U.S. Environmental Protection Agency, September, 1978.
4 Method 624 may be extended to screen samples for Acrolein and Acrylonitrile. However, when they are known to be present, the preferred method for these two compounds is Method
603 or Method 1624B.
5 Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they are known to be present,
Methods 605, 607, and 612, orMethod 1625B, are preferred methods for these compounds.
""Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency," Supplement to the Fifteenth Edition of Standard Methods for the Examination
of Water and Wastewater (1981).
tffl
W
-------
7Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624B, and 16258 |See Ap-
pendix A of this Part 136) in accordance with procedures each in Section 8-2 of each of these Methods- Additionally, each laboratory, on an on-going basis must spike and analyze 10%
(5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) at all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8,4 of these
Methods, When the recovery oi any parameter fails outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to dem-
onstrate regulatory compliance.
NOTE: These warning limits are promulgated as an "interim final action with a request for comments,"
8"Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk" 3M Corporation Revised 10/28/94.
9USGS Method 0-3116-87 from "Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and
Fluvial Sediments" U.S. Geological Survey, Open File Report 93-125.
TABLE ID—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES"!
Parameter
3, Aminocarb
7. Barban
8. a-BHC
tO 9 B-BHC
10 5-BHC
11. 7~BHC (Lindane)
12, Captan
13 Carbary!
14. Carbophenothion
15. Ghlordane
17. 2,4-D
18. 4,4'-DDD , .
19. 4,4'-DDE
20 44'-DDT
21. Demeton-O
22. Demeton-S
23 Diazinon .....
24. Dicamba
28. Oichloran
Method
GC ..
GC/MS
GC
TLC
GC
GC
GC
TLC
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
TLC
GC
GC
GC/MS
TLC
GC
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
GC
GC
GC
GC .
GC
EPA-'
608
625
608
625s
608
6255
608
625*
608
625
608
625
608
625
608
625
608
62S
Standard Methods
18th, 19th, 20th
Ed.
8830 B & C
6410 B
6630 B&C
6410 B
6630 C .
6410 B.
6630 C
6410 B.
6630 B&C....
6410 B.
6830 B
6830B&C
641 OB,
6640 B
6630 B&C
6410 B
6630 B& C
6410 B.
6630 B&C
6410 B.
6830 B&C
ASTM
03086-90
D3086-90
03086-90
D3086-90
D3086-90
D3086-90
D3086-90
D3086-90
D3086-9Q
D3086-90
Other
Note 3, p. 7- Note 4 p 27- Note 8
Note 3 p 83' Note 6 p S68
Note 3, p 94- Note 6, p. S16
Note 3, p 83' Note 6 p S68
Note 3 p 83- Note 6 p S68- Note 9
Note 3 p 25' Note 6 p SS1
Note 3, p. 104; Note 6, p. S64.
Note 3, p 7; Note 8.
Note 8.
Note 8
Note 3 p 7' Note 4 p 27' Note 8
Note 3 p 7
Note 3 p 94 Note 8 p S60
Note 4, p. 27; Note 6, p. 373.
Note 3, p. 7- Note 4 p 27; Note 8.
Note 3, p 104' Note 6 p S64
Note 3. p. 115; Note 4, p. 40.
Note 3 p 7- Note 4 p 27' Note 8
Note 3, p. 7; Note 4 p 27' Note 8
Note 3 p 7- Note 4 p 27' Note 8
Note 3, p. 25; Note 6, p. SS1.
Note 3, p. 25' Note 6 p S51
Note 3 p 25' Note 4 p 271 Note 6 p
S51.
Note3, p. 115.
Note 4, p. 27' Note 6 p S73
Note 3. p. 7.
o
-n
TO
O
*>.
m
a
-------
27. Dlcofoi
29. Dioxathfon
30. Disulfoton
31. Diuron ........ .
32. Endosulfan I
33. Endosulfan II
34 Endosulfan Sulfate
35. Endrin
36. Endrin aldehyde
37. Ethion
39. Fenuron-TCA
41. Heptaehtor epoxide
42, Isodrin
44. Malathion
48 Mirex
52. Parathion methy!
53 Parathion ethyl
54. PCNB
62. Siduron .
64. Strobane . ........
65 Swep
68. 2.4.5-T
GC
GC
GC/MS
GC
GC
TLC
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
GC/MS
GC
TLC
TLC
GC
GC/MS
GC
GC/MS
GC
GC
GC
TLC
GC
TLC
GC
TLC
TLC
TLC
GC
GC
GC
GC
GC
GC
GC
TLC
TLC
TLC . . .
TLC
GC
GC
TLC
GC
60S
625
608
625s
608
6255
608
625 . .
608
625«
608
625
608
625
608
625
6630 B & C
6410 B.
6630 B & C
6410 B
6630 B&C
6410 B
6630 C
6410B
6630 B&C
6410 B
6630 B&C
6410 B
6630 B & C
6410 B.
6630 C
6630 B&C
6630 B&C
6630 C
6630 C
6630 B&C
6630 B&C
6640 B
D3Q86-90
D3086-90
D3Q86-90
D3086-iO
3086-90
D3086-90
03086-90
D3086-90
Note 3 p ?• Note 4 p 27' Note a
Note 4, p. 27; Note 6, p. S73.
Note 3, p. 25; Note 6 p. S51.
Note 3 p. 104 Note 6 p S64
Note 3, p. 7; Note 4, p. 27; Note 8.
Note 3, p. 7; Note 8.
Note 8
Note 3, p. 7; Note 4. p. 27; Note B.
Note 8.
Note 4, p. 27; Note 6, p. 873.
Note 3, p. 104- Note 6 p S64
Note 3, p. 104- Note 6, p. S64.
Note 3 p 7' Note 4 p 27- Note 8
Note 3, p. 7; Note 4, p. 27; Note 6, p. S73;
Note 8.
Note 4, p 27; Note 6 p S73
Note 3, p. 104; Note 6, p. S64.
Note 3, p. 25- Note 4 p 27' Note 8 p S51
Note 3, p. 94; Nota 6, p. S60.
Note 3, p. 7- Note 4 p 27- Note 8
Note 3, p. 94; Note 6, p. S60.
Note 3 p 7' Note 4 p 27
Note 3, p. 104' Note 8 p S64
Note 3 p 104' Note 6 p S64
Note 3, p 104- Note 6 p S64
Note 3, p. 25; Note 4, p. 27.
Note 3 p 25* Note 4 p 27
Note 3, p 7,
Note 4 p 27
Note 3, p 83; Note 6 p S68; Note 9
Note 3 p 83" Note 6 p S68' Note 9
Note 3 p. 83' Note 6 p S68- Note 9
Note 3, p. 104; Note 6, p. S64.
Note 3 p 94' Note 6 p S60
Note 3 p. 83- Note 6 p S6S
Note 3, p. 104; Note 6, p. S84.
Note 3, p. 83' Note 6 p S68' Note 9
Note 3, p. 7
Note 3 p 104' Note 6 p S64
Note 3. o. 115: Note 4. o. 40.
3
3
-------
TABLE ID—List OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued
CO
o
Parameter
67. 2 4,5-TP (Silvex) ..
70. Trifiuralin
Method
GC
GC .. .
GC ,
GC/MS
GC
EPA"
608
625
Standard Methods
18th, 19th, 20th ASTM
Ed.
6640 B
6630 B & C D3086 — 90
6410B.
6630 B
Other
Note 3, p. 115: Note 4, p. 40.
Note 3, p. 83; Note 6 p S68
Note 3 p 7- Note 4 p 27- Note 8
Note 3. D. 7: Note 9.
Table ID notes:
1 Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, where entries are listed by chemical name.
2 The full text of Methods 808 and 625 are given at Appendix A. 'Test Procedures tor Analysis of Organic Pollutants," of this Part 136- The standardized test procedure to be used to de-
termine the method detection limit (MDL) for these test procedures is given at Appendix B, "Definition and Procedure for the Determination of the Method Detection Limit," of this Part 136.
3£*Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater," U.S. Environmental Protection Agency, September 1978, This
EPA publication includes thin-layer chromatography (TLC) methods.
4 "Methods for Analysis of Organic Substances in Water and Fluvial Sediments," Techniques of Water-Resources Investigations of the U.S, Geological Survey, Book 5, Chapter A3 (1987).
5 The method may be extended to include a-BHC, y-BHC, endosutfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.
^"Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency." Supplement to the Fifteenth Edition of Standard Methods for the Examination
of Water and Wastewater (1981).
7 Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 (See Appendix A of this Part 136) in
accordance with procedures given in Section 8,2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 10% of all samples analyzed with
Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of
any parameter fails outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory compliance.
These quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
Note: These warning limits are promulgated as an "Interim final action with a request for comments,"
a"Organ0chiorine Pesticides and PCBs in Wastewater Using Empore™ Disk", 3M Corporation, Revised 10/28/94.
SUSGS Method 0-3106-93 from "Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Triazine and Other Nitrogen-containing Com-
pounds by Gas Chromatography with Nitrogen Phosphorus Detectors" U.S. Geologicai Survey Open File Report 94-37.
TABLE IE—LIST OF APPROVED RAOIOLOGIC TEST PROCEDURES
Parameter and units
1. Alpha-Total, pCi per liter
2. Alpha-Counting error, pCi per liter .
3, Beta-Total, pCi per liter
4. Beta-Counting error. pCi
5, (a) Radium Total pCi per liter .,.
(b) Ra, pCi per liter
Table 1E notes:
1 "Prescribed Procedures for Measu
2Fishman, M.J. and Brown, Eugene
3The method found on p. 75 measi
"total".
Method
Proportional or scintiliation counter
Proportional or scintillation counter
Proportional counter
Proportional counter
Scintillation counter
Reference (method number or page)
EPA1
900
Appendix B
900,0
Appendix B
903,0
903,1
Standard Methods
18th. 19th, 20th Ed.
7110 B
7110 B
7110 B
7110 B
7500Ra B
7500Ha C
ASTM
D 1943-90
D1 943-90
D1 890-90
D1 890-90
D2460-9Q
D3454-91
USGSZ
pp. 75 and 78 3
p. 79
pp. 75 and 78 3
p. 79
p. 81
of Radioactivity in Drinking Water," EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.
=ted Methods of the U.S. Geological Survey of Analysis ot Wastewaters," U.S- Geological Survey, Open-File Report 76-177 (1978).
y the dissolved portion while the method on p 78 measures only the suspended portion. Therefore, the two results must be added to obtain the
o
•n
;o
O
o
-------
Environmental Protection Agency
§136.3
TABLE IF—LIST OF APPROVED METHODS FOR PHARMACEUTICAL POLLUTANTS
Pharmaceuticals pollutants
tert-butyl alcohol
n-heptane ....
Methyl Cellosolve a
methylene chloride
4-methyl"2-pentanone (MIBK)
2-propanone (acetone)
triethlyamine
xvlenes .
CAS registry hfo.
75-05-8
623-63-7
71^11-0
71_43_2
123-86-4
75-65-0
108-90-7
67-66-3
95-50-1
•) 07-06-2
} 09-89-7
67-68-5
84-17-5
141-78-6
142-82-5
110-54-3
78-84-2
67-63-0
108-21-4 ....
108-20-3
67-56-1
109-86-4
75-09-2
107-31-3 ....
10S-10-1
108-95-2
71-23-8
67-64-1
109-99-9
108-88-3
121^*4-8
(Note 11
Analytical method number
1 666/1 671/D3371 /D3695
1 666/D3695
1666/D3695
D4763/D3695/502 2/524 2
1866/D3895.
1666.
502 2/524 2
502 2/524, 2/551 .
1625C/502.2/524.2.
D3695/502 2/524 2
1666/1671
1666/1671
1666/1671/D3695.
1666/D3685.
1666/D369S.
1666/D3695.
1666/1667.
1 666/D3695
1 666/D3695
1666/D3695
1666/1 671 /D3695.
1666/1671
502.2/524.2
1666
1 624C/1 666/D368&D4763/524 2
D4763.
1666/1 671. '03695
D3695/D4763/524.2.
1666/5242
D3695/D4763/502.2/524.2
1666/1671.
1624C/1666.
Table IF note:
1. 1624C: m-xylene 108-38-3, o,p-xylene E-14095 (Not & CAS number; this is the number provided in the Environmental
Monitoring Methods Index (EMMI) database.); 1666: rn,p-xylene 136777-61-2, o-xylene 95^17-6.
(b) The full texts of the methods from
the following references which are
cited in Tables IA, IB, 1C, ID, IE,and IP
are incorporated by reference into this
regulation and may be obtained from
the sources identified. All costs cited
are subject to change and must be
verified from the indicated sources.
The full texts of all the test procedures
cited are available for inspection at the
National Exposure Research Labora-
tory, Office of Research and Develop-
ment, U.S. Environmental Protection
Agency, 26 West Martin Luther King
Dr., Cincinnati, OH and the Na-
tional Archives and Records Adminis-
tration (NARA). For information on
the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archwes.gov/fedeTal register/
code of federal regulations/
ibr locations .html.
REFERENCES, SOURCES, COSTS, AND
TABLE CITATIONS:
(1) The full texts of Methods 601-613,
624, 625, 1613, 1624, and 1625 are printed
in appendix A of this part 136. The full
text for determining the method detec-
tion limit when using the test proce-
dures is given in appendix B of this
part 136. The full text of Method 200,7 is
printed in appendix C of this part 136.
Cited in: Table IB, Note 5; Table 1C,
Note 2; and Table ID, Note 2.
(2) USEPA. 1978. Microbiological
Methods for Monitoring the Environ-
ment, Water, and Wastes. Environ-
mental Monitoring and Support Lab-
oratory, U.S. Environmental Protec-
tion Agency, Cincinnati, Ohio. EPA/600/
8-78/017. Available from: National Tech-
nical Information Service, 5285 Port
Royal Road, Springfield. Virginia 22161,
Publ. No. PB-290329/AS. Cost: $36.95.
Table IA, Note 3.
(3) "Methods for Chemical Analysis of
Water and Wastes," U.S. Environ-
mental Protection Agency, EPA-600/4-
31
-------
§136.3
40 CFR Ch. I (7-1-04 Edition)
79-020, March 1979, or "Methods for
Chemical Analysis of Water and
Wastes," U.S. Environmental Protec-
tion Agency, EPA-600/4-79-020, Revised
March 1983. Available from: OBD Publi-
cations, CERI, U.S. Environmental
Protection Agency, Cincinnati, Ohio
45268, Table IB, Note 1.
(4) "Methods for Benzidine,
Chlorinated Organic Compounds,
Pentachlorophenol and Pesticides in
Water and Wastewater," U.S. Environ-
mental Protection Agency, 1978. Avail-
able from: ORD Publications, CERI,
U.S. Environmental Protection Agen-
cy, Cincinnati, Ohio 45268, Table 1C,
Note 3; Table D, Note 3.
(5) "Prescribed Procedures for Meas-
urement of Radioactivity in Drinking
Water," U.S. Environmental Protection
Agency, EPA-600/4-8(M)32, 1980. Avail-
able from: ORD Publications, CERI,
U.S. Environmental Protection Agen-
cy, Cincinnati, Ohio 45268, Table IE,
Note 1.
(6) American Public Health Associa-
tion. 1992, 1995, and 1998. Standard
Methods for the Examination of Water
and Wastewater. 18th, 19th, and 20th
Edition (respectively). Available from:
Amer. Publ. Hlth. Assoc., 1015 15th
Street, NW., Washington, DC 20005.
Table IA, Note 4. Tables IB, 1C, ID, IE.
(7) Ibid, 15th Edition, 1980. Table IB,
Note 30; Table ID.
(8) Ibid, 14th Edition, 1975. Table IB,
Notes 17 and 27.
(9) "Selected Analytical Methods Ap-
proved and Cited by the United States
Environmental Protection Agency,"
Supplement to the 15th Edition of
Standard Methods for the Examination
of Water and Wastewater, 1981. Avail-
able from: American Public Health As-
sociation, 1015 Fifteenth Street NW.,
Washington, DC 20036. Cost available
from publisher. Table IB, Note 10;
Table 1C, Note 6; Table ID, Note 6.
(10) Annual Book of ASTM Stand-
ards, Water, and Environmental Tech-
nology, Section 11, Volumes 11.01 and
11.02, 1994, 1996, 1999, and Volume 11.02,
2000 in 40 CFR 136.3, Tables IA, IB, 1C,
ID, and IE.
(11) USGS. 1989. U.S. Geological Sur-
vey Techniques of Water-Resources In-
vestigations, Book 5, Laboratory Anal-
ysis, Chapter A4, Methods for Collec-
tion and Analysis of Aquatic Biological
and Microbiological Samples, U.S. Geo-
logical Survey, U.S. Department of the
Interior, Reston, Virginia. Available
from: USGS Books and Open-File Re-
ports Section, Federal Center, Box
25425, Denver. Colorado 80225. Cost:
$18.00. Table IA, Note 5.
(12) "Methods for Determination of
Inorganic Substances in Water and
Fluvial Sediments," by M.J. Fishman
and Linda C. Friedman, Techniques of
Water-Resources Investigations of the
U.S. Geological Survey, Book 5 Chapter
Al (1989). Available from: U.S. Geologi-
cal Survey, Denver Federal Center, Box
25425, Denver, CO 80225. Cost: $108.75
(subject to change). Table IB, Note 2.
(13) "Methods for Determination of
Inorganic Substances in Water and
Fluvial Sediments," N.W. Skougstad
and others, editors. Techniques of
Water-Resources Investigations of the
U.S. Geological Survey, Book 5, Chap-
ter Al (1979). Available from: U.S. Geo-
logical Survey, Denver Federal Center,
Box 25425, Denver, CO 80225. Cost: $10.00
(subject to change), Table IB, Note 8.
(14) "Methods for the Determination
of Organic Substances in Water and
Fluvial Sediments," Wershaw, R.L., et
al, Techniques of Water-Resources In-
vestigations of the U.S. Geological Sur-
vey, Book 5, Chapter A3 (1987). Avail-
able from: U.S. Geological Survey,
Denver Federal Center, Box 25425, Den-
ver, CO 80225. Cost: $0.90 (subject to
change). Table IB, Note 24; Table ID,
Note 4.
(15) "Water Temperature—Influential
Factors, Field Measurement and Data
Presentation," by H.H. Stevens, Jr., J.
Ficke, and G.F. Smoot, Techniques of
Water-Resources Investigations of the
U.S. Geological Survey, Book 1, Chap-
ter Dl, 1975. Available from: U.S. Geo-
logical Survey, Denver Federal Center,
Box 25425, Denver, CO 80225. Cost: $1.60
(subject to change). Table IB, Note 32.
(16) "Selected Methods of the U.S. Ge-
ological Survey of Analysis of
Wastewaters," by M.J. Fishman and
Eugene Brown; U.S. Geological Survey
Open File Report 76-77 (1976). Available
from: U.S. Geological Survey, Branch
of Distribution, 1200 South Eads Street,
Arlington, VA 22202. Cost: $13.50 (sub-
ject to change). Table IE, Note 2.
(17) "Official Methods of Analysis of
the Association of Official Analytical
32
-------
Environmental Protection Agency
§136.3
Chemicals", Methods manual, 15th Edi-
tion (1990). Price: $240.00. Available
from: The Association of Official Ana-
lytical Chemists, 2200 Wilson Boule-
vard. Suite 400, Arlington, VA 22201.
Table IB, Note 3.
(18) "American National Standard on
Photographic Processing Effluents,"
April 2, 1975. Available from: American
National Standards Institute, 1430
Broadway, New York, New York 10018.
Table IB, Note 9.
(19) "An Investigation of Improved
Procedures for Measurement of Mill Ef-
fluent and Receiving Water Color,"
NCASI Technical Bulletin No. 253, De-
cember 1971. Available from: National
Council of the Paper Industry for Air
and Stream Improvements, Inc., 260
Madison Avenue, New York, NY 10016.
Cost available from publisher. Table
IB, Note 18.
(20) Ammonia, Automated Electrode
Method, Industrial Method Number
379-75WE, dated February 19, 1976.
Technicon Auto Analyzer II. Method
and price available from Technicon In-
dustrial Systems, Tarrytown, New
York 10591. Table IB, Note 7.
(21) Chemical Oxygen Demand, Meth-
od 8000, Hach Handbook of Water Anal-
ysis, 1979. Method price available from
Hach Chemical Company, P.O. Box 389,
Loveland, Colorado 80537. Table IB,
Note 14.
(22) QIC Chemical Oxygen Demand
Method, 1978. Method and price avail-
able from Oceanography International
Corporation, 512 West Loop, P.O. Box
2980, College Station, Texas 77840.
Table IB, Note 13.
(23) ORION Research Instruction
Manual, Residual Chlorine Electrode
Model 97-70, 1S77. Method and price
available from ORION Research Incor-
poration, 840 Memorial Drive, Cam-
bridge, Massachusetts 02138. Table IB,
Note 16.
(24) Bicinehonmate Method for Cop-
per. Method 8506, Hach Handbook of
Water Analysis, 1979, Method and price
available from Hach Chemical Com-
pany. P.O. Box 300, Loveland, Colorado
80537. Table IB, Note 19.
(25) Hydrogen Ion (pH) Automated
Electrode Method, Industrial Method
Number 378-75WA. October 1976. Bran &
Luebbe (Technicon) Auto Analyzer II.
Method and price available from Bran
& Luebbe Analyzing Technologies, Inc.
Elmsford, N.Y. 10523. Table IB, Note 21.
(26) 1,10-Phenanthroline Method
using FerroVer Iron Reagent for Water,
Hach Method 8008, 1980. Method and
price available from Hach Chemical
Company, P.O. Box 389 Loveland, Colo-
rado 80537. Table IB, Note 22.
(27) Periodate Oxidation Method for
Manganese, Method 8034, Hach Hand-
book for Water Analysis, 1979. Method
and price available from Hach Chem-
ical Company. P.O. Box 389, Loveland.
Colorado 80537. Table IB, Note 23.
(28) Nitrogen, Nitrite—Low Range,
Diazotization Method for Water and
Wastewater, Hach Method 8507, 1979.
Method and price available from Hach
Chemical Company, P.O. Box 389,
Loveland, Colorado 80537. Table IB,
Note 25.
(29) Zincon Method for Zinc, Method
8009. Hach Handbook for Water Anal-
ysis, 1979. Method and price available
from Hach Chemical Company, P.O.
Box 389, Loveland, Colorado 80537.
Table IB, Note 33.
(30) "Direct Determination of Ele-
mental Phosphorus by Gas-Liquid
Chromatography," by R.F. Addison and
R.Q. Ackman, Journal of Chroma-
tography, Volume 47, No. 3, pp. 421-426,
1970. Available in most public libraries.
Back volumes of the Journal of Chro-
matography are available from
Elsevier/North-Holland, Inc., Journal
Information Centre, 52 Vanderbilt Ave-
nue, New York, NY 10164. Cost avail-
able from publisher. Table IB, Note 28.
(31) "Direct Current Plasma (DCP)
Optical Emission Spectrometric Meth-
od for Trace Elemental Analysis of
Water and Wastes", Method AES 0029,
1986-Revised 1991, Fison Instruments,
Inc., 32 Commerce Center, Cherry Hill
Drive. Danvers, MA 01923. Table B,
Note 34.
(32) "Closed Vessel Microwave Diges-
tion of Wastewater Samples for Deter-
mination of Metals, OEM Corporation,
P.O. Box 200, Matthews, North Carolina
28106-0200, April 16, 1992. Available from
the OEM Corporation. Table IB, Note
36.
(33) "Organochlorine Pesticides and
PCBs in Wastewater Using Empore ™
Disk" Test Method 3M 0222, Revised 10/
28/94. 3M Corporation, 3M Center Build-
ing 220-9E-10, St. Paul. MN 55144-1000.
33
-------
§136.3
40 CFR Ch, I (7-1-04 Edition)
Method available from 3M Corporation.
Table 1C, Note 8 and Table ID, Note 8.
(34) USBPA. October 2002. Methods
for Measuring the Acute Toxicity of
Effluents and Receiving Waters to
Freshwater and Marine Organisms.
Fifth Edition, U.S. Environmental Pro-
tection Agency, Office of Water, Wash-
ington, DC EPA 821-R-02-012. Available
from: National Technical Information
Service, 5285 Port Royal Road, Spring-
field, Virginia 22161, Pub. No. PB2Q02-
108488. Table IA, Note 29.
(35) "Nitrogen, Total Kjeldabl, Meth-
od PAI-DK01 (Block Digestion, Steam
Distillation, Titrlmetric Detection)",
revised 12/22/94. Available from
Perstorp Analytical Corporation, 9445
SW Bidder Rd., Suite 310, P.O. Box 648,
Wilsonville, OK 97070. Table IB, Note
39.
(36) "Nitrogen, Total Kjeldahl, Meth-
od PAI-DK02 (Block Digestion, Steam
Distillation, Colorimetric Detection)",
revised 12/22/94. Available from
Perstorp Analytical Corporation, 9445
SW Ridder Rd.. Suite 310, P.O. Box 648.
Wilsonville, OK 97070, Table IB, Note
40,
(37) "Nitrogen, Total Kjeldahl, Meth-
od PAI-DK03 (Block Digestion, Auto-
mated FIA Gas Diffusion)", revised 12/
22/94. Available from Perstorp Analyt-
ical Corporation, 9445 SW Ridder Rd.,
Suite 310, P.O. Bos 848, Wilsonville, OK
97070. Table IB, Note 41.
(38) USEPA. October 2002. Short-
Term Methods for Measuring the
Chronic Toxicity of Effluents and Re-
ceiving Waters to Freshwater Orga-
nisms. Fourth Edition. U.S. Environ-
mental Protection Agency, Office of
Water, Washington, DC EPA-821-R-02-
013. Available from: National Technical
Information Service, 5285 Port Royal
Road, Springfield, Virginia 22161, Pub.
No. PB2002-108489. Table I A, Note 30.
(39) USEPA. October 2002. Short-
Term Methods for Measuring the
Chronic Toxicity of Effluents and Re-
ceiving Waters to Marine and Estua-
rine Organisms. Third Edition. U.S.
Environmental Protection Agency, Of-
fice of Water, Washington, DC EPA-
821-R-02-014. Available from; National
Technical Information Service, 5285
Port Royal Road, Springfield, Virginia
22161, Pub. No. PB2002-108490. Table IA,
Note 31.
(40) EPA Methods 1666, 1667, and 1671
listed in the table above are published
in the compendium titled Analytical
Methods for the Determination of Pol-
lutants in Pharmaceutical Manufac-
turing Industry Wastewaters (EPA 821-
B-88-016). EPA Methods 502.2 and 524.2
have been incorporated by reference
into 40 CFR 141.24 and are in Methods
for the Determination of Organic Com-
pounds in Drinking- Water, EPA-600/4-
88-039, December 1988, Revised, July
1991, and Methods for the Determina-
tion of Organic Compounds in Drinking
Water-Supplement II, EPA-600/R-92-
129, August 1992, respectively. These
EPA test method compendia are avail-
able from the National Technical Infor-
mation Service, NTIS PB91-231480 and
PB92-207703, U.S. Department of Com-
merce, 5285 Port Royal Road, Spring-
field, Virginia 22161, The toll-free num-
ber is 800-553-6847. ASTM test methods
D3371, D3695, and D4763 are available
from the American Society for Testing
and Materials, 100 Barr Harbor Drive,
West Conshohocken, PA 19428-2959,
(41) USEPA. 2002. Method 1631, Revi-
sion E, "Mercury in Water by Oxida-
tion, Purge and Trap, and Cold Vapor
Atomic Fluorescence Spectrometry."
September 2002. Office of Water, U.S.
Environmental Protection Agency
(EPA-821-RT-02-019). Available from:
National Technical Information Serv-
ice, 5285 Port Royal Road, Springfield,
Virginia 22161. Publication No. PB2002-
108220. Cost: $25.50 (subject to change).
(42) [Reserved]
(43) Method OTA-1677, Available Cya-
nide by Flow Injection, Ldgand Ex-
change, and Amperometry. August
1999. ALPKEM, OI Analytical, Box 648,
Wilsonville, Oregon 97070 (EPA-821-R-
99-013). Available from: National Tech-
nical Information Service, 5285 Port
Royal Road, Springfield, Virginia 22161.
Publication No. PB99-132011. Cost:
$22.50. Table IB, Note 44.
(44) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory Determination of
Ammonium Plus Organic Nitrogen by a
Kjeldahl Digestion Method and an
Automated Photometric Finish that
Includes Digest Cleanup by Gas Diffu-
sion", Open File Report (OFR) 00-170.
34
-------
Environmental Protection Agency
§136.3
Available from: U.S. Geological Sur-
vey, Denver Federal Center, Box 25425,
Denver, CO 80225. Table IB, Note 45.
(45) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Chromium in Water by Graphite Fur-
nace Atomic Absorption
Spectrophotometry", Open File Report
(OPR) 93-449. Available from: U.S. Geo-
logical Survey, Denver Federal Center,
Box 25425, Denver. CO 80225. Table IB,
Note 46.
(46) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Molybdenum in Water by Graphite
Furnace Atomic Absorption
Spectrophotometry". Open File Report
(OFR) 97-198. Available from: U.S. Geo-
logical Survey, Denver Federal Center,
Box 25425, Denver, CO 80225. Table IB.
Note 47.
(47) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Total Phosphorus by Kjeldahl Diges-
tion Method and an Automated Colori-
metric Finish That Includes Dialysis"
Open File Report (OFR) 92-146. Avail-
able from: U.S. Geological Survey,
Denver Federal Center, Box 25425, Den-
ver, CO 80225. Table IB, Note 48.
(48) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Arsenic and Selenium in Water and
Sediment by Graphite Furnace—Atom-
ic Absorption Spectrometry" Open File
Report (OFR) 98-639. Table IB, Note 49.
(49) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Elements in Whole-Water Digests
Using Inductively Coupled Plasma-Op-
tical Emission Spectrometry and In-
ductively Coupled Plasma-Mass Spec-
trometry" , Open File Report (OFR) 98-
165. Available from: U.S. Geological
Survey, Denver Federal Center, Box
25425, Denver, CO 80225. Table IB, Note
50.
(50) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Triazine and Other Nitrogen-con-
taining Compounds by Gas Chroma-
tography with Nitrogen Phosphorus
Detectors" U.S.Geological Survey Open
File Report 94-37. Available from: U.S.
Geological Survey, Denver Federal
Center, Box 25425, Denver, CO 80225.
Table ID, Note 9.
(51) "Methods of Analysis by the U.S.
Geological Survey National Water
Quality Laboratory—Determination of
Inorganic and Organic Constituents in
Water and Fluvial Sediments", Open
File Report (OFR) 93-125. Available
from: U.S. Geological Survey, Denver
Federal Center, Box 25425. Denver. CO
80225. Table IB, Note 51; Table 1C, Note
9.
(52) IDEXX Laboratories, Inc. 2002.
Description of Colilert®, Colilert-18®",
Quanti-Tray®, Quanti-Tray®/2000,
Bnterolert® methods are available
from IDBXX Laboratories, Inc., One
Idexx Drive, Westbrook, Maine 04092.
Table IA, Notes 17 and 23.
(53) Hach Company, Inc. Revision 2,
1999. Description of m-ColiBlue24®
Method, Total Coliforms and E. coli, is
available from Hach Company, 100 Day-
ton Ave., Ames, IA 50010. Table IA,
Note 18.
(54) USEPA. 2002. Method 1103.1: Esch-
erichia coli (E. coli) in Water by Mem-
brane Filtration Using membrane-
Thermotolerant Escherichia coli Agar
(mTEC). U.S. Environmental Protec-
tion Agency, Office of Water, Wash-
ington D.C. September 2002, EPA-821-
R-02-020. Available at NTIS, PB2003-
100125. Table IA, Note 20.
(55) USEPA. 2002. Method 1106.1:
Enterococci in Water by Membrane
Filtration Using membrane-
Enterococcus-Esculin Iron Agar (mE-
EIA). U.S. Environmental Protection
Agency. Office of Water. Washington
D.C. September 2002, EPA-821-R-02-021.
Available at NTIS, PB2003-100126. Table
IA, Note 24.
(56) USEPA. 2002. Method 1603: Esch-
erichia coli (E. coli) in Water by Mem-
brane Filtration Using Modified mem-
brane-Thermotolerant Escherichia coli
Agar (Modified mTEC). U.S. Environ-
mental Protection Agency, Office of
Water, Washington, DC September 2002,
EPA-821-R-02-023. Available at NTIS.
PB2003-100128. Table IA, Note 21.
(57) Brenner et al. 1993. New Medium
for the Simultaneous Detection of
Total Coliforms and Escherichia coli in
Water. Appl, Environ. Microbiol. 59:3534-
35
-------
§136,3
40 CFR Ch. I (7-1-04 Edition)
3544. Available from the American So-
ciety for Microbiology, 1752 N Street
NW,, Washington, DC 20036. Table IA,
Note 22.
(58) USBPA. 2002. Method 1604: Total
Coliforms and Escherichia coli (E, coli)
in Water by Membrane Filtration using
a Simultaneous Detection Technique
(MI Medium). U.S. Environmental Pro-
tection Agency, Office of Water, Wash-
ington D.C.. September 2002, EPA 821-
R-02-024. Available from NTIS, PB2003-
100129. Table IA, Note 22.
(59) USBPA. 2002. Method 1600:
Enterococci in Water by Membrane
Filtration using membrane-
Enterococcus Indoxyl-p-D-Glucoside
Agar (mEI). U.S. Environmental Pro-
tection Agency, Office of Water, Wash-
ington B.C. September 2002, EPA-821-
R^02-022. Available from NTIS, PB2003-
100127. Table IA, Note 25.
(60) USBPA. 2001. Method 1622:
Cryptosporidium in Water by Filtration/
IMS/FA. U.S. Environmental Protec-
tion Agency, Office of Water, Wash-
ington, DC April 2001, EPA-821-R-01-
026.
Available from NTIS, PB2Q02-1087Q9.
Table IA, Note 26.
(61) USEPA. 2001. Method 1623:
Cryptosporidium and Giardia in Water
by Filtration/IMS/FA. U.S. Environ-
mental Protection Agency, Office of
Water, Washington, DC April 2001,
EPA-«21-R-01-025. Available from
NTIS. PB2002^108710. Table IA. Note 27.
(62) AOAC. 1995. Official Methods of
Analysis of AOAC International, 16th
Edition, Volume I, Chapter 17. AOAC
International. 481 North Frederick Av-
enue, Suite 500, Gaithersburg, Mary-
land 20877-2417. Table IA, Note 11.
(c) Under certain circumstances the
Regional Administrator or the Director
in the Region or State where the dis-
charge will occur may determine for a
particular discharge that additional
parameters or pollutants must be re-
ported. Under such circumstances, ad-
ditional test procedures for analysis of
pollutants may be specified by the Re-
gional Administrator, or the Director
upon the recommendation of the Direc-
tor of the Environmental Monitoring
Systems Laboratory—Cincinnati.
(d) Under certain circumstances, the
Administrator may approve, upon rec-
ommendation by the Director, Envi-
ronmental Monitoring Systems Lab-
oratory—Cincinnati, additional alter-
nate test procedures for nationwide
use.
(e) Sample preservation procedures,
container materials, and maximum al-
lowable holding times for parameters
cited in Tables IA, IB, 1C, ID, and IB
are prescribed in Table II. Any person
may apply for a variance from the pre-
scribed preservation techniques, con-
tainer materials, and maximum hold-
ing times applicable to samples taken
from a specific discharge. Applications
for variances may be made by letters
to the Regional Administrator in the
Region in which the discharge will
occur. Sufficient data should be pro-
vided to assure such variance does not
adversely affect the integrity of the
sample. Such data will be forwarded,
by the Regional Administrator, to the
Director of the Environmental Moni-
toring Systems Laboratory—Cin-
cinnati, Ohio for technical review and
recommendations for action on the
variance application. Upon receipt of
the recommendations from the Direc-
tor of the Environmental Monitoring
Systems Laboratory, the Regional Ad-
ministrator may grant a variance ap-
plicable to the specific charge to the
applicant. A decision to approve or
deny a variance will be made within 90
days of receipt of the application by
the Regional Administrator.
TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES
Parameter No./name
Table SA— Bacteria Tests:
1-5 Coliform, total, fecal, and E call ...............
Table IA— Protozoa Tests:
Table 1A — Aquatic Toxicity Tests:
6-10 Toxicttv, acute and chronic
Container •
PP, e
PP, G
PP, G
LOPE
LOPE
P.G
Preservation2-3
Cool, <10 °C, 0.0008%
Na2S2O,s.
Cool, <1 0° 0.0008% Na2SiCM
Cool,
-------
Environmental Protection Agency § 136.3
TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Parameter No./name
Container n
Preservation2'3
Maximum holding time4
Table IB — Inorganic Tests:
1 Acidity
2 Alkalinity
10 Boron
14. Biochemical oxygen demand, carbonaceous
17. Chlorine, total residual
21 Color
chlorination.
25. Fluoride
31 43 Kjetdahl and organic nitrogen
Metals:7
18 Chromium VI7
35 Mercury17
3 5-8 1213 19 20 22 26 29 30 32-34
36, 37, 45, 47, 51, 52, 58-60, 62, 63, 70-72,
74, 75. Metals except boron, chromium VI
and mercury7.
38 Nitrate
40 Nitrite
41 Oil and grease
42. Organic Carbon
44 Orthophosphate
47 Winkler
48 Phenols
50 Phosphorus total
53. Residue, total
54 Residue Filterable
55 Residue, Nonfilterable (TSS)
56 Residue, Settleable
57 Residue volatile
61 Silica
65 Sulfate
66. Sulfide
67 Sulfite
73 Turbidity
Table 1C— Organic Tests8
13, 18-20, 22, 24-28, 34-37, 39-43, 45-47,
56, 76, 104, 105, 108-111, 113. Purgeable
Halocarbons.
6, 57, 106. Purgeable aromatic hydrocarbons ...
3, 4. Acrolein and acrylonitrile
23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112.
Phenols".
7 38 Benzidines"
14 17 48 50-52. Phthalate esters "
p G
P G
P G
p, G
P PFTE or
Quartz.
P G
P, G
p G
P G
P, G
P G
P G
P
P G
P G
P, G
P G
P, G
P G
P G
P, G
P G
G
P, G
P, G
G Bottle and
top.
do
G only
G
P, G
P, G
P, G
P, G
P, G
P G
P PFTE or
Quartz.
P G
P, G
P, G
p, G
P G
P G
P, G
G, Teflon-
lined sep-
tum,
do
do
G, Teflon-
lined cap..
do
do
Cool, 4°C
do
Cool 4°C HiSO4 to pH<2
Cool, 4°C
HNOiTOpH<2
Cool, 4°C
Cool, 4°C, H2SO4 to pH<2
do
Cool 4°C
Cool 4°C NaOH to pH>12
0.6g ascorbic acid 5.
None required
HNOi to pH<2, H2SO4 to pH<2
Cool, 4°C, H,SO4 to pH<2
Cool 4 °C
HNOitopH<2
do
Cool 4°C
Cool, 4°C, H2SO4 to pH<2
Cool 4°C ...
Cool to 4°C, HCI or H2SO4 to
pH<2.
Cool to 4 °C HC1 or H2SO4 or
H3PO4, to pH<2.
Filter immediately, Cool, 4°C ...
Cool, 4°C, HiSO4 to pH<2
Cool 4°C
Cool, 4°C, H2SO4 to pH<2
Cool, 4°C
do
do
do
do
Cool 4 °C
do
do
Cool, 4°C add zinc acetate
plus sodium hydroxide to
pH>9.
None required
Cool 4°C
Cool, 4°C
Cool, 4 °C, 0.008% Na2S2O35.
Cool, 4 °C, 0.008% Na2S2Oi,5
HCI to pH29.
Cool, 4 °C, 0.008% Na2S,O,,5
adjust pH to 4-5'°.
Cool, 4 °C, 0.008% Na2S2O,5
... .do
Cool, 4 °C
14 days.
Do.
28 days.
48 hours.
6 months.
28 days.
48 hours.
28 days.
Do.
Analyze immediately.
48 hours.
14 days.'
28 days.
6 months.
Analyze immediately.
28 days.
24 hours.
28 days.
6 months.
48 hours.
28 days.
48 hours.
28 days.
28 days.
48 hours.
Analyze immediately.
8 hours.
28 days.
48 hours.
28 days.
7 days.
7 days.
7 days.
48 hours.
7 days.
28 days.
Do.
Do.
7 days.
Analyze immediately.
48 hours.
Analyze.
48 hours.
14 days.
Do.
Do.
7 days until extraction;
40 days after extrac-
tion.
7 days until extraction.11
7 days until extraction;
40 days after extrac-
tion.
37
-------
§136.3
40 CFR Ch. I (7-1-04 Edition)
TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AMD HOLDING TIMES—Continued
Parameter No./narne
82-84. Nitrosamines '•
88-94. RGBs" .........
Container1
54, 55, 75, 70. Nitroaromatics
isophoroneH, •
i 2, 5, 8-12, 32, 33, 58, 59, 74f 78, 09, 101. | ......do
Poiynuclear aromatic hydrocarbons !i.
15, 16, 21, 31, 87, Haioethers
29, 35-37, 63-65, 73, 107, Chlorinated hydro-
carbons u.
60-62, 66-72, 85, 86, 95-97, 102, 103, GDDs/
CDFs'i.
aqueous: field and lab preservation. ,,.,,...,...
Solids, mixed phase, and tissue; field preserva-
tion..
Solids, mixed phase, and tissue: lab preserva-
tion.
Table ID—Pesticides Tests:
1-70, Pesticides11
Table IE—Radiological Tests;
1-5- Alpha, beta and radium .,,,.,,,„.,..,.„..,.,
..do
..do ,
G
do
do
do
P, G ...
Preservation 2-
Maximum holding time4
Do.
Cool, 4 °C, 0.008% NajSzO.!,5 j
store in dark, j
Cool, 4 °C | Do
Cool, 4 "C, 0,008% Na2S:O,,5 Do
store in dark,
do i Do
Cool, 4 °C, 0.008% Na
Cooi, 4 °C .,.,,.............,
Cool, Q~4 *C, pH<9, 0.008%
Cool, <4 °C
Freeze, <-1Q °C
I Cool, 4"C, pHS-91'
HNO3IopH<2
Do.
Do.
1 year.
7 days.
1 year.
Do,
8 months.
Table II Notes
1 Polyethylene (P) or glass (G), For microbiology, plastic sample containers must be made of sterilizable materials (poly-
propylene or other autoclavable plastic).
2 Sample preservation should be performed immediately upon sample collection, For composite chemical samples each aliquot
should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot,
then chemical samples may be preserved by maintaining at 4°C until compositing and sample splitting is completed.
3 When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply with the De-
partment of Transportation Hazardous Materials Regulations (49 CFR part 172), The person offering such material for transpor-
tation is responsible for ensuring such compliance. For the preservation requirements of Table II, the Office of Hazardous Mate-
rials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations
do not apply to the following materials; Hydrochloric acid (HC!) in water solutions at concentrations of 0.04% by weight or less
(pH about 1.96 or greater); Nitric acid (HNQ^) in water solutions at concentrations of 0.15% by weight or less (pH about 1,62 or
greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
Sodium hydroxide (NaQH) in water solutions at concentrations of 0-080% by weight or less {pH about 12.30 or less),
4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that sampies may
be held before analysis and still be considered valid. Samples may be held for longer periods only if the permittee, or monitoring
laboratory, has data on file to show that for the specific types of samples under study, the analytes are stable for the longer time,
and has received a variance from the Regional Administrator under §136.3(e). Some samples may not be stable tor the max-
imum time period given in the table, A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if
knowledge exists to show that this is necessary to maintain sample stability. See § 136,3{e) for details. The term "analyze imme-
diately" usually means within 15 minutes or less of sample coliection,
5 Should only be used in the presence of residual chlorine.
6 Maximum holding time is 24 hours when sulfide is present. Optionally ail samples may be tested with lead acetate paper be-
fore pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium
nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is added to pH 12,
7 Samples should be filtered immediately on-site before adding preservative for dissolved metals.
g Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds,
9 Sample receiving no pH adjustment must be analyzed within seven days of sampling,
"'The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be
analyzed within 3 days of sampling.
"When the extractabie analytes of concern fail within a single chemical category the specified preservative and maximum
holding times should be observed for optimum safeguard of sample integrity. When the analytes of concern fail within two or
more chemical categories, the sample may be preserved by cooling to 4"C, reducing residual chlorine with 0,008% sodium
thiosulfate, storing in the dart;, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days be-
fore extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted
in footnote 5 (re the requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of benzi"
dine).
!2lf 1,2-diphenylhydrazine is likely to b€ present, adjust the pH of the sample to 4,0±0,2 to prevent rearrangement to benzi-
dine,
u Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free) atmosphere.
!ipor tne analysis of diphenylnitrosamlne, add 0.008% Na-=S^Ch and adjust pH to 7-tO with NaOH within 24 hours of sam-
pling.
15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the sampies are extracted within
72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2CK,
^Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still present when the sam-
ples arrive at the laboratory. However, even if ice is present when the samples arrive, it is necessary to immediately measure the
temperature of the samples and confirm that the 4C temperature maximum has not been exceeded. In the isolated cases where
it can be documented that this holding temperature can not be met, the permittee can be given the option of on-site testing or
can request a variance. The request for a variance should include supportive data which show that the toxicity of the effluent
samples is not reduced because of the increased holding temperature.
17 Samples collected for the determination of trace level mercury (100 ng/L) using EPA Method 1631 must be collected in tight-
ly-capped fluoropolymer or glass bottles and preserved with BrCI or HCI solution within 48 hours of sample collection. The time
to preservation may be extended to 28 days if a sample is oxidized in the sample bottle. Samples collected for dissolved trace
level mercury should be filtered in the laboratory. However, if circumstances prevent overnight shipment, samples should be fil-
tered in a designated clean area In the field in accordance with procedures given in Method 1689, Samples that have been col-
lected for determination of total or dissolved trace level mercury must be analyzed within 9G days of sample collection.
38
-------
Environmental Protection Agency
§136.5
[38 FR 28758, Oct. 16, 1973, as amended at 41 FB 52781, Deo. 1, 1976; 49 FR 43251, 43258, 43259,
Oct. 26, 1984; 50 FB 691, 692, 695, Jan. 4, 1985; 51 FB 23693, June 30, 1986; 52 FR 33543, Sept. 3,
1987; 55 FB 24534, June 15, 1990; 55 FB 33440, Aug. 15, 1990; 56 FB 50759, Oct. 8, 1991; 57 FR 41833,
Sept. 11, 1992; 58 FB 4505, Jan. 31. 1994; 60 FB 17160, Apr. 4, 1995; 60 FR 39588, 39590, Aug. 2, 1995:
60 FR 44672, Aug. 28, 1995; 60 FB 53542, 53543, Oct. 16, 1995; 62 FR 48403, 48404, Sept. 15, 1997;
63 FR 50423, Sept. 21, 1998; 64 FB 4978, Feb. 2, 1999; 64 FB 10392, Mar. 4, 1999: 64 FB 26327, May
14, 1999; 64 FB 30433, 30434, June 8, 1999; 64 FR 73423, Deo. 30, 1999; 66 FR 32776, June 18, 2001;
67 FB 65226, Oct. 23, 2002; 67 FR 65886, Oct. 29, 2002; 67 FB 69971, Nov. 19, 2002; 68 FB 43278, July
21, 2003; 68 FR 54934, Sept. 19, 2003; 69 FB 18803, Apr. 9, 2004]
§ 136.4 Application for alternate test
procedures.
(a) Any person may apply to the Re-
gional Administrator in the Region
where the discharge occurs for ap-
proval of an alternative test procedure.
(b) When the discharge for which an
alternative test procedure is proposed
occurs within a State having a permit
program approved pursuant to section
402 of the Act, the applicant shall sub-
mit his application to the Regional Ad-
ministrator through the Director of
the State agency having responsibility
for issuance of NPDES permits within
such State.
(c) Unless and until printed applica-
tion forms are made available, an ap-
plication for an alternate test proce-
dure may be made by letter in trip-
licate. Any application for an alternate
test procedure under this paragraph (c)
shall:
(1) Provide the name and address of
the responsible person or firm making
the discharge (if not the applicant) and
the applicable ID number of the exist-
ing or pending permit, issuing agency,
and type of permit for which the alter-
nate test procedure is requested, and
the discharge serial number.
(2) Identify the pollutant or param-
eter for which approval of an alternate
testing procedure is being requested.
(3) Provide justification for using
testing procedures other than those
specified in Table I.
(4) Provide a detailed description of
the proposed alternate test procedure,
together with references to published
studies of the applicability of the alter-
nate test procedure to the effluents in
question.
(d) An application for approval of an
alternate test procedure for nationwide
use may be made by letter in triplicate
to the Director. Analytical Methods
Staff, Office of Science and Technology
(4303), Office of Water, U.S. Environ-
mental Protection Agency, 1200 Penn-
sylvania Ave., NW., Washington, DC
20460. Any application for an alternate
test procedure under this paragraph (d)
shall:
(1) Provide the name and address of
the responsible person or firm making
the application.
(2) Identify the pollutant(s) or pa-
rameter(s) for which nationwide ap-
proval of an alternate testing proce-
dure is being requested.
(3) Provide a detailed description of
the proposed alternate procedure, to-
gether with references to published or
other studies confirming the general
applicability of the alternate test pro-
cedure to the pollutant(s) or para-
meter^) in waste water discharges
from representative and specified in-
dustrial or other categories.
(4) Provide comparability data for
the performance of the proposed alter-
nate test procedure compared to the
performance of the approved test pro-
cedures.
[38 FB 28760, Oct. 16, 1973, as amended at 41
FR 52785, Dec. 1, 1976; 62 FR 30763, June 5,
1997]
§ 136.5 Approval of alternate test pro-
cedures.
(a) The Regional Administrator of
the region in which the discharge will
occur has final responsibility for ap-
proval of any alternate test procedure
proposed by the responsible person or
firm making the discharge.
(b) Within thirty days of receipt of an
application, the Director will forward
such application proposed by the re-
sponsible person or firm making the
discharge, together with his rec-
ommendations, to the Regional Admin-
istrator. Where the Director rec-
ommends rejection of the application
for scientific and technical reasons
which he provides, the Regional Ad-
ministrator shall deny the application,
39
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
and shall forward a copy of the rejected
application and his decision to the Di-
rector of the State Permit Program
and to the Director of the Analytical
Methods Staff, Washington, DC.
(c) Before approving any application
for an alternate test procedure pro-
posed by the responsible person or firm
making the discharge, the Regional
Administrator shall forward a copy of
the application to the Director of the
Analytical Methods Staff, Washington,
DC.
(d) Within ninety days of receipt by
the Regional Administrator of an ap-
plication for an alternate test proce-
dure, proposed by the responsible per-
son or firm making the discharge, the
Regional Administrator shall notify
the applicant and the appropriate
State agency of approval or rejection,
or shall specify the additional informa-
tion which is required to determine
whether to approve the proposed test
procedure. Prior to the expiration of
such ninety day period, a recommenda-
tion providing the scientific and other
technical basis for acceptance or rejec-
tion will be forwarded to the Regional
Administrator by the Director of the
Analytical Methods Staff, Washington,
DC. A copy of all approval and rejec-
tion notifications will be forwarded to
the Director, Analytical Methods Staff,
Washington, DC, for the purposes of na-
tional coordination.
(e) Approval for nationwide use. (1)
Within sixty days of the receipt by the
Director of the Analytical Methods
Staff, Washington, DC, of an applica-
tion for an alternate test procedure for
nationwide use, the Director of the An-
alytical Methods Staff shall notify the
applicant in writing whether the appli-
cation is complete. If the application is
incomplete, the applicant shall be in-
formed of the information necessary to
make the application complete.
(2) Within ninety days of the receipt
of a complete package, the Analytical
Methods Staff shall perform any anal-
ysis necessary to determine whether
the alternate method satisfies the ap-
plicable requirements of this part, and
the Director of the Analytical Methods
Staff shall recommend to the Adminis-
trator that he/she approve or reject the
application and shall also notify the
applicant of such recommendation.
(3) As expeditiously as practicable,
an alternate method determined by the
Administrator to satisfy the applicable
requirements of this part shall be pro-
posed by EPA for incorporation in sub-
section 136.3 of 40 CPR part 136. EPA
shall make available for review all the
factual bases for its proposal, including
any performance data submitted by the
applicant and any available EPA anal-
ysis of those data.
(4) Following a period of public com-
ment, EPA shall, as expeditiously as
practicable, publish in the FEDERAL
REGISTER a final decision to approve or
reject the alternate method.
[38 FR 28760, Oct. 16, 1973, as amended at 41
FR 52785, Dec. 1, 1976; 55 FR 33440, Aug. 15,
1990; 62 FR 30763, June 5, 1997]
APPENDIX A TO PART 136—METHODS FOR
ORGANIC CHEMICAL ANALYSIS OF
MUNICIPAL AND INDUSTRIAL WASTE-
WATER
METHOD 601—PUROEABLE HALOCARBONS
1. Scope and Application
1.1 This method covers the determination
of 29 purgeable halocarbons.
The following parameters may be deter-
mined by this method:
Parameter
Bromodichloromethane
Bromoform ...
Bromomethane
Carbon tetrachloride
Chlorobenzene
Chloroethane
2-Chloroethylvinyl ether
Chloroform
Dibromochloromethane
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
Dichlorodif luoromethane
1,1-Dichloroethane
1 ,2-Dichloroethane
1 1-Dichloroethane
trans-1,2-Dichloroethene
cis-1 ,3-Dichloropropene
trans-1 ,3-Dichloropropene
Methylene chloride
1 ,1 ,2,2-Tetrachloroethane
Tetrachloroethene
1,1,1-Trichloroethane
1 , 1 ,2-Trichloroethane
Tetrachloroethene
Vinvl chloride
STORET
No.
32101
32104
34413
32102
34301
34311
34576
32106
34418
32105
34536
34566
34571
34668
34496
34531
34501
34546
34541
34704
34699
34423
34516
34475
34506
34511
39180
34488
39715
CAS No.
75-27^t
75-25-2
74-83-9
56-23-5
108-90-7
75-00-3
100-75-8
67-«6-3
74-87-3
124-48-1
95-50-1
541-73-1
106-46-7
75-71-8
75-34-3
107-06-2
75-35-4
156-60-5
78-87-5
10061-01-5
10061-02-«
75-09-2
79-34-5
127-18-4
71-55-6
79-00-5
79-01 -6
75-69-4
75-01^t
40
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
1.2 This is a purge and trap gas chroma-
tographic (GC) method applicable to the de-
termination of the compounds listed above
in municipal and industrial discharges as
provided under 40 CFR 136.1. When this meth-
od is used to analyze unfamiliar samples for
any or all of the compounds above, com-
pound identifications should be supported by
at least one additional qualitative tech-
nique. This method describes analytical con-
ditions for a second gas chromatographic
column that can be used to confirm measure-
ments made with the primary column. Meth-
od 624 provides gas chromatograph/mass
spectrometer (GO/MS) conditions appro-
priate for the qualitative and quantitative
confirmation of results for most of the pa-
rameters listed above.
1.3 The method detection limit (MDL, de-
fined in Section 12.1)' for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the operation of a purge and trap
system and a gas chromatograph and in the
interpretation of gas chromatograms. Each
analyst must demonstrate the ability to gen-
erate acceptable results with this method
using the procedure described in Section 8.2.
2. Summary of Method
2.1 An inert gas is bubbled through a 5-mL
water sample contained in a specially-de-
signed purging chamber at ambient tempera-
ture. The halocarbons are efficiently trans-
ferred from the aqueous phase to the vapor
phase. The vapor is swept through a sorbent
trap where the halocarbons are trapped.
After purging is completed, the trap is heat-
ed and backflushed with the inert gas to
desorb the halocarbons onto a gas
chromatographic column. The gas chro-
matograph is temperature programmed to
separate the halocarbons which are then de-
tected with a halide-specific detector.2-1
2.2 The method provides an optional gas
chromatographic column that may be help-
ful in resolving the compounds of interest
from interferences that may occur.
J. Interferences
3.1 Impurities in the purge gas and or-
ganic compounds outgassing from the plumb-
ing ahead of the trap account for the major-
ity of contamination problems. The analyt-
ical system must be demonstrated to be free
from contamination under the conditions of
the analysis by running laboratory reagent
blanks as described in Section 8.1.3. The use
of non-Teflon plastic tubing, non-Teflon
thread sealants, or flow controllers with rub-
ber components in the purge and trap system
should be avoided.
3.2 Samples can be contaminated by diffu-
sion of volatile organics (particularly fluoro-
carbons and methylene chloride) through the
septum seal ilto the sample during shipment
and storage. A field reagent blank prepared
from reagent water and carried through the
sampling and handling protocol can serve as
a check on such contamination.
3.3 Contamination by carry-over can
occur whenever high level and low level sam-
ples are sequentially analyzed. To reduce
carry-over, the purging device and sample
syringe must be rinsed with reagent water
between sample analyses. Whenever an un-
usually concentrated sample is encountered,
it should be followed by an analysis of rea-
gent water to check for cross contamination.
For samples containing large amounts of
water-soluble materials, suspended solids,
high boiling compounds or high organohalide
levels, it may be necessary to wash out the
purging device with a detergent solution,
rinse it with distilled water, and then dry it
in a 105°C oven between analyses. The trap
and other parts of the system are also sub-
ject to contamination; therefore, frequent
bakeout and purging of the entire system
may be required.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified4 6 for
the information of the analyst.
4.2 The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens: carbon tetrachloride, chlo-
roform, 1,4-dichlorobenzene, and vinyl chlo-
ride. Primary standards of these toxic com-
pounds should be prepared in a hood. A
NIOSH/MESA approved toxic gas respirator
should be worn when the analyst handles
high concentrations of these toxic com-
pounds.
41
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
5. Apparatus and Materials
5.1 Sampling equipment, for discrete sam-
pling.
5,1.1 Vial—25-mL capacity or larger,
equipped with a screw cap with a hole in the
center (Pierce #13075 or equivalent). Deter-
gent wash, rinse with tap and distilled water,
and dry at 105 °C before use.
5.1.2 Septum—Teflon-faced silicone
(Pierce #12722 or equivalent). Detergent
wash, rinse with tap and distilled water, and
dry at 105 °C for 1 h before use.
5,2 Purge and trap system—The purge and
trap system consists of three separate pieces
of equipment: a purging device, trap, and
desorber. Several complete systems are now
commercially available.
5,2.1 The purging device must be designed
to accept 5-rnL samples with a water column
at least 3 cm deep. The gaseous head space
between the water column and the trap must
have a total volume of less than 15 mL. The
purge gas must pass through the water col-
umn as finely divided bubbles with a diame-
ter of less than 3 mm at the origin. The
purge gas must be introduced no more than
5 mm from the base of the water column.
The purging device illustrated in Figure 1
meets these design criteria.
5.2.2 The trap must be at least 25 cm long
and have an inside diameter of at least 0.105
in. The trap must be packed to contain the
following minimum lengths of adsorbents: 1.0
cm of methyl silicone coated packing (Sec-
tion 6.3.3), 7.7 cm of 2,6-diphenylene oxide
polymer (Section 6.3.2), 7.7 cm of silica gel
(Section 6.3.4), 7.7 cm of coconut charcoal
(Section 6.3.1). If it is not necessary to ana-
lyze for diehlorodifluoromethane, the char-
coal can be eliminated, and the polymer sec-
tion lengthened to 15 cm. The minimum
specifications for the trap are illustrated in
Figure 2,
5.2.3 The desorber must be capable of rap-
idly heating the trap to 180 "0. The polymer
section of the trap should not be heated
higher than 180 °C and the remaining sec-
tions should not exceed 200 °C. The deaorber
illustrated in Figure 2 meets these design
criteria.
5.2.4 The purge and trap system may be
assembled as a separate unit or be coupled to
a gas chrornatograph as illustrated in Fig-
ures 3 and 4.
5.3 Gas chromatograph—An analytical
system complete with a temperature pro-
grammable gas chromatograph suitable for
on-column injection and all required acces-
sories including syringes, analytical col-
umns, gases, detector, and strip-chart re-
corder. A data system is recommended for
measuring peak areas.
5.3.1 Column 1—8 ft long x 0.1 in. ID stain-
less steel or glass, packed with 1% SP-1000
on Carbopack B (60/80 mesh) or equivalent.
This column was used to develop the method
performance statements in Section 12.
Guidelines for the use of alternate column
packings are provided in Section 10.1.
5.3.2 Column 2—6 ft long x 0.1 in. ID stain-
less steel or glass, packed with chemically
bonded n-octane on Porasil-C (100/120 mesh)
or equivalent.
5.3.3 Detector—Electrolytic conductivity
or microcoulometrio detector. These types of
detectors have proven effective in the anal-
ysis of wastewaters for the parameters listed
in the scope (Section 1.1). The electrolytic
conductivity detector was used to develop
the method performance statements in Sec-
tion 12. Guidelines for the use of alternate
detectors are provided in Section 10.1.
5.4 Syringes—5-mL glass hypodermic with
Luerlok tip (two each), if applicable to the
purging device.
5.5 Micro syringes—25-nL, 0.006 in. ID nee-
dle.
5.6 Syringe valve—2-way, with Luer ends
(three each).
5.7 Syringe—5-mL, gas-tight with shut-off
valve.
5.8 Bottle—15-nnLi, screw-cap, with Teflon
cap liner.
5.9 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
6, Reagents
6.1 Reagent water—Reagent water is de-
lined as a water in which an interferent is
not observed at the MBL of the parameters
of interest.
6.1.1 Reagent water can be generated by
passing tap water through a carbon filter bed
containing about 1 Ib of activated carbon
(Filtrasorb-300, Calgon Corp., or equivalent).
6.1.2 A water purification system
(Millipore Super-Q or equivalent) may be
used to generate reagent water.
6.1.3 Reagent water may also be prepared
by boiling water for 15 min. Subsequently,
while maintaining the temperature at 90 °C,
bubble a contaminant-free inert gas through
the water for 1 h. While still hot, transfer
the water to a narrow mouth screw-cap bot-
tle and seal with a Teflon-lined septum and
cap.
6.2 Sodium thiosulfate—(ACS) Granular.
6.3 Trap Materials:
6.3.1 Coconut charcoal—6/10 mesh sieved
to 26 mesh, Barnabey Cheney, CA-580-26 lot #
M-2649 or equivalent.
6.3.2 2,6-Diphenylene oxide polymer—
Tenax, (60/80 mesh), chromatographic grade
or equivalent.
6.3.3 Methyl silicone packing—3% OV-1 on
Chromosorb-W (60/80 mesh) or equivalent.
6.3.4 Silica gel—35/60 mesh, Davison,
grade-15 or equivalent.
6.4 Methanol—Pesticide quality or equiv-
alent.
6.5 Stock standard solutions—Stock
standard solutions may be prepared from
42
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
pure standard materials or purchased as cer-
tified solutions. Prepare stock standard solu-
tions in methancl using assayed liquids or
gases as appropriate. Because of the toxicity
of some of the organohalides, primary dilu-
tions of these materials should be prepared
in a hood. A NIOSH/MESA approved toxic
gas respirator should be used when the ana-
lyst handles high concentrations of such ma-
terials.
6.5.1 Place about 9.8 mL of methanol into
a 10-mL ground glass stoppered volumetric
flask. Allow the flask to stand, unstoppered,
for about 10 rain or until all alcohol wetted
surfaces have dried. Weigh the flask to the
learest 0.1 mg.
6.5.2 Add the assayed reference material:
6.5,2.1 Liquid—Using a 100 jiL syringe, im-
mediately add two or more drops of assayed
reference material to the flask, then re-
weigh. Be sure that the drops fall directly
into the alcohol without contacting the neck
of the flask.
6.5.2.2 Gases—To prepare standards for
any of the six halocarbons that boil below
30 °C (bromomethane, chloroethane, chloro-
methane, dichlorodifluoromethane,
trichlorofluoromethane, vinyl chloride), fill
a 5-mL valved gas-tight syringe with the ref-
erence standard to the 5.0-rnL mark. Lower
the needle to 5 mm above the methanol me-
niscus, Slowly introduce the reference stand-
ard above the surface of the liquid (the heavy
gas will rapidly dissolve into the methanol}.
6.5.3 Reweigh, dilute to volume, stopper,
then mix by inverting the flask several
times. Calculate the concentration in ng/^L
from the net gain in weight. When compound
purity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the malufacturer or by an inde-
pendent source.
6.5.4 Transfer the stock standard solution
into a Teflon-sealed screw-cap bottle. Store,
with minimal headspace, at —10 to -20 °C
and protect from light.
6.5.5 Prepare fresh standards weekly for
the six gases and 2-chloroethylvinyl ether.
All other standards must be replaced after
one month, or sooner if comparison with
check standards indicates a problem.
6.6 Secondary dilation standards—Using
stock standard solutions, prepare secondary
dilution standards in methanol that contain
the compounds of interest, either singly or
mixed together. The secondary dilution
standards should be prepared at concentra-
tions such that the aqueous calibration
standards prepared in Section 7.3.1 or 7.4.1
will bracket the working range of the ana-
lytical system. Secondary dilution standards
should be stored with minimal headspaee and
should be checked frequently for signs of
degradation or evaporation, especially just
prior to preparing calibration standards from
them.
6.7 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Assemble a purge and trap system that
meets the specifications in Section 5.2. Con-
dition the trap overnight at 180 °C by
baekflushing with an inert gas flow of at
least 20 mL/min. Condition the trap for 10
min once daily prior to use.
7.2 Connect the purge and trap system to
a gas chromatograph. The gas chro-
matograph must be operated using tempera-
ture and flow rate conditions equivalent to
those given in Table 1. Calibrate the purge
and trap-gas chromatographic system using
either the external standard technique (Sec-
tion 7.3) or the internal standard technique
(Section 7.4).
7.3 External standard calibration proce-
dure;
7,3.1 Prepare calibration standards at a
mimimim of three concentration levels for
each parameter by carefully adding 20.0 nL of
one or more secondary dilution standards to
100, 500, or 1000 nL of reagent water. A 25-|iL
syringe with a 0.006 in, ID needle should be
used for this operation. One of the external
standards should be at a concentration near,
but above, the MDL (Table 1) and the other
concentrations should correspond to the ex-
pected range of concentrations found in real
samples or should define the working range
of the detector. These aqueous standards can
be stored up to 24 h, if held in sealed vials
with zero headspace as described in Section
9.2. If not so stored, they must be discarded
after 1 h,
7.3.2 Analyze each calibration standard
according to Section 10, and tabulate peak
height or area responses versus the con-
centration in the standard. The results can
be used to prepare a calibration curve for
each compound. Alternatively, if the ratio of
response to concentration (calibration fac-
tor) is a constant over the working range
(<10% relative standard deviation, BSD), lin-
earity through the origin can be assumed
and the average ratio or calibration factor
can be used in place of a calibration curve.
7.4 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar In analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples. The compounds recommended for use as
surrogate spikes in Section 8,7 have been
used successfully as internal standards, be-
cause of their generally unique retention
times.
43
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
7,4.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest as described in
Section 7.3,1,
7,4.2 Prepare a spiking solution con-
taining' each of the internal standards using
the procedures described in Sections 6.5 and
6.6. It is recommended that the secondary di-
lution standard be prepared at a concentra-
tion of 15 ng/mL of each Internal standard
compound. The addition of 10 uL of this
standard to 5,0 mL of sample or calibration
standard would be equivalent to 30 ug/L.
7.4.3 Analyze each calibration standard
according to Section 10, adding 10 (iL of in-
ternal standard spiking solution directly to
the syringe (Section 10.4). Tabulate peak
height or area responses against concentra-
tion for each compound and internal stand-
ard, and calculate response factors (EP) for
each compound using Equation 1,
RF =
(As)(Cis)
(Me.)
Equation 1
where:
A«=Response for the parameter to be meas-
ured.
A,s=Response for the internal standard.
CiS=Concentration of the internal standard.
C»=Concentratlon of the parameter to be
measured.
If the BP value over the working range is a
constant (<10% RSD), the RF can be assumed
to be invariant and the average R.P can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, A/Ais, vs. BF.
7.5 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of a
QC check sample.
7,5,1 Prepare the QC check sample as de-
scribed in Section 8.2.2.
7.5.2 Analyze the QC check sample accord-
ing- to Section 10.
7.5.3 For each parameter, compare the re-
sponse (Q) with the corresponding calibra-
tion acceptance criteria found in Table 2. If
the responses for all parameters of interest
fall within the designated ranges, analysis of
actual samples can begin. If any individual Q
falls outside the range, proceed according to
Section 7,5.4.
NOTE: The large number of parameters in
Table 2 present a substantial probability
that one or more will not meet the calibra-
tion acceptance criteria when all parameters
are analyzed.
7.5.4 Repeat the test only for those pa-
rameters that failed to meet the calibration
acceptance criteria. If the response for a pa-
rameter does not fall within the range in
this second test, a new calibration curve,
calibration factor, or BF must be prepared
for that parameter according to Section 7,3
or 7.4.
8. Quality Control
8.1 Bach laboratory that uses this- method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1,2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tion 10.1) to improve the separations or lower
the cost of measurements. Bach time such a
modification is made to the method, the ana-
lyst is required to repeat the procedure in
Section 8.2.
8.1.3 Bach day, the analyst must analyze a
reagent water blank to demonstrate that
interferences from the analytical system are
under control.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria,
8,1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 10
jig/mL in methanol. The QC check sample
concentrate must be obtained from the U.S.
44
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using- stock standards prepared independ-
ently from those used for calibration.
8.2.2 Prepare a QC check sample to con-
tain 20 |ig/L of each parameter by adding 200
|iL of QC check sample concentrate to 100 mL
of reagent water.
8.2.3 Analyze four 5-mL aliquots of the
well-mixed QC check sample according to
Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in |ig/L, for each parameter of in-
terest using the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s ex_ceeds the precision limit
or any individual X falls outside the range
for accuracy, then the system performance is
unacceptable for that parameter.
NOTE: The large number of parameters in
Table 2 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.3.
8.2.6.2 Beginning with Section 8.2.3, repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning- with Section 8.2.3.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 20 \igfL or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.2 Analyze one 5-mL sample aliquot to
determine the background concentration (B)
of each parameter. If necessary, prepare a
new QC check sample concentrate (Section
8.2.1) appropriate for the background con-
centrations in the sample. Spike a second 5-
mL sample aliquot with 10 |iL of the QC
check sample concentrate and analyze it to
determine the concentration after spiking
(A) of each parameter. Calculate each per-
cent recovery (P) as 100(A-B)%/T, where T is
the known true value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.7 If spiking was
performed at a concentration lower than 20
|ig/L, the analyst must use either the QC ac-
ceptance criteria in Table 2, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 3, substituting
the spike concentration (T) for C; (2) cal-
culate overall precision (S') using the equa-
tion in Table 3, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X7T)±2.44(100 S'/T)%.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory. If the entire list of parameters in Table
2 must be measured in the sample in Section
8.3, the probability that the analysis of a QC
check standard will be required is high. In
this case the QC check standard should be
routinely analyzed with the spiked sample.
8.4.1 Prepare the QC check standard by
adding 10 nL of QC check sample concentrate
45
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
(Section 8.2.1 or 8.3.2) to 5 mL of reagent
water. The QC check standard needs only to
contain the parameters that failed criteria
in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration,
8.4.3 Compare the percent recovery (P5)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (Sp). Express the accuracy assessment
as a percent recovery interval from P —2s,, to
P+2Sp. If p=90% and %=!()%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8,6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such as
gas ehromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
8.7 The analyst should monitor both the
performance of the analytical system and
the effectiveness of the method in dealing
with each sample matrix by spiking each
sample, standard, and reagent water blank
with surrogate halocarbons. A combination
of bromochloromethane, 2-brorno-l-
chloropropane, and 1,4-dichlorobutane is rec-
ommended to encompass the range of the
temperature program used in this method.
Prom stock standard solutions prepared as
in Section 6.5, add a volume to give 150 \ig of
each surrogate to 45 mL of reagent water
contained in a 50-mL volumetric flask, mix
and dilute to volume for a concentration of
15 ng/jtL. Add 10 nL of this surrogate spiking
solution directly into the 5-mLi syringe with
every sample and reference standard ana-
lyzed. Prepare a fresh surrogate spiking solu-
tion on a weekly basis. If the internal stand-
ard calibration procedure is being used, the
surrogate compounds may be added directly
to the internal standard spiking solution
(Section 7,4.2).
9. Sample Collection, Preservation, and
Handling
9.1 All samples must be iced or refrig-
erated from the time of collection until anal-
ysis. If the sample contains free or combined
chlorine, add sodium thiosulfate preserva-
tive (10 mg/40 mL is sufficient for up to 5
ppm Clz) to the empty sample bottle just
prior to shipping to the sampling site. EPA
Methods 330.4 and 330.5 may be used for
measurement of residual chlorine.8 Field test
kits are available for this purpose.
9.2 Grab samples must be collected in
glass containers having a total volume of at
least 25 mL. Fill the sample bottle just to
overflowing in such a manner that no air
bubbles pass through the sample as the bot-
tle is being filled. Seal the bottle so that no
air bubbles are entrapped in it. If preserva-
tive has been added, shake vigorously for 1
min. Maintain the hermetic seal on the sam-
ple bottle until time of analysis,
9.3 All samples must be analyzed within
14 days of collection.3
10. Procedure
10,1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are esti-
mated retention times and MDL that can be
achieved under these conditions. An example
of the separations achieved by Column 1 is
shown in Figure 5. Other packed columns,
chromatographic conditions, or detectors
may be used if the requirements of Section
8.2 are met.
10,2 Calibrate the system daily as de-
scribed in Section 7.
10.3 Adjust the purge gas (nitrogen or he-
lium) flow rate to 40 mL'min. Attach the
trap inlet to the purging device, and set the
purge and trap system to purge (Figure 3).
Open the syringe valve located on the purg-
ing device sample introduction needle.
10.4 Allow the sample to come to ambient
temperature prior to introducing it to the
syringe. Remove the plunger from a 5-mL sy-
ringe and attach a closed syringe valve. Open
the sample bottle (or standard) and carefully
pour the sample into the syringe barrel to
just short of overflowing. Replace the sy-
ringe plunger and compress the sample. Open
the syringe valve and vent any residual air
while adjusting the sample volume to 5.0 mL.
Since this process of taking an aliquot de-
stroys the validity of the sample for future
46
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
analysis, the analyst should fill a second sy-
ringe at this time to protect, against possible
loss of data. Add 10,0 iiL of the surrogate
spiking solution (Section 8.7) and 10.0 (iL of
the internal standard spiking solution (Sec-
tion 7.4.2). if applicable, through the valve
bore, then close the valve.
10.5 Attach the syringe-syringe valve as-
sembly to the syringe -valve on the purging
device, Open the syringe valves and inject
the sample into the purging chamber.
10.6 Close both valves and purge the sam-
ple for 11.0±0.1 min at ambient temperature.
10.7 After the 11-min purge time, attach
the trap to the ehromatograph, adjust the
purge and trap system to the desorb mode
(Figure 4), and begin to temperature pro-
gram the gas ehromatograph. Introduce the
trapped materials to the GO column by rap-
idly heating the trap to 180 °C while
backflushing the trap with an inert gas be-
tween 20 and 60 mL/min for 4 min. If rapid
heating of the trap cannot be achieved, the
GO column must be used as a secondary trap
by cooling it to 30 "0 (subambient tempera-
ture, if poor peak geometry or random reten-
tion time problems persist) instead of the
initial program temperature of 45 °C
10.8 While the trap is being desorbed into
the gas ehromatograph, empty the purging
chamber using the sample introduction sy-
ringe. Wash the chamber with two 5-mL
flushes of reagent water.
10.9 After desorbing the sample for 4 min.
recondition the trap by returning- the purge
and trap system to the purge mode. Wait 16
s then close the syringe valve on the purging
device to begin gas flow through the trap.
The trap temperature should be maintained
at 180 "C After approximately 7 min, turn off
the trap heater and open the syringe valve to
stop the g-as flow through the trap. When the
trap is cool, the next sample can be ana-
lyzed.
10.10 Identify the parameters in the sam-
ple by comparing the retention times of the
peaks in the sample chromatograrn with
those of the peaks in standard
ehromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst, should weigh heavily in the
interpretation of chromatograms.
10.11 If the response for a peak exceeds
the working range of the system, prepare a
dilution of the sample with reagent water
from the aliquot in the second syringe and
reanalyze.
11. Calculations
11.1 Determine the concentration of indi-
vidual compounds in the sample.
11,1,1 If the external standard calibration
procedure is used, calculate the concentra-
tion of the parameter being measured from
the peak response using the calibration
curve or calibration factor determined in
Section 7.3.2.
11.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RP) determined In Section 7.4.3 and Equa-
tion 2.
Equation 2
Concentration (|Xg/L) =
(AS)(C1S)
(Ais)(RF)
where:
As=Response for the parameter to be meas-
ured.
Ai5=Response for the internal standard.
C,i=Concentration of the internal standard.
11.2 Report results In jig/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
12. Method Performance
12.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.' The MDL concentration listed in
Table 1 were obtained using reagent water.''.
Similar results were achieved using
representative wastewaters. The MDL actu-
ally achieved in a given analysis will vary
depending on instrument sensitivity and ma-
trix effects.
12.2 This method is recommended for use
in the concentration range from the MDL to
lOOOxMDL. Direct aqueous injection tech-
niques should be used to measure concentra-
tion levels above lOOOxMDL.
12.3 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water. and three industrial
wastewaters spiked at six concentrations
over the range 8,0 to 500 )ig/L.* Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
References
1. 40 CPR part 136, appendix B.
2. Bellar, T.A., and Lichtenberg, J.J. "De-
termining Volatile Organics at Microgram-
per-Litre-Levels by Gas Chromatography,"
Journal of the American Water WoTks Associa-
tion, 66, 739 (1974).
3. Bellar, T.A., and Lichtenberg, J.J.
"Semi-Automated Headspace Analysis of
Drinking Waters and Industrial Waters for
47
-------
Pt. 136, App. A, Meth. 601
Purgeable Volatile Organic Compounds,"
Proceedings from Symposium on Measure-
ment of Organic Pollutants in Water and
Wastewater, American Society for Testing
and Materials, STP 686, C.E. Van Hall, edi-
tor, 1978.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry" (29 CFR part 1910), Occupa-
tional Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
40 CFR Ch. I (7-1-04 Edition)
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
8. "Methods 330.4 (Titrimetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes, EPA
600/4-79-020, U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268,
March 1979.
9. "EPA Method Study 24, Method 601—
Purgeable Halocarbons by the Purge and
Trap Method," EPA 600/4-84-064, National
Technical Information Service, PB84-212448,
Springfield, Virginia 22161, July 1984.
10. "Method Validation Data for EPA Meth-
od 601," Memorandum from B. Potter, U.S.
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory,
Cincinnati, Ohio 45268, November 10, 1983.
11. Bellar, T. A., Unpublished data, U.S.
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory,
Cincinnati, Ohio 45268, 1981.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
Retention time (min)
Column 1
Column 2
Method detection
limit (ng/L)
Chloromethane
Bromomethane
Dtchlorodifluoromethane
Vinyl chloride
Chloroethane
Methylene chloride
Trichlorofluoromethane
1,1-Dichloroethene
1,1-Dichloroethane
trans-1,2-Dichloroethene
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Carbon telrachloride
Bromodichloromethane
1,2-Dichloropropane
cis-1,3-Dichloropropene
Trichloroethene
Dibromochloromethane
1,1,2-Trichloroethane
trans-1,3-Dichloropropene
2-Chloroethylvinyl ether
Bromoform
1,1,2,2-Tetrachloroethane
Tetrachloroethene
Chlorobenzene
1,3-Dichlorobenzene
1,2-Dichlorobenzene
1,4-Dichlorobenzene
1.50
2.17
2.62
2.67
3.33
5.25
7.18
7.93
9.30
10.1
10.7
11.4
12.6
13.0
13.7
14.9
15.2
15.8
16.5
16.5
16.5
18.0
19.2
21.6
21.7
24.2
34.0
34.9
35.4
5.28
7.05
nd
5.28
8.68
10.1
nd
7.72
12.6
9.38
12.1
15.4
13.1
14.4
14.6
16.6
16.6
13.1
16.6
18.1
18.0
nd
19.2
nd
15.0
18.8
22.4
23.5
22.3
0.08
1.18
1.81
0.18
0.52
0.25
nd
0.13
0.07
0.10
0.05
0.03
0.03
0.12
0.10
0.04
0.34
0.12
0.09
0.02
0.20
0.13
0.20
0.03
0.03
0.25
0.32
0.15
0.24
Column 1 conditions: Carbopack B (60/80 mesh) coated with 1% SP-1000 packed in an 8 ft x 0.1 in. ID stainless steel or
glass column with helium carrier gas at 40 mL/min flow rate. Column temperature held at 45 °C for 3 min then programmed at 8
°C/min to 220 °C and held for 15 min.
Column 2 conditions: Porisil-C (100/120 mesh) coated with n-octane packed in a 6 ft x 0.1 in. ID stainless steel or glass col-
umn with helium carrier gas at 40 mL/min flow rate. Column temperature held at 50 °C for 3 min then programmed at 6 °C/min
to 170 °C and held for 4 min.
nd=not determined.
48
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
TABLE 2—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 601:
Parameter
Brornomethane - ......
2-ChloroethyMnyl ether
1 ,4-DichIorobenzene
1,1-DichIoroethane
1 ,2-Dichloroethane
1,1-Dichloroethene
trans-1 ,3~Dichloropropene
Vinvl chloride
Range for Q
fug/L)
152-24.8
14.7-25.3
11.7-28.3
137-263
14.4-25.6
15.4-24.6
12.0-28.0
15.0-25.0
1 1 9-28 1
13.1-26.9
140-260
9.9-30.1
13.9-26.1
16.8-23.2
14.3-25.7
12.6-27.4
12,8-272
148-252
12.8-27,2
12,8-27.2
15.5-24.5
9 8-30 2
14.0-26.0
14.2-25.8
1 5 7-24 3
1 5.4-24 6
1 3 3-26 7
13.7-26.3
Limit for s
(ug/L)
43
4.7
7.8
5 6
5.0
4 4
8,3
45
7 4
63
5 5
9,1
5.5
3.2
5.2
6.6
64
5 2
73
7.3
4.0
9 2
5.4
49
39
4 2
6 0
5.7
Range for X
&19/L)
10.7-320
50-293
3.4-24.5
1 1 8-25 3
10.2-27.4
1 1 .3-25 2
4.5-35.5
12.4-24 0
D-34 9
7,9-35 1
1 7-38 9
6 2-32 6
11.5-25.5
11.2-24.6
13.0-26.5
10.2-27.3
1 1 4-27 1
10 1-29 9
6 2-33 8
6.2-33.8
7.0-27 6
66-31 8
8.1-29 6
10.8-248
96-254
9 2-26 6
7 4-28 1
8.2-29.9
Range P.
P, (%)
42-172
13-159
D-144
43-143
38-150
46-137
14-186
49-133
D-193
24-191
D-208
7-187
42-143
47-132
51-147
28-167
38-155
44-156
22-1 78
22-178
25-1 62
8-184
26-162
41-138
39-136
35-146
21-156
28-163
u Criteria were calculated assuming a QC check sample concentration of 20 ug/L.
Q=Concerrtration measured in QC check sample, in fig/L (Section 7.5,3),
s=Standard deviation of four recovery measurements, in ^g/L (Section 8,2.4),
X-Average recovery for four recovery measurements, in M-g/L (Section 8,2.4),
P, ps=Percent recovery measured (Seclion 8-3.2, Section 9,4.2).
D=Detected; result must be greater than zero,
NOTE: These criteria are based directly upon the method performance data in Table 3- Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limils to concentrations below those used to develop Table 3.
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 601
Accuracy, as re- Single analyst pre- , Overall precision,
yiether" mil"
ethane
oefhene
ropene«
lane
ethane
covery, X' (pg/L)
1.12C-1.02
0 96C - 2 05
0.76C-1.27
0 98C - 1 04
1 .000 - 1 .23
0.99C - 1 ,53
1.00C
0.93C - 0.39
0.77C+0.18
0.94C+2.72
0 93C4-1 70
0.95C+0.43
093C-0.09
0 95C - 1 08
1 04C - 1 06
0.98C-0.87
0.97C-0.10
1.00C
1.00C
1 OOC
0 91 C- 0.93
0.95C+0.19
0 94C4-0 06
0.90C-0.16
0.86C 4-0.30
0.87C+Q.48
0.89C-0.07
0.97C-0.36
cision, s/ (iig/L)
0.11X4-0.04
0 12X4-058
0.28X-0.27
0 1 5X4-0 38
0.15X-0.02
014X-0 13
0.20X
0.13X4-0.15
0.28X-0.31
011X4-1 10
0 20X+0 97
0.14X4-2.33
0 15X4-029
009X4-0 17
0 1 1 X+0 70
Q.21X-Q.23
0.11X4-1.46
0.13X
0.18X
018X
011X4-033
0 14X+2.41
0 14X4-0 38
0.15X4-0,04
0.13X-0.14
0.13X^0.03
0.15X4-0.67
0.13X»0.65
S' (ng/u)
0.20x4-1.00
021X+241
0 36X4-0 94
0 20X4-0 39
0.18X+1.21
0 17X4-063
0.35X
0.19X-0.02
0.52X4.1.31
0 24X+1 68
0 13X+6 13
0 26X+2.34
0 20X4-0 41
0 14X4-0 94
0 15X4-0 94
0.29X-040
0.17X4-1.46
0.23X
0.32X
032X
021X»1 43
0 23X+2 79
0 18X4-2 21
0.20X4-0.37
0.19X,067
0 23X*0 30
0.26X+0.91
0.27X4-0.40
Bromoform ..,,.,,,
Bromomethane .
Carbon tetrachbride
Chlorobenzene
Choroethane ...........
2-Ghloroethyiv
Chiofoforrn —,
Chloromethan'
Dibromochlorc
1,2-Dichlorobenzene
1,3-Dich!orobenzene
1.4-Dichlorobenzene
1,1'Dichloroethane .
1,2-Dichloroethane ...
1,1-Dichloroethene .
trans-1,2-DiChloroefl"
1,2-DicWoropropane
cis-l .3-Dichloroprop*
trgns-1,3-Dichloroprc
Methyiene chloride ..
1.1,2.2-Tetrachlorc
Tetrachloroethene
1,1,1 -Trichloroethane
1,1,2-TricWoroethane
Trichloroethene
Trichlorofluoron
Vinyl chloride ,
X'=Expected recovery for one or more measurements of a sample containing a concentration of C,
49
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
sn'=Expected single analyst standard deviation of measurements at an average concentration found of X, in \ig/L.
S1=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in jig/L.
C=True value for the concentration, in |ig/L
X=Average recovery found for measurements of samples containing a concentration of C, in (ig/L
"Estimates based upon the performance in a single laboratory.10
OPTIONAL
FOAM
TRAP
-EXIT Y« IN.
0. D.
-•-14MM 0. D.
INLET '/« IN.
0. D.
% IN.
0. D. EXIT
SAMPLE INLET
2-WAY SYRINGE VALVE
17CM. 20 GAUGE SYRINGE NEEDLE
6MM. 0. D. RUBBER SEPTUM
~10MM. 0. D.
INLET
1/« IN. 0. D.
1/16 IN. O.D.
y STAINLESS STEEL
13X MOLECULAR
SIEVE PURGE
GAS FILTER
PURGE GAS
FLOW
CONTROL
10MM GLASS FRIT
MEDIUM POROSITY
Figure 1. Purging device.
50
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 601
PACKING PROCEDURE
CONSTRUCTION
GLASS 5MMR /-"-/KJOT
WOOL TQ RESISTANCE
ACTIVATED
CHARCOAL 7.7C
GRADE 15 ._ _r
SILICA GEL/-/U
III
,1
i
T
T
i
TENAX 7.7 Cf
fl
3*0 V-1 -
GLASS WOOL1UW»
5MM
_
WIRE WRAPPED
SOLID
-------
Pt. 136, App. A, Meth. 601
40 CFR Ch. I (7-1-04 Edition)
CARRIER GAS FLOW CONTROL LIQUID INJECTION PORTS
- COLUMN OVEN
PRESSURE REGULATOR
\
PURGE GAS
FLOW CONTROL \|—
13X MOLECULAR
SIEVE FILTER
— CONFIRMATORY COLUMN
TO DETECTOR
— ANALYTICAL COLUMN
\ OPTIONAL 4-PORT COLUMN
6-PORT SELECTION VALVE
RESISTANCE WIRE
CHEATER CONTROL
PURGING
DEVICE
Note:ALL LINES BETWEEN
TRAP AND GC
SHOULD BE HEATED
TO BOX
Figure 3. Purge and trap system-purge mode.
CARRIER GAS
FLOW CONTROL
PRESSURE
REGULATOR
PURGE GAS
FLOW CONTROL , ,
13X MOLECULAR
SIEVE FILTER
LIQUID INJECTION PORTS
, COLUMN OVEN
^.CONFIRMATORY COLUMN
r>TO DETECTOR
ANALYTICAL COLUMN
OPTIONAL 4-PORT COLUMN
SELECTION VALVE
6-PORT TRAP INLET
VALVE J RESISTANCE WIRE HEATER
•^ CONTROL
Note:
ALL LINES BETWEEN
TRAP AND GC
SHOULD BE HEATED
TO 80°C.
PURGING
DEVICE
Figure 4. Purge and trap system - desorb mode.
52
-------
89
£
5
ui
o
at
IB
B)
O
IB
3
3
•o
to
£
30
£ ™
I s»
£. —
O 2
BROMOMETHANE
CHLOROETHAME
CHLOROMETHANE
1,1-DICHLOROETHENE
trons-1,2-DICHLOROETHENE
1,1,1- TRICHLOROETHANE
, 2-DICHLOROPROPANE
cis - 1,3-OiCHLOROPROPENI
trans • 1.3-OICHLOROPROPENE
1, 2-D1BROMOETHANE
1,1,1,2-TETRACHLOROETHANE
MMPMMHW*
1, 2, 3-TRICHLOROPROPANE
1, 1, 2, 2-TETRACHLOROETHANE
CHLORO BENZENE
. 1-CHLOROHEXANE
EROMOBENZEME
2-CHLOROTOLUENE
1. 4-DICHLOROBENZENE
3°
O =ogj
02f?
—i oo
§=§
t*2
s-:e
o
o
§
O
-------
Pt. 136, App. A, Meth. 602
40 CFR Ch. I (7-1-04 Edition)
METHOD 602—PURGE ABLE AROMATIC s
1. Scope and Application
1.1 This method covers the determination
of various purgeable aromatics. The fol-
lowing parameters may tie determined by
this method:
Parameter
Chlorobenzene
1 ,3-Dichlorobenzene
Ethylbenzene
Toluene
STORE!
No.
34030
34301
34536
34566
34571
34371
34010
CAS No.
71-43-2
108-90-7
95-50-1
541-73-1
106-46-7
100-41-4
108-S8-3
1.2 This is a purge and trap gas
chromatographic (GO) method applicable to
the determination of the compounds listed
above in municipal and industrial discharges
as provided under 40 CFR 136.1. When this
method is used to analyze unfamiliar sam-
ples for any or all of the compounds above,
compound identifications should tie sup-
ported by at least one additional qualitative
technique. This method describes analytical
conditions for a second gas chromatographic
column that can be used to confirm measure-
ments made with the primary column. Meth-
od 624 provides gas chromatograph/mass
spectrometer (GC/MS) conditions appro-
priate for the qualitative and quantitative
confirmation of results for all of the param-
eters listed above.
1.3 The method detection limit (MDL, de-
fined in Section 12.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the operation of a purge and trap
system and a gas chromatograph and in the
interpretation of gas chromatograms. Each
analyst must demonstrate the ability to gen-
erate acceptable results with this method
using the procedure described in Section 8.2.
2. Summary of Method
2.1 An inert gas is bubbled through a 5-mL
water sample contained in a specially-de-
signed purging chamber at ambient tempera-
ture. The aromatics are efficiently trans-
ferred from the aqueous phase to the vapor
phase. The vapor is swept through a sorbent
trap where the aromatics are trapped. After
purging is completed, the trap is heated and
backflushed with the inert gas to desorb the
aromatics onto a gas chromatographic col-
umn. The gas chromatograph is temperature
programmed to separate the aromatics
which are then detected with a
photoionization detector.2-3
2.2 The method provides an optional gas
chromatographic column that may be help-
ful in resolving the compounds of interest
from interferences that may occur.
3. Interferences
3.1 Impurities in the purge gas and or-
ganic compounds outgassing from the plumb-
ing ahead of the trap account for the major-
ity of contamination problems. The analyt-
ical system must be demonstrated to be free
from contamination under the conditions of
the analysis by running laboratory reagent
blanks as described in Section 8.1.3. The use
of non-Teflon plastic tubing, non-Teflon
thread sealants, or flow controllers with rub-
ber components in the purge and trap system
should be avoided.
3.2 Samples can be contaminated by diffu-
sion of volatile organics through the septum
seal into the sample during shipment and
storage. A field reagent blank prepared from
reagent water and carried through the sam-
pling and handling protocol can serve as a
check on such contamination.
3.3 Contamination by carry-over can
occur whenever high level and low level sam-
ples are sequentially analyzed. To reduce
carry-over, the purging device and sample
syringe must be rinsed with reagent water
between sample analyses. Whenever an un-
usually concentrated sample is encountered,
it should be followed by an analysis of rea-
gent water to check for cross contamination.
For samples containing large amounts of
water-soluble materials, suspended solids,
high boiling compounds or high aromatic
levels, it may be necessary to wash the purg-
ing device with a detergent solution, rinse it
with distilled water, and then dry it in an
oven at 105 °C between analyses. The trap and
other parts of the system are also subject to
contamination; therefore, frequent bakeout
and purging of the entire system may be re-
quired.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
54
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 602
are available and have been identified** for
the information of the analyst,
4.2 The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mam-
malian carcinogens: benzene and 1,4-
dlchlorobenzene. Primary standards of these
toxic compounds should be prepared In a
hood. A NIOSH/MESA approved toxic gas
respirator should be worn when the analyst
handles high concentrations of these toxic
compounds.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete sam-
pling,
5.1.1 Vial]25-mL capacity or larger,
equipped with a screw cap with a hole in the
center (Pierce #13075 or equivalent). Deter-
gent wash, rinse with tap and distilled water,
and dry at 105 °C before use.
5.1.2 Septum—Teflon-faced silicone
(Pierce #12722 or equivalent). Detergent
wash, rinse with tap and distilled water, and
dry at 105 °C for 1 h before use.
5.2 Purge and trap system—The purge and
trap system consists of three separate pieces
of equipment: A purging device, trap, and
desorber. Several complete systems are now
commercially available.
5,2.1 The purging device must be designed
to accept 5-mL samples with a water column
at least 3 cm deep. The gaseous head space
between the water column and the trap must
have a total volume of less than 15 mL. The
purge gas must pass through the water col-
umn as finely divided bubbles with a diame-
ter of less than 3 mm at the origin. The
purge gas must be introduced no more than
5 mm from the base of the water column.
The purging device illustrated in Figure 1
meets these design criteria.
5.2.2 The trap must be at least 25 cm long
and have an inside diameter of at least 0.105
in.
5.2.2,1 The trap is packed with 1 cm of
methyl silicone coated packing (Section
6.4.2) and 23 cm of 2,6-diphenylene oxide poly-
mer (Section 6,4,1) as shown in Figure 2. This
trap was used to develop the method per-
formance statements in Section 12.
5.2.2.2 Alternatively, either of the two
traps described in Method 601 may be used,
although water vapor will preclude the meas-
urement of low concentrations of benzene.
5.2.3 The desorber must be capable of rap-
idly heating the trap to 180 °C. The polymer
section of the trap should not be heated
higher than 180 °C and the remaining sec-
tions should not exceed 200 °C. The desorber
illustrated in Figure 2 meets these design
criteria,
5,2.4 The purge and trap system may be
assembled as a separate unit or be coupled to
a gas chroniatograph as illustrated in Fig-
ures 3, 4, and 5.
5.3 G-as chromatograph—An analytical
system complete with a temperature pro-
grammable gas chromatograph suitable for
on-colnmn injection and all required acces-
sories including syringes, analytical col-
umns, gases, detector, and strip-chart re-
corder. A data system Is recommended for
measuring peak areas.
5.3.1 Column 1—6 ft long x 0.082 in. ID
stainless steel or glass, packed with 5% SP-
1200 and 1.75% Bentone-34 on Supeleoport
(100/120 mesh) or equivalent. This column
was used to develop the method performance
statements in Section 12, Guidelines for the
use of alternate column packings are pro-
vided in Section 10.1.
5.3.2 Column 2—8 ft long x 0.1 in ID stain-
less steel or glass, packed with 5% 1,2,3-
Tris(2-cyanoethoxy)propane on Chromosorb
W-AW (60/80 mesh) or equivalent.
5.3.3 Detector—Photoionization detector
(h-Nu Systems, Inc. Model PI-51-02 or equiv-
alent). This type of detector has been proven
effective in the analysis of wastewaters for
the parameters listed in the scope (Section
1.1). and was used to develop the method per-
formance statements in Section 12. Guide-
lines for the use of alternate detectors are
provided in Section 10.1.
5.4 Syringes—5-niL glass hypodermic with
Luerlok tip (two each), if applicable to the
purging device.
5.5 Micro syringes—25-pL, 0.006 in. ID nee-
dle.
5.6 Syringe valve—2-way, with Luer ends
(three each).
5.7 Bottle—15-mL, screw-cap, with Teflon
cap liner.
5.8 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
6, Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.1.1 Reagent water can be generated by
passing tap water through a carbon filter bed
containing about 1 Ib of activated carbon
(Filtrasorb-300, Calgon Corp., or equivalent),
6.1.2 A water purification system
(Millipore Super-Q or equivalent) may be
used to generate reagent water.
6.1,3 Reagent water may also be prepared
by boiling water for 15 mln. Subsequently,
while maintaining the temperature at 90 °C,
bubble a contaminant-free inert gas through
the water for 1 h. While still hot, transfer
the water to a narrow mouth screw-cap bot-
tle and seal with a Teflon-lined septum and
cap,
6.2 Sodium thiosulfate—(ACS) Granular.
8,3 Hydrochloric acid (1+1)—Add 50 mL of
concentrated HC1 (ACS) to SO mL of reagent
water.
6.4 Trap Materials:
55
203-160 D-3
-------
Pt. 136, App. A, Meth. 602
40 CFR Ch, I (7-1-04 Edition)
6,4.1 2,6-Diphenylene oxide polymer—
Tenax, (60/80 mesh), chromatographie grade
or equivalent,
6.4.2 Methyl silioone packing—3% OV-1 on
Chromosorb-W (60/80 mesh) or equivalent.
6.5 Methanol—Pesticide quality or equiv-
alent.
6.6 Stock standard solutions—Stock
standard solutions may be prepared from
pure standard materials or purchased as cer-
tified solutions. Prepare stock standard solu-
tions in methanol using assayed liquids. Be-
cause of the toxicity of benzene and 1,4-
diehlorobenzene, primary dilutions of these
materials should be prepared in a hood. A
NIOSH/MESA approved toxic gas respirator
should be used when the analyst handles
high concentrations of such materials.
6.6.1 Place about 9.8 mL of methanol into
a 10-mL ground glass stoppered volumetric
flask. Allow the flask to stand, unstoppered,
for about 10 min or until all alcohol wetted
surfaces have dried. Weigh the flask to the
nearest 0.1 mg.
6.6.2 Using a 100-uL syringe, immediately
add two or more drops of assayed reference
material to the flask, then reweigh. Be sure
that the drops fall directly into the alcohol
without contacting- the neck of the flask.
6.6.3 Reweigh, dilute to volume, stopper,
then mix by inverting the flask several
times. Calculate the concentration in (ig/nL
from the net gain in weight. When compound
purity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.6.4 Transfer the stock standard solution
into a Teflon-sealed screw-cap bottle. Store
at 4 °C and protect from light.
6.6.5 All standards must be replaced after
one month, or sooner if comparison with
check standards indicates a problem.
6,7 Secondary dilution standards—Using
stock standard solutions, prepare secondary
dilution standards in methaaol that contain
the compounds of interest, either singly or
mixed together. The secondary dilation
standards should be prepared at concentra-
tions such that the aqueous calibration
standards prepared in Section 7.3.1 or 7,4,1
will bracket the working range of the ana-
lytical system. Secondary solution standards
must be stored with zero headspace and
should be checked frequently for signs of
degradation or evaporation, especially just
prior to preparing- calibration standards from
them.
6.8 Quality control check sample con-
centrate—See Section 8,2,1.
7. Calibration
7.1 Assemble a purge and trap system that
meets the specifications in Section 5.2. Con-
dition the trap overnight at 180 °C by
backflushing with an inert gas flow of at
least 20 mL/min, Condition the trap for 10
min once daily prior to use.
7.2 Connect the purge and trap system to
a gas chromatograph. The gas chro-
matograph must be operated using tempera-
ture and flow rate conditions equivalent to
those given in Table 1. Calibrate the purge
and trap-gas chromatographic system using
either the external standard technique (Sec-
tion 7.3) or the internal standard technique
(Section 7.4).
7.3 External standard calibration proce-
dure:
7,3,1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter by carefully adding 20,0 nL of
one or more secondary dilution standards to
100, 500, or 1000 mL of reagent water. A 25-jiL
syringe with a 0.006 in. ID needle should be
used for this operation. One of the external
standards should be at a concentration near,
but above, the MDL (Table 1) and the other
concentrations should correspond to the ex-
pected range of concentrations found in real
samples or should define the working range
of the detector. These aqueous standards
must be prepared fresh daily.
7.3.2 Analyze each calibration standard
according to Section 10, and tabulate peak
height or area responses versus the con-
centration in the standard. The results can
be used to prepare a calibration curve for
each compound, Alternatively, if the ratio of
response to concentration (calibration fac-
tor) is a constant over the working range
(<10% relative standard deviation, BSD), lin-
earity through the origin can be assumed
and the average ratio or calibration factor
can be used in place of a calibration curve.
7.4 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples. The compound, a,«,a,-trifluorotoluene,
recommended as a surrogate spiking com-
pound in Section 8.7 has been used success-
fully as an Internal standard.
7.4.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest as described in
Section 7.3.1.
7.4.2 Prepare a spiking solution con-
taining each of the internal standards using
the procedures described in Sections 6.6 and
6.7. It is recommended that the secondary di-
lution standard be prepared at a concentra-
tion of 15 jig/mi of each internal standard
compound. The addition of 10 p,l of this
56
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 602
standard to 5.0 mL. of sample or calibration
standard would be equivalent to 30 jig/L,
7.4.3 Analyze each calibration standard
according to Section 10, adding 10 jXL of in-
ternal standard spiking solution directly to
the syringe (Section 10.4). Tabulate peak
height or area responses against concentra-
tion for each compound and internal stand-
ard, and calculate response factors (BF) for
each compound using Equation 1.
RF= (As)(Cis) (Ais)(Cs)
Equation 1
where:
As=Besponse for the parameter to be meas-
ured.
Ai«=Besponse for the internal standard.
C,«=Concentration of the internal standard
C«=Concentration of the parameter to be
measured.
If the BF value over the working range is a
constant (<10% RSD). the BF can be assumed
to be invariant and the average BF can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, A JAis, vs. RF.
7.5 The working calibration curve, cali-
bration factor, or BF must be verified on
each working day by the measurement of a
QC check sample.
7.5,1 Prepare the QC check sample as de-
scribed in Section 8,2.2.
7.5.2 Analyze the QC check sample accord-
ing to Section 10,
7.5.3 For each parameter, compare the re-
sponse (Q) with the corresponding calibra-
tion acceptance criteria found in Table 2. If
the responses for all parameters of interest
fall within the designated ranges, analysis of
actual samples can begin. If any individual Q
falls outside the range, a new calibration
curve, calibration factor, or RF must be pre-
pared for that parameter according to Sec-
tion 7,3 or 7.4.
8. Quality Control
8.1 Bach laboratory that uses this method
is required to operate a formal quality con-
trol program. The mimimum requirements
of this program consist of an initial dem-
onstration of laboratory capability and an
ongoing analysis of spiked samples to evalu-
ate and document data quality. The labora-
tory must maintain records to document the
quality of data that is generated. Ongoing-
data quality checks are compared with es-
tablished performance criteria to determine
if the results of analyses meet the perform-
ance characteristics of the method. When re-
sults of sample spikes indicate atypical
method performance, a quality control check
standard must be analyzed to confirm that
the measurements were performed in an In-
control mode of operation.
8.1.1 The analyst must make an initial,
one-tirne, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2,
8.1.2 In recognition of advances that are
occurring in ehrornatography, the analyst is
permitted certain options (detailed in Sec-
tion 10,1) to improve the separations or lower
the cost of measurements. Each time such a
modification is made to the method, the ana-
lyst is required to repeat the procedure in
Section 8.2.
8.1.3 Each day, the analyst must analyze a
reagent water blank to demonstrate that
interferences from the analytical system are
under control.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.8 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8,2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 10
Hg/mL, in methanol. The QC check sample
concentrate must be obtained from the U.S.
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must he prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8.2.2 Prepare a QC check sample to con-
tain 20 ng/L of each parameter by adding 200
HL of QC check sample concentrate to 100 mL
of reagant water.
8.2.3 Analyze four 5-mL aliquots of the
well-mixed QC check sample according to
Section 10.
8.2.4 Calculate the average recovery (X) in
ug/L, and the standard deviation of the re-
covery (s) in iig/L, for each parameter of in-
terest using the four results,
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
57
-------
Pt. 136, App. A,Meth. 602
40 CFR Ch. I (7-1-04 Edition)
for precision and accuracy, respectively,
found in Table 2, If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Table 2 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.3.
8.2.6.2 Beginning with. Section 8.2.3, repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2.3,
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows;
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 20 (ig/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.2 Analyze one 5-mL sample aliquot to
determine the background concentration (B)
of each parameter. If necessary, prepare a
new QC check sample concentrate (Section
8.2.1) appropriate for the background con-
centrations in the sample. Spike a second 5-
mL sample aliquot with 10 uli of the QC
check sample concentrate and analyze it to
determine the concentration after spiking
(A) of each parameter. Calculate each per-
cent recovery (P) as 1QO(A-B)%/T, where T is
the known true value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.' If spiking was
performed at a concentration lower than 20
(ig/L, the analyst must use either the QC ac-
ceptance criteria in Table 2, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 3, substituting
the spike concentration (T) for C; (2) cal-
culate overall precision (S') using the equa-
tion in Table 3, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X'/T) ±2.44(100 SVT)%,7
8.3,4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8,4.1 Prepare the QC check standard by
adding 10 nL of QC check sample concentrate
(Section 8.2.1 or 8.3.2) to 5 mL of reagent
water. The QC check standard needs only to
contain the parameters that failed criteria
in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8,4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 2, Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
58
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 602
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P — 2sp to
P+2sp. If P=9Q% and sp=10%, for example, the
accuracy interval is expressed as 70-110%,
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram. confirmatory techniques such as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
8.7 The analyst should monitor both the
performance of the analytical system and
the effectiveness of the method in dealing
with each sample matrix by spiking- each
sample, standard, and reagent water blank
with surrogate compounds (e.g. a, a, a,-
trifluorotoluene) that encompass the range
of the temperature program used in this
method. From stock standard solutions pre-
pared as in Section 6.6, add a volume to give
750 ng of each surrogate to 45 mL of reagent
water contained in a 50-mL volumetric flask,
mix and dilute to volume for a concentration
of 15 mg/nL. Add 10 uL of this surrogate spik-
ing solution directly into the 5-mL syringe
with every sample and reference standard
analyzed. Prepare a fresh surrogate spiking
solution on a weekly basis. If the internal
standard calibration procedure is being used,
the surrogate compounds may be added di-
rectly to the internal standard spiking solu-
tion (Section 7.4.2),
9. Sample Collection, Preservation, and
Handling
9.1 The samples must be iced or refrig-
erated from the time of collection until anal-
ysis. If the sample contains free or combined
chlorine, add sodium thiosulfate preserva-
tive (10 mg/40 mL is sufficient for up to 5
ppm Cl2> to the empty sample bottle just
prior to shipping to the sampling site. EPA
Method 330.4 or 330.5 may tie used for meas-
urement of residual chlorine.8 Field test kits
are available for this purpose.
9.2 Collect about 500 mL of sample in a
clean container. Adjust the pH of the sample
to about 2 by adding 1+1 HC1 while stirring.
Fill the sample bottle in such a manner that
no air bubbles pass through the sample as
the bottle is being filled. Seal the bottle so
that no air bubbles are entrapped in it. Main-
tain the hermetic seal on the sample bottle
until time of analysis,
9.3 All samples must be analyzed within
14 days of collection.3
10. Procedure
10,1 Table 1 summarizes the recommended
operating conditions for the gas chrom-
atograph. Included in this table are esti-
mated retention times and MDL that can be
achieved under these conditions. An example
of the separations achieved by Column 1 is
shown in Figure 6. Other packed columns,
chromatographic conditions, or detectors
may be used if the requirements of Section
8.2 are met.
10.2 Calibrate the system daily as de-
scribed in Section 7.
10.3 Adjust the purge gas (nitrogen or he-
lium) flow rate to 40 mL/min. Attach the
trap inlet to the purging device, and set the
purge and trap system to purge (Figure 3).
Open the syringe valve located on the purg-
ing device sample introduction needle.
10.4 Allow the sample to come to ambient
temperature prior to introducing it to the
syringe. Remove the plunger from a 5-mL sy-
ringe and attach a closed syringe valve. Open
the sample bottle (or standard) and carefully
pour the sample into the syringe barrel to
just short of overflowing. Replace the sy-
ringe plunger and compress the sample. Open
the syringe valve and vent any residual air
while adjusting the sample volume to 5.0 mL.
Since this process of taking an aliquot de-
stroys the validity of the sample for future
analysis, the analyst should fill a second sy-
ringe at this time to protect against possible
loss of data. Add 10.0 jiL of the surrogate
spiking solution (Section 8,7) and 10.0 uL of
the internal standard spiking solution (Sec-
tion 7.4.2), if applicable, through the valve
bore, then close the valve.
10.5 Attach the syringe-syringe valve as-
sembly to the syringe valve on the purging
device. Open the syringe valves and inject
the sample into the purging chamber.
10.6 Close both valves and purge the sam-
ple for 12.0±0.1 min at ambient temperature.
10.7 After the 12-min purge time, dis-
connect the purging device from the trap.
Dry the trap by maintaining a flow of 40 mL/
min of dry purge gas through it for 6 min
(Figure 4), If the purging device has no provi-
sion for bypassing the purger for this step, a
dry purger should be inserted into the device
to minimize moisture in the gas. Attach the
trap to the chromatograph, adjust the purge
and trap system to the desorb mode (Figure
5), and begin to temperature program the gas
chromatograph. Introduce the trapped mate-
rials to the GC column by rapidly heating
the trap to 180 "C while backflushing the trap
with an Inert gas between 20 and 60 mL/min
for 4 min. If rapid heating of the trap cannot
be achieved, the GO column must be used as
59
-------
Pt. 136, App. A, Meth. 602
40 CFR Ch. I (7-1-04 Edition)
a secondary trap by cooling it to 30 °C (sub-
ambient temperature, if poor peak geometry
and random retention time problems persist)
instead of the initial program temperature of
50 °C.
10.8 While the trap is being desorbed into
the gas chromatograph column, empty the
purging chamber using the sample introduc-
tion syringe. Wash the chamber with two 5-
mL flushes of reagent water.
10.9 After desorbing the sample for 4 min,
recondition the trap by returning the purge
and trap system to the purge mode. Wait 15
s, then close the syringe valve on the purg-
ing device to begin gas flow through the
trap. The trap temperature should be main-
tained at 180 °C. After approximately 7 min,
turn off the trap heater and open the syringe
valve to stop the gas flow through the trap.
When the trap is cool, the next sample can
be analyzed.
10.10 Identify the parameters in the sam-
ple by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
10.11 If the response for a peak exceeds
the working range of the system, prepare a
dilution of the sample with reagent water
from the aliquot in the second syringe and
reanalyze.
11. Calculations
11.1 Determine the concentration of indi-
vidual compounds in the sample.
11.1.1 If the external standard calibration
procedure is used, calculate the concentra-
tion of the parameter being measured from
the peak response using the calibration
curve or calibration factor determined in
Section 7.3.2.
11.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.4.3 and Equa-
tion 2.
Concentration (|0.g/L) -
(As)(Cis)
Equation 2
where:
As = Response for the parameter to be meas-
ured.
Ais = Response for the internal standard.
Cls = Concentration of the internal standard.
11.2 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
12. Method Performance
12.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.9
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
12.2 This method has been demonstrated
to be applicable for the concentration range
from the MDL to 100 x MDL.9 Direct aqueous
injection techniques should be used to meas-
ure concentration levels above 1000 x MDL.
12.3 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 2.1 to 550 |ig/L.9 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
References
1. 40 CFR part 136, appendix B.
2. Lichtenberg, J.J. "Determining Volatile
Organics at Microgram-per-Litre-Levels by
Gas Chromatography," Journal American
Water Works Association, 66, 739 (1974).
3. Bellar, T.A., and Lichtenberg, J.J.
"Semi-Automated Headspace Analysis of
Drinking Waters and Industrial Waters for
Purgeable Volatile Organic Compounds,"
Proceedings of Symposium on Measurement
of Organic Pollutants in Water and Waste-
water. American Society for Testing and Ma-
terials, STP 686, C.E. Van Hall, editor, 1978.
4. "Carcinogens—Working with Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health. Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Safety, 3rd Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3. is two
times the value 1.22 derived in this report.)
60
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Environmental Protection Agency
Pt. 136, App. A, Meth. 602
TABLE 1 — CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMITS — Continued
8."Methods 330.4 (Titrimetric, DPD-PAS)
and 330.5 (Speotrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
BPA-6QO/4-79-020, U.S. Environmental Pro-
tection Agency, Office of Research and De-
velopment, Environmental Monitoring and
Support Laboratory, Cincinnati, Ohio 45268.
March 1979.
9. "EPA Method Study 25, Method 602,
Purgeable Aromatics." EPA 600/4-84-042, Na-
tional Technical Information Service, PB84-
196682, Springfield, Virginia 22161, May 1984.
Column 1 conditions: Supelcoport {100/120 mesh) coated
TABLE 1—CHROMATOGRAPHIG CONDITIONS AND with 5% sp-i2oo/u5% Bentone-34 packed in a e ft x O.OBS
MET-rur\r\ rir-rc^-nr^i I ifcai-re* in. ID stainless steel column with helium carrier gas at 36 mU
METHOD DETECTION LIMITS mjn ftow rate Co,umn temperature held at 50 °C for 2 min
then programmed at 6 °C/rnin to 90 ~C for a final hold.
Column 2 conditions: Chrome-sorb W-AW (60/80 mesh)
coated with 5% 1,2,3-Tris(2-cyanoethyoxy)propane packed in
a 6 ft x 0.085 in ID stainless steel column with helium carrier
gas at 30 mL/min flow rale. Column temperature held at 40
"C for 2 min then programmed at 2 ;'C/min to 100 '3C for a
final hold,
TABLE 2—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 602a
Parameter
,
Retention time (min)
Column 1
Toluene ! 5.75
Ethylbenzene j 8.25
Chlorobenzene '. 9.17
1 ,4-Dichlorobenzerie 16.8
1 ,3-Dichlorobenzene I 18.2
1 ,2-Dichlorobenzene | 25.9
Column 2
4.25
6.25
8.02
16.2
15.0
19.4
Method
detection
limit
IFW ;
0.2
0.2
0.2
0.3
0,4
0.4
Retention time (min) Method
_™_j detection
Parameter
1 ,2-Dichlorobenzene
Toluene
Range for Q
(H9/L)
15.4-246
16 1-239
13.6-26.4
1 4 5-25 5
1 3 9-26 1
1 2 6-27 4
15.5-24.5
Limit for
s (ng/L)
41
35
5.8
50
55
67 I
4.0 1
Range for X
«L)
100-279
127-254
10.6-27.6
12 8-255
1 1 6-25 5
100-282
11.2-27.7
Range for
P, P,(%)
39-150
55-135
37-154
50-141
42-143
32-1 60
46-148
GsConeentration measured In QC check sample, in fig/L (Section 7.5,3).
s^Standard deviation of four recovery measurements, in pg/L (Section 8 2.4).
X=Average recovery for four recovery measurements, in jig/L (Section 8-2.4).
P^, p=Percent recovery measured (Section 8.3-2. Section 8.4.2),
a Criteria were calculated assuming a QC check sample concentration of 20 ^g/L.
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits for recovery
have been broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
TABLE 3—-METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 602
Parameter
Ethylbenzene
Toluene
Accuracy, as
recovery, X'
(ng/L)
0 92C+0 57
0 95C+0 02
0 93C+0 52
0 96C - 0 05
0 93C - 0 09
0.94C+0.31
0.94C+0.65
Single analyst
precision, s'
(M9/L)
0 09X+0 59
0 09X+0 23
0 17X-004
0 15X-0 10
0 15X+028
0.17X+0.46
0.09X+0.48
Overall preci-
sion, S' ftjg/L)
0 21 X*0 56
017X+010
0 22X~0 53
0 1 9X-0 09
0 20X+0 41
0.26X+0.23
0.18X+0.71
X'=Expected recovery for one or more measurements of a sample containing a concentration of C, in ^jn/L
S*=Expeded single analyst standard deviation of measurements at an average concentration found of X, in X lag/
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in pg/L
C=True value lor the Concentration, in jig/L,
X-Average recovery found for measurements of samples containing a concentration ot C. in jig/L
61
-------
Pt. 136, App. A, Meth. 602
40 CFR Ch. I (7-1-04 Edition)
OPTIONAL
FOAM
TRAP
-EXIT 1/4 IN.
0. D,
—-14MM 0. D.
INLET % IN.
0. D.
V4 IN.
0, D. EXIT
SAMPLE INLET
2-WAY SYRINGE VALVE
17CM. 20 GAUGE SYRINGE NEEDLE
. 0. D. RUBBER SEPTUM
~10MM. 0. D.
-INLET
1/4 IN. 0. D.
1/16 IN. O.D.
/STAINLESS STEEL
13X MOLECULAR
SIEVE PURGE
GAS FILTER
PURGE GAS
FLOW
CONTROL
10MM GLASS FRIT
MEDIUM POROSITY
Figure 1. Purging device.
62
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 602
PACKING PROCEDURE
GLASS 5MM
WOOL
TENAX 23CM
3°/.OV-1
GLASS WOOL
CONSTRUCTION
COMPRESSION FITTING
NUT AND FERRULES
14FT.7A/FOOT RESISTANCE
'WIRE WRAPPED SOLID
THERMOCOUPLE/
CONTROLLER
SENSOR
TRAP INLET
ELECTRONIC
TEMPERATURE
CONTROL
AND
PYROMETER
TUBING 25CM.
0.105 IN. I.D.
0.125 IN. O.D.
STAINLESS STEEL
Figure 2. Trap packings and construction to include
desorb capability.
63
-------
Pt. 136, App. A, Meth. 602
40 CFR Ch. I (7-1-04 Edition)
Carrier Gas Flow Control Liquid Injection Ports
Pressure Regulator Y~*^ k*d
Purge Gas
Flow Control \i—
13X Molecular
Sieve Filter
Column Oven
., Confirmatory Column
To Detector
Analytical Column
Valve-3
Optional 4-Port Column
Selection Valve
Trap Inlet (Tenax End)
Resjstance Wire
Trap
22°C
, Heater Control
Note: All Lines Between
Trap and GC
Should be Heated
to 80°C
Valve-2
Figure 3. Purge and trap system - purge mode
Carrier Gas Flow Control
Pressure Regulator
Liquid Injection Ports
Purge Gas
Flow Control \
13X Molecular^
Sieve Filter
Column Oven
!_ , Confirmatory Column
]_/> To Detector
I "" -Analytical Column
Valve-3
Optional 4-Port Column
Selection Valve
Trap Inlet (Tenax End)
/ Resistance Wire
TraplkL Trap
'" 22°C
Heater Control
Note:
Valve-2
All Lines Between
Trap and GC
Should be Heated
to 80 °C
Figure 4. Purge and trap system-dry mode.
64
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Environmental Protection Agency
Pt. 136, App. A, Meth. 602
Carrier Gas Flow Control Liquid Injection Ports
Pressure Regulator \IiCIkiU_
Purge Gas
Flow Control \|—
Lj
13X Molecular _
Sieve Filter
Purging
Device
Column Oven
_ Confirmatory Column
To Detector
"~ Analytical Column
Valve-3
Optional 4-Port Column
Selection Valve
Valve-1 Jrap lnlet (Tenax End)
•** Resistance Wire
7*~
-Trap ( On
180°C
Heater Control
Note: All Lines Between
Trap and GC
Should be Heated
to 80°C
Varve-2
Figure 5. Purge and trap system-desorb mode.
g g Column: 5% SP 1200/1.75% Bentone
c N on Supelcoport
O « $ Program: 50 °C for 2 min.
,-•*>*—
§ £ P Detector: Photoionization,
o 3 e o
S ,° c 5=
3
0
1
15
•
~
e
u
i
«rf
UJ
^
.
J £ O
i|
o •"
— o
!§ -g
9 5
* A
LJ .
6°C/min to
10.2V
o
c
§
n
p
o
•5
5
/L
-34
90°C
.•> "•*
} 2 4 6 8 10 12 14 16 18 20 22 24 26 28
Retention Time, Min.
Figure 6. Gas chromatogram of purgeable aromatics.
65
-------
W. 136, App. A, Meth. 603
40 CFR Ch. I (7-1-04 idltion)
METHOD 603—ACROLEIN AND ACRYLONITRILE
1. Scope and Application
1,1 This method covers the determination
of acrolein and acrylonitrile. The following
parameters may be determined by this meth-
od:
Parameter
Acrvlonitrile
STORE!
No.
34210
34215
CAS No.
107-02-8
107-13-1
1,2 This is a purge and trap gas
ehromatographic (GO method applicable to
the determination of the compounds listed
above in municipal and industrial discharges
as provided under 40 CFR 136.1. When this
method is used to analyze unfamiliar sam-
ples for either or both of the compounds
above, compound identifications should be
supported by at least one additional quali-
tative technique. This method describes ana-
lytical conditions for a second gas
ehromatographic column that can be used to
confirm measurements made with the pri-
mary column. Method 624 provides gas chro-
matograph/mass spectrometer (GO/MS) con-
ditions appropriate for the qualitative and
quantitative confirmation of results for the
parameters listed above, if used with the
purge and trap conditions described in this
method.
1.3 The method detection limit (MDL, de-
fined in Section 12.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 138.5.
1,5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the operation of a purge and trap
system and a gas chromatograph and in the
interpretation of gas chromatograms. Each
analyst must demonstrate the ability to gen-
erate acceptable results with this method
using the procedure described in Section 8,2.
2. Summary of Method
2.1 An inert gas is bubbled through a 5-rnL
water sample contained in a heated purging
chamber. Acrolein and acrylonitrile are
transferred from the aqueous phase to the
vapor phase. The vapor is swept through a
sorbent trap where the analytes are trapped.
After the purge is completed, the trap is
heated and backflushed with the inert gas to
desorb the compound onto a gas
ehromatographic column. The gas chro-
matograph is temperature programmed to
separate the analytes which are then de-
tected with a flame ionization detector.2-'
2.2 The method provides an optional gas
ehromatographic column that may be help-
ful in resolving the compounds of interest
from the interferences that may occur,
3. Interferences
3.1 Impurities in the purge gas and or-
ganic compound outgassing from the plumb-
ing of the trap account for the majority of
contamination problems. The analytical sys-
tem must be demonstrated to be free from
contamination under the conditions of the
analysis by running laboratory reagent
blanks as described in Section 8.1.3. The use
of non-Teflon plastic tubing, non-Teflon
thread sealants, or flow controllers with rub-
ber components in the purge and trap system
should be avoided,
3.2 Samples can be contaminated by diffu-
sion of volatile organics through the septum
seal into the sample during shipment and
storage. A field reagent blank prepared from
reagent water and carried through the sam-
pling and handling protocol can serve as a
check on such contamination.
3,3 Contamination by carry-over can
occur whenever high level and low level sam-
ples are sequentially analyzed. To reduce
carry-over, the purging device and sample
syringe must be rinsed between samples with
reagent water. Whenever an unusually con-
centrated sample is encountered, it should be
followed by an analysis of reagent water to
check for cross contamination. For samples
containing large amounts of water-soluble
materials, suspended solids, high boiling
compounds or high analyte levels, it may be
necessary to wash the purging device with a
detergent solution, rinse it with distilled
water, and then dry it ia an oven at 105 "0 be-
tween analyses. The trap and other parts of
the system are also subject to contamina-
tion, therefore, frequent bakeout and purg-
ing of the entire system may be required.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method lias not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this view point, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified4-6 for
the information of the analyst.
66
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Environmental Protection Agency
Pt. 136, App. A, Meth. 603
5. Apparatus and Materials
5.1 Sampling equipment, for discrete sam-
pling.
5,1,1 Vial—25-mL capacity or larger,
equipped with a screw cap with a hole In the
center (Pierce #13075 or equivalent). Deter-
gent wash, rinse with tap and distilled water,
and dry at 105 °C before use.
5.1.2 Septum—Teflon-faced silicone
(Pierce #12722 or equivalent). Detergent
wash, rinse with tap and distilled water and
dry at 105 °0 for 1 h before use.
5,2 Purge and trap system—The purge and
trap system consists of three separate pieces
of equipment: a purging device, trap, and
desorber. Several complete systems are now
commercially available,
5.2.1 The purging device must be designed
to accept 5-mL, samples with a water column
at least 3 cm deep. The gaseous head space
between the water column and the trap must
have a total volume of less than 15 mL. The
purge gas must pass through the water col-
umn as finely divided bubbles with a diame-
ter of less than 3 mm at the origin. The
purge gas must be introduced no more than
5 mm from the base of the water column.
The purging device must be capable of being
heated to 85 °C within 3.0 min after transfer
of the sample to the purging device and
being' held at 85 ±2 °C during the purge cycle.
The entire water column in the purging de-
vice must be heated. Design of this modifica-
tion to the standard purging device is op-
tional, however, use of a water bath is sug-
gested.
5.2.1.1 Heating mantle—To be used to heat
water bath.
5.2.1.2 Temperature controller—Equipped
with thermocouple/sensor to accurately con-
trol water bath temperature to ±2 °C. The
purging device illustrated In Figure 1 meets
these design criteria.
5.2.2 The trap must be at least 25 cm long
and have an inside diameter of at least 0,105
in. The trap must be packed to contain 1,0
cm of methyl silicone coated packing (Sec-
tion 6.5.2) and 23 cm of 2,6-diphenylene oxide
polymer (Section 6.5.1). The minimum speci-
fications for the trap are illustrated in Fig-
ure 2.
5.2.3 The desorber must be capable of rap-
idly heating the trap to 180 "C, The desorber
illustrated in Figure 2 meets these design
criteria,
5.2.4 The purge and trap system may be
assembled as a separate unit as illustrated in
Figure 3 or be coupled to a gas chro-
matograph,
5.3 pH paper—Narrow pH range, about 3.5
to 5.5 (Fisher Scientific Short Range Alkacid
No. 2, #14-837-2 or equivalent).
5.4 Gas chromatogrraph—An analytical
system complete with a temperature pro-
grammable gas chromatograph suitable for
on-column injection and all required acces-
sories including syringes, analytical col-
umns, gases, detector, and strip-chart re-
corder. A data system is recommended for
measuring peak areas,
5.4.1 Column 1—10 ft long x 2 mm ID glass
or stainless steel, packed with Porapak-QS
(80/100 mesh) or equivalent. This column was
used to develop the method performance
statements in Section 12. Guidelines for the
use of alternate column packings are pro-
vided in Section 10.1.
5.4.2 Column 2—6 ft long x 0.1 in. ID glass
or stainless steel, packed with Chromosorb
101 (60/80 mesh) or equivalent.
5.4.3 Detector—Flame ionization detector.
This type of detector has proven effective in
the analysis of wastewaters for the param-
eters listed in the scope (Section 1.1), and
was used to develop the method performance
statements in Section 12. Guidelines for the
use of alternate detectors are provided in
Section 10.1.
5.5 Syringes—5-mL, glass hypodermic
with Luerlok tip (two each).
5.6 Micro syringes—25-jiL, 0.006 in. ID nee-
dle.
5.7 Syringe valve—2-way, with Luer ends
(three each).
5.8 Bottle—15-rnL, screw-cap, with Teflon
cap liner.
5.9 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
6. Reagents
6,1 Reagent water—Reagent water is de-
fined as a water in which, an interferent Is
not observed at the MDL of the parameters
of interest.
6.1.1 Reagent water can be generated by
passing tap water through a carbon filter bed
containing about 1 Ib of activated carbon
(Filtrasorb-300, Calg-on Corp., or equivalent).
6.1.2 A water purification system
(Millipore Super-Q or equivalent) may be
used to generate reagent water.
6.1,3 Regent water may also be prepared
by boiling water for 15 min. Subsequently,
while maintaining the temperature at 90 "C,
bubble a contaminant-free inert gas through
the water for 1 h. While still hot, transfer
the water to a narrow mouth screw-cap bot-
tle and seal with a Teflon-lined septum and
cap.
6.2 Sodium thiosulfate—(ACS) Granular.
6.3 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 mL,
6.4 Hydrochloric acid (1+1)—Slowly, add
50 mL of concentrated HC1 (ACS) to 50 mL of
reagent water.
6.5 Trap Materials:
6.5.1 2,6-Diphenylene oxide polymer—
Tenax (60/80 mesh), chromatographic grade
or equivalent,
6.5.2 Methyl silicone packing—3% OV-1 on
Chromosorb-W (60/80 mesh) or equivalent.
67
-------
Pt. 136, App. A, Meth. 603
40 CFR Ch, I (7-1-04 Edition)
6.6 Stock standard solutions—Stock
standard solutions may be prepared from
pure standard materials or purchased as cer-
tified solutions. Prepare stock standard solu-
tions in reagent water using assayed liquids.
Since acrolein and acrylonitrile are
lachrymators, primary dilutions of these
compounds should be prepared in a hood. A
NIOSH/MBSA approved toxic gas respirator
should be used when the analyst handles
high concentrations of such materials.
6.6.1 Place about 9.8 mL of reagent water
into a 10-mL ground glass stoppered volu-
metric flask. For acrolein standards the rea-
gent water must be adjusted to pH 4 to 5.
Weight the flask to the nearest 0.1 mg.
6.6.2 Using a 100-|iL syringe, immediately
add two or more drops of assayed reference
material to the flask, then reweigh. Be sure
that the drops fall directly into the water
without contacting the neck of the flask.
6.6.3 Reweigh, dilute to volume, stopper,
then mix by inverting the flask several
times. Calculate the concentration in ug/pL
from the net gain in weight. When compound
purity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock
staldard. Optionally, stock standard solu-
tions may be prepared using the pure stand-
ard material by volumetrically measuring
the appropriate amounts and determining
the weight of the material using the density
of the material. Commercially prepared
stock standards may be used at any con-
centration if they are certified by the
manufactaurer or by an independent source.
6.6.4 Transfer the stock standard solution
into a Teflon-sealed screw-cap bottle. Store
at 4 °C and protect from light.
6.6.5 Prepare fresh standards daily.
6.7 Secondary dilution standards—Using
stock standard solutions, prepare secondary
dilution standards In reagent water that con-
tain the compounds of interest, either singly
or mixed together. The secondary dilution
standards should be prepared at concentra-
tions such that the aqueous calibration
standards prepared in Section 7.3.1 or 7.4.1
will bracket the working range of the ana-
lytical system. Secondary dilution standards
should be prepared daily and stored at 4 °C.
6.8 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Assemble a purge and trap system that
meets the specifications in Section 5.2. Con-
dition the trap overnight at 180 °C by
backflushing with an inert gas flow of at
least 20 mL/min. Condition the trap for 10
min once daily prior to use.
7.2 Connect the purge and trap system to
a gas chromatograph. The gas chro-
matograph must be operated using tempera-
ture and flow rate conditions equivalent to
those given in Table 1. Calibrate the purge
and trap-gas chromatographic system using
either the external standard technique (Sec-
tion 7.3) or the internal standard technique
(Section 7.4).
7.3 External standard calibration proce-
dure:
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter by carefully adding 20.0 jiL of
one or more secondary dilution standards to
100, 500, or 1000 mL of reagent water. A 25-^L
syringe with a 0.006 in. ID needle should be
used for this operation. One of the external
standards should be at a concentration near,
but above, the MDL and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector. These standards must be pre-
pared fresh daily.
7.3.2 Analyze each calibration standard
according to Section 10, and tabulate peak
height or area responses versus the con-
centration of the standard. The results can
be used to prepare a calibration curve for
each compound. Alternatively, if the ratio of
response to concentration (calibration fac-
tor) is a constant over the working range (<
10% relative standard deviation, RSD), lin-
earity through the origin can be assumed
and the average ratio or calibration factor
can be used in place of a calibration curve.
7,4 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.4.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest as described in
Section 7.3.1.
7.4.2 Prepare a spiking solution con-
taining each of the internal standards using
the procedures described IE Sections 6.6 and
6.7. It is recommended that the secondary di-
lution standard be prepared at a concentra-
tion of 15 ug/mL of each internal standard
compound. The addition of 10 uL of this
standard to 5.0 mL of sample or calibration
standard would be equivalent to 30 ng/L.
7.4.3 Analyze each calibration standard
according to Section 10, adding 10 jiL of in-
ternal standard spiking solution directly to
the syringe (Section 10.4). Tabulate peak
height or area responses against concentra-
tion for each compound and internal stand-
ard, and calculate response factors (RP) for
each compound using Equation 1.
68
-------
Environmental Protection Agency
RF= (A,)(C,S) (A,5)(CS)
Equation 1
where:
As=Response for the parameter to be meas-
ured.
Ais=Response for the internal standard,
C«=Coneentration of the internal standard.
Cs=Concentration of the parameter to be
measured.
If the RP value over the working range is a
constant (<10% RSD), the RP can be assumed
to be invariant and the average RP can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, AS/A«, vs. RF.
7.5 The working calibration curve, cali-
bration factor, or RP must be verified on
each working- day by the measurement of a
QC check sample.
7.5.1 Prepare the QC check sample as de-
scribed in Section 8,2,2.
7.5.2 Analyze the QC check sample accord-
ing to Section 10.
7.5.3 For each parameter, compare the re-
sponse (Q) with the corresponding calibra-
tion acceptance criteria found in Table 2. If
the responses for all parameters of interest
fall within the designated ranges, analysis of
actual samples can begin. If any individual Q
falls outside the range, a new calibration
curve, calibration factor, or RF must be pre-
pared for that parameter according- to Sec-
tion 7.3 or 7.4.
8. Quality Control
8.1 Bach laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options {detailed in Sec-
tion 10.1) to improve the separations or lower
the cost of measurements. Bach time such a
Pt. 136, App. A, Meth. 603
modification is made to the method, tlie ana-
lyst is required to repeat the procedure in
Section 8.2.
8.1.3 Each day, the analyst must analyze a
reagent water blank to demonstrate that
interferences from the analytical system are
under control.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8,3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 25
jig/mL in reagent water. The QC check sam-
ple concentrate must be obtained from the
U.S. Environmental Protection Agency, En-
vironmental Monitoring and Support Lab-
oratory in Cincinnati, Ohio, if available. If
not available from that source, the QC check
sample concentrate must be obtained from
another external source. If not available
from either source above, the QC check sam-
ple concentrate must be prepared by the lab-
oratory using stock standards prepared inde-
pendently from those used for calibration.
8.2.2 Prepare a QC check sample to con-
tain 50 ug/L of each parameter by adding 200
liL of QC check sample concentrate to 100 mL
of reagent water.
8.2.3 Analyze four 5-mL aliquots of the
well-mixed QC check sample according to
Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in fig/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 3. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
either s exceeds the precision limit or X falls
outside the range for accuracy, the system
performance is unacceptable for that param-
eter, Locate and correct the source of the
69
-------
Pt. 136, App. A, Meth. 603
40 CFR Ch. 1 (7-1-04 Edition)
problem and repeat the test for each com-
pound of interest.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being; monitored to assess
accuracy. For laboratories analyzing one to
tea samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows;
8,3.1.1 If, as in compliance monitoring:,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 50 ug/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.2 Analyze one 5-mL sample aliquot to
determine the background concentration (B)
of each parameter. If necessary, prepare a
new QC check sample concentrate (Section
8.2.1) appropriate for the background con-
centrations in the sample. Spike a second 5-
mLi sample aliquot with 10 jil. of the QC
check sample concentrate and analyze it to
determine the concentration after spiking
(A) of each parameter. Calculate each per-
cent recovery (P) as 100(A-B)%/T, where T is
the known true value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 3. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that tie analyst's spike to back-
ground ratio approaches 5:1.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8,4,
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing- each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory,
8.4.1 Prepare the QC check standard by
adding 10 \iL of QC check sample concentrate
(Section 8.2.1 or 8.3.2) to 5 mL of reagent
water. The QC check standard needs only to
contain the parameters that failed criteria
in the test in Section 8.3,
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (P,) as 100 (A/T)%, where T is the true
value of the standard concentration.
8,4,3 Compare the percent recovery (F«)
for each parameter with the corresponding
QC acceptance criteria found in Table 3. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be oat of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery Interval from P - 2% to
P-t-2%, If P=90% and %=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such as
gas chromatography with a dissimilar col-
umn or mass spectrometer must be used.
Whenever possible, the laboratory should
analyze standard reference materials and
participate in relevant performance evalua-
tion studies.
S. Sample Collection, Preservation, and
Handling
9.1 All samples must be iced or refrig-
erated from the time of collection until anal-
ysis. If the sample contains free or combined
chlorine, add sodium thiosulfate preserva-
tive (10 mg/40 mL is sufficient for up to 5
ppm Clz) to the empty sample bottle just
prior to shipping to the sampling site, EPA
Methods 330.4 and 330.5 may be used for
measurement of residual chlorine.8 Field test
kits are available for this purpose.
9.2 If acrolein is to be analyzed, collect
about 500 mL of sample in a clean glass con-
tainer. Adjust the pH of the sample to 4 to 5
using acid or base, measuring with narrow
70
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 603
range pH paper. Samples for aeroleln anal-
ysis receiving no pH adjustment must be
analyzed within 3 days of sampling'.
9.3 Grab samples must be collected in
glass containers having a total volume of at
least 25 mL. Fill the sample bottle just to
overflowing in such a manner that no air
bubbles pass through the sample as the bot-
tle is being: filled. Seal the bottle so that no
air bubbles are entrapped in it. If preserva-
tive has been added, shake vigorously for 1
min. Maintain the hermetic seal on the sam-
ple bottle until time of analysis.
9.4 All samples must be analyzed within
14 days of collection.3
10. Procedure
10.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are esti-
mated retention times and MDL that can be
achieved under these conditions. An example
of the separations achieved by Column 1 is
shown in Figure 5. Other packed columns,
ehromatographie conditions, or detectors
may be used if the requirements of Section
8.2 are met.
10.2 Calibrate the system daily as de-
scribed in Section 7.
10.3 Adjust the purge gas (nitrogen or he-
lium) flow rate to 20 mL-min. Attach the
trap inlet to the purging device, and set the
purge and trap system to purge (Figure 3).
Open the syringe valve located on the purg-
ing device sample introduction needle.
10.4 Remove the plunger from a 5-mL sy-
ringe and attach a closed syringe valve. Open
the sample bottle (or standard) and carefully
pour the sample into the syringe barrel to
just short of overflowing. Replace the sy-
ringe plunger and compress the sample. Open
the syringe valve and vent any residual air
while adjusting the sample volume to 5.0 mL.
Since this process of taking an aliquot de-
stroys the validity of the sample for future
analysis, the analyst should fill a second sy-
ringe at this time to protect against possible
loss of data. Add 10.0 |iL of the internal
standard spiking solution (Section 7.4.2), if
applicable, through the valve bore then close
the valve.
10.5 Attach the syringe-syringe valve as-
sembly to the syringe valve on the purging
device. Open the syringe valves and inject
the sample into the purging chamber.
10.6 Close both valves and purge the sam-
ple for 15.0 ± 0.1 rnin while heating at 85 ± 2
°f
10.7 After the 15-min purge time, attach
the trap to the chrornatograph, adjust the
purge and trap system to the desorb mode
(Figure 4), and begin to temperature pro-
gram the gas chromatograph. Introduce the
trapped materials to the QC column by rap-
idly heating the trap to 180 °C while
backflushinir the trap with an inert gas be-
tween 20 and 60 mL/min for 1.5 min.
10.8 While the trap is being deserted into
the gas chromatograph, empty the purging
chamber using the sample introduction sy-
ringe. Wash the chamber with two 5-mL
Hushes of reagent water.
10.9 After desorbing the sample for 1.5
min, recondition the trap by returning the
purge and trap system to the purge mode.
Wait 15 s then close the syringe valve on the
purging device to begin gas flow through the
trap. The trap temperature should be main-
tained at 210 °C. After approximately 7 min,
turn off the trap heater and open the syringe
valve to stop the gas flow through the trap.
When the trap is cool, the next sample can
be analyzed.
10.10 Identify the parameters in the sam-
ple by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatogrrams.
11. Calculations
11.1 Determine the concentration of indi-
vidual compounds in the sample.
11.1.1 If the external standard calibration
procedure is used, calculate the concentra-
tion of the parameter being measured from
the peak response using the calibration
curve or calibration factor determined in
Section 7.3.2.
11.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.4.3 and Equa-
tion 2.
Concentration (|Hg/L) =
(AS)(C1S)
(A1S)(RF)
Equation 2
where:
As=Besponse for the parameter to be meas-
ured.
A,s=Response for the internal standard.
Cis=Concentration of the internal standard.
11.2 Report results in ug/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
12, Method Performance
12.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
71
-------
Pt. 136, App. A, Meth. 603
40 CFR Ch. I (7-1-04 Edition)
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983).
8. "Methods 330.4 (Titrimetric, DPD-PAS)
and 330.5 (Speetrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45Z68, March 1979.
9. "Evaluation of Method 603 (Modified),"
EPA-600/4-84-ABC, National Technical Infor-
mation Service, PB84-, Springfield, Virginia
22161, Nov. 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMITS
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.9
The MDL actually achieved in a given anal-
ysis will vary depending on instrument sen-
sitivity and matrix effects.
12.2 This method is recommended for the
concentration range from the MDL to
l,OOOxMDL. Direct aqueous injection tech-
niques should be used to measure concentra-
tion levels above l.OQOxMDL.
12.3 In a single laboratory (Battelle-Co-
lumbus), the average recoveries and standard
deviations presented in Table 2 were ob-
tained.9 Seven replicate samples were ana-
lyzed at each spike level.
References
1. 40 CPR part 136, appendix B.
2. Bellar, T.A., and Lichtenberg, J.J. "De-
termining Volatile Organics at Microgram-
per-Litre-Levels by Gas Chromatography,"
Journal American Water Works Association, 66,
739 (1974).
3. "Evaluate Test Procedures for Acrolein
and Acrylonitrile," Special letter report for
EPA Project 4719-A, U.S. Environmental
Protection Agency, Environmental Moni-
toring and Support Laboratory, Cincinnati,
Ohio 45268, 27 June 1979.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CPR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
TABLE 2—SINGLE LABORATORY ACCURACY AND PRECISION—METHOD 603
Acrylonitrile
Column 1
10.6
12.7
Column 2
82
9.8
0.7
0.5
Column 1 conditions: Porapak-QS (80/100 mesh) packed in
a 10 ft x 2 mm ID glass or stainless steel column with helium
earner gas at 30 nnL/rnin flow rate. Column temperature held
isothermal at 110 GC for 1.5 min (during desorption), then
heated as rapidly as possible to 150 °C and held for 20 min;
column bakeout at 190 °C for 10 rnin.9
Column 2 conditions: Chromosorb 101 (60/80 mesh)
packed in a 6 ft. x 0.1 in. ID glass or stainless steel column
with helium carrier gas at 40 rnL/min flow rate. Column tem-
perature held isothermal at SO °C for 4 min, then programmed
at 50 °C/min to 120 °C and held tor 12 min.
Parameter
Sample
matrix
RW
RW
POTW
POTW
IW
IW
RW
RW
POTW
POTW
IW
IW
Spike
cone.
(pg/L)
50
50.0
5.0
50.0
5.0
100.0
5.0
50.0
20.0
100.0
10.0
100.0
Average
recovery
(Mflfl-)
52
51.4
4.0
44.4
0.1
9.3
4,2
51.4
20.1
101.3
9.1
104.0
Standard
deviation
(MB"-)
02
0.7
0.2
0.8
0.1
1.1
0.2
1.5
0.8
1.5
0.8
3.2
Average
percent
recovery
104
103
80
89
2
9
84
103
100
101
91
104
ARW=Reagent water.
APOTW=Prechlorination secondary effluent from a municipal sewage treatment plant.
AIW=lndustrial wastewater containing an unidentified acrolein reactanl,
TABLE 3—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 603 A
Acrolein
Parameter
Range for Q
45.9-54.1
Limit for
S (ngrL)
4.6
Range for X
(M/L)
42.9-60.1
Range for
P, P. !%)
88-118
72
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 603
TABLE a—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 603*—Continued
Parameter
Acrylonitrile ..,,..... , , >,.,..,.„,.... ,..,,.,.,...
Range for Q
(H9/L)
41 .2-58.8
Limit for
S {(ig/L)
9.9
Range for X
((ig/L)
33.1-69.9
Range lot
P, P, (%)
71-135
«=Criteria were calculated assuming a QC check sample concentration ol SO \ig/L."-
Q=Concentration measured in QC check sample, in ng/L (Section 7.5.3).
s=Standard deviation of four recovery measurements, in ug/l_ (Section 8.2.4).
X=Average recovery for four recovery measurements, in pg/L (Section 8.2.4).
P, Ps=Percent recovery measured (Section 8.3.2, Section 8.4.2).
OPTIONAL
FOAM
TRAP
-EXIT V4 IN,
0, D.
—-14MM 0. D.
INLET % IN.
0. D.
'4 IN.
0, D. EXIT
SAMPLE INLET
2-WAY SYRINGE VALVE
17CM. 20 GAUGE SYRINGE NEEDLE
. 0. D. RUBBER SEPTUM
10MM. 0. D.
-INLET
!4 IN. 0. D.
1/16 IN. O.D
/STAINLESS STEEL
13X MOLECULAR
SIEVE PURGE
GAS FILTER
PURGE GAS
~"~|FLOW
CONTROL
1QMM GLASS FRIT
MEDIUM POROSITY
Figure 1, Purging device.
73
-------
Pt. 136, App. A, Meth. 603
40 CFR Ch. I (7-1-04 Edition)
PACKING PROCEDURE
GLASS
WOOL
TENAX 23CM
3% OV-1
GLASS WOOL
1CMJ
5MM
CONSTRUCTION
COMPRESSION FIHING
NUT AND FERRULES
14FT.7A/FOOT RESISTANCE
'WIRE WRAPPED SOLID
THERMOCOUPLE/
CONTROLLER
SENSOR
TRAP INLET
ELECTRONIC
TEMPERATURE
CONTROL
AND
PYROMETER
TUBING 25CM.
0.105 IN. I.D.
0.125 IN. O.D.
STAINLESS STEEL
Figure 2. Trap packings and construction to include
desorb capability.
74
-------
Environmental Protection Agency
Pt. 136, App. A,Meth. 603
13X MOLECULAR
SIEVE FILTER
GC INJECTION
PORT
HEATED
WATER BATH
Figure 3. Purge and trap system-purge mode.
13X MOLECULAR
SIEVE FILTER
GC INJECTION
PORT
PURGE
FLOW
CONTROLLER
k GC FLOW
CONTROLLER
2 POSITION
6-PORT VALVE
COUNTER-
CLOCKWISE
ROTATION
Figure 4. Purge and trap system-desorb mode.
75
-------
Pt. 136, App. A, Meth. 604
40 CFR Ch. I (7-1-04 Edition)
Column: Porapak-QS
Program: 110°C for 1.5 min, rapidly
heated to 150°C
Detector: Flame lonization
I
4.5
I
6.0
II I I I I
7.5 9.0 10.5 12.0 13.5 15.0
1.5 3.0
RETENTION TIME, MIN.
Figure 5. Gas chromatogram of acrolein and acrylonitrile.
METHOD 604—PHENOLS
1. Scope and Application
1.1 This method covers the determination
of phenol and certain substituted phenols.
The following parameters may be deter-
mined by this method:
Parameter
4-Chloro-3-methylphenol
2— Chlorophenol
2,4-Dichlorophenol
2,4-Dimethylphenol
2,4-Dinitrophenol
2-Methyl-4,6-dinitrophenol
2-Nitrophenol
4-Nitrophenol
Phenol
2,4,6-Trichlorophenol
STORE!
No.
34452
34586
34601
34606
34616
34657
34591
34646
39032
34694
34621
CAS No.
59-50-7
95-57-8
120-83-2
105-67-9
51-28-5
534-52-1
88-75-5
100-02-7
87-86-5
108-95-2
88-06-2
1.2 This is a flame ionization detector gas
chromatographic (FIDGC) method applicable
to the determination of the compounds listed
above in municipal and industrial discharges
as provided under 40 CFR 136.1. When this
method is used to analyze unfamiliar sam-
ples for any or all of the compounds above,
compound identifications should be sup-
ported by at least one additional qualitative
technique. This method describes analytical
conditions for derivatization, cleanup, and
electron capture detector gas chroma-
tography (ECDGC) that can be used to con-
firm measurements made by FIDGC. Method
625 provides gas chromatograph/mass spec-
trometer (GC/MS) conditions appropriate for
the qualitative and quantitative confirma-
tion of results for all of the parameters list-
ed above, using the extract produced by this
method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix. The MDL listed in Table
1 for each parameter was achieved with a
flame ionization detector (FID). The MDLs
that were achieved when the derivatization
cleanup and electron capture detector (BCD)
were employed are presented in Table 2.
76
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 604
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is acidified and extracted
with methylene chloride using a separatory
funnel. The methylene chloride extract is
dried and exchanged to 2-propanol during
concentration to a volume of 10 mL or less.
The extract is separated by gas chroma-
tography and the phenols are then measured
with an FID.2
2.2 A preliminary sample wash under
basic conditions can be employed for samples
having high general organic and organic base
interferences.
2.3 The method also provides for a
derivatization and column chromatography
cleanup procedure to aid in the elimination
of interferences.2-3 The derivatives are ana-
lyzed by BCDGC.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.4 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are coextracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The derivatization cleanup proce-
dure in Section 12 can be used to overcome
many of these interferences, but unique sam-
ples may require additional cleanup ap-
proaches to achieve the MDL listed in Tables
1 and 2.
3.3 The basic sample wash (Section 10.2)
may cause significantly reduced recovery of
phenol and 2,4-dimethylphenol. The analyst
must recognize that results obtained under
these conditions are minimum concentra-
tions.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling-
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified5 7 for
the information of analyst.
4.2 Special care should be taken in han-
dling pentafluorobenzyl bromide, which is a
lachrymator, and 18-crown-6-ether, which is
highly toxic.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Tenon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4°C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
77
-------
Pt. 136, App. A, Meth. 604
40 CFR Ch. I (7-1-04 Edition)
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2-L, with Teflon
stopcock.
5.2.2 Drying column—Chromatographic
column, 400 mm long x 19 mm ID, with coarse
frit filter disc.
5.2.3 Chromatographic column—100 mm
long x 10 mm ID, with Teflon stopcock.
5.2.4 Concentrator tube, Kuderna-Dan-
ish—10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.6 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.7 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5.2.8 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.2.9 Reaction flask—15 to 25-mL round
bottom flask, with standard tapered joint,
fitted with a water-cooled condenser and U-
shaped drying tube containing granular cal-
cium chloride.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2°C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighting 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with a temperature pro-
grammable gas chromatograph suitable for
on-column injection and all required acces-
sories including syringes, analytical col-
umns, gases, detector, and strip-chart re-
corder. A data system is recommended for
measuring peak areas.
5.6.1 Column for underivatized phenols—
1.8 m long x 2 mm ID glass, packed with 1%
SP-1240DA on Supelcoport (80/100 mesh) or
equivalent. This column was used to develop
the method performance statements in Sec-
tion 14. Guidelines for the use of alternate
column packings are provided in Section
11.1.
5.6.2 Column for derivatized phenols—1.8
m long x 2 mm ID glass, packed with 5% OV-
17 on Chromosorb W-AW-DMCS (80/100 mesh)
or equivalent. This column has proven effec-
tive in the analysis of wastewaters for
derivatization products of the parameters
listed in the scope (Section 1.1), and was used
to develop the method performance state-
ments in Section 14. Guidelines for the use of
alternate column packings are provided in
Section 11.1.
5.6.3 Detectors—Flame ionization and
electron capture detectors. The FID is used
when determining the parent phenols. The
ECD is used when determining the
derivatized phenols. Guidelines for the use of
alternatve detectors are provided in Section
11.1.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 mL.
6.3 Sodium hydroxide solution (1 N)—Dis-
solve 4 g of NaOH (ACS) in reagent water and
dilute to 100 mL.
6.4 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400°C for 4 h in
a shallow tray.
6.5 Sodium thiosulfate—(ACS) Granular.
6.6 Sulfuric acid (1+1)—Slowly, add 50 mL
of H2SO4 (ACS, sp. gr. 1.84) to 50 mL of rea-
gent water.
6.7 Sulfuric acid (1 N)—Slowly, add 58 mL
of H2SO4 (ACS, sp. gr. 1.84) to reagent water
and dilute to 1 L.
6.8 Potassium carbonate—(ACS) Pow-
dered.
6.9 Pentafluorobenzyl bromide (ot-
Bromopentafluorotoluene)—97% minimum
purity.
NOTE: This chemical is a lachrymator. (See
Section 4.2.)
6.10 18-crown-6-ether (1,4,7,10,13,16-
Hexaoxacyclooctadecane)—98% minimum
purity.
NOTE: This chemical is highly toxic.
6.11 Derivatization reagent—Add 1 mL of
pentafluorobenzyl bromide and 1 g of 18-
crown-6-ether to a 50-mL volumetric flask
and dilute to volume with 2-propanol. Pre-
pare fresh weekly. This operation should be
carried out in a hood. Store at 4 °C and pro-
tect from light.
6.12 Acetone, hexane, methanol, meth-
ylene chloride, 2-propanol, toluene—Pes-
ticide quality or equivalent.
6.13 Silica gel—100/200 mesh, Davison,
grade-923 or equivalent. Activate at 130 °C
overnight and store in a desiccator.
6.14 Stock standard solutions (1.00 \ig/
HL)—Stock standard solutions may be pre-
pared from pure standard materials or pur-
chased as certified solutions.
6.14.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in 2-propanol
78
-------
Environmental Protection Agency
Pt. 136, App. A.Meth. 604
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can tie used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.14.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially Just prior to preparing
calibration standards from them.
6.14,3 Stock standard solutions must be
replaced after six months, or sooner if com-
parison with check standards indicates a
problem.
6.15 Quality control check sample con-
centrate—See Section 8.2,1,
7. Calibration
7.1 To calibrate the FIDGC for the
anaylsis of underivatized phenols, establish
gas chromatographic operating conditions
equivalent to those given in Table 1. The gas
chromatographic system can be calibrated
using the external standard technique (Sec-
tion 7.2) or the internal standard technique
(Section 7.3).
7.2 External standard calibration proce-
dure for FIDGC:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
2-propanol. One of the external standards
should be at a concentration near, but above,
the MDD (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2.2 Using injections of 2 to 5 jil, analyze
each calibration standard according to Sec-
tion 11 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound, Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure for FIDGC—To use this approach, the
analyst must select one or more internal
standards that are similar in analytical be-
havior to the compounds of interest. The an-
alyst must further demonstrate that the
measurement of the internal standard is not
affected by method or matrix interferences.
Because of these limitations, no internal
standard can be suggested that is applicable
to all samples.
7.3,1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with 2-propanol, One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 2 to 5 (iL, analyze
each calibration standard according to Sec-
tion 11 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (RP) for each compound using
Equation 1.
BF= (AiXCu) (A,«)(CS)
Equation 1
where:
As=Response for the parameter to be meas-
ured.
Ais=Response for the internal standard.
C,s=Concentration of the internal standard
Cs=Concentration of the parameter to be
measured (jig/L).
If the RF value over the working range is
a constant (<10% RSD), the RF can be as-
sumed to be invariant and the average RF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, AJA^,, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound.
7,5 To calibrate the ECDGC for the anal-
ysis of phenol derivatives, establish gas
chromatographic operating conditions equiv-
alent to those given in Table 2.
7.5.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
2-propanol. One of the external standards
should be at a concentration near, but above.
the MDL (Table 2) and the other concentra-
tions should correspond to the expected
79
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Pt. 136, App. A, Meth. 604
40 CFR Ch. I (7-1-04 Edition)
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.5.2 Each time samples are to be
derivatized, simultaneously treat a 1-mL ali-
quot of each calibration standard as de-
scribed in Section 12.
7.5.3 After derivatization, analyze 2 to 5
HL of each column eluate collected according
to the method beginning in Section 12.8 and
tabulate peak height or area responses
against the calculated equivalent mass of
underivatized phenol injected. The results
can be used to prepare a calibration curve for
each compound.
7.6 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.6 and 11.1) to improve the separa-
tions or lower the cost of measurements.
Each time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 100
|ig/mL in 2-propanol. The QC check sample
concentrate must be obtained from the U.S.
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at a concentration of 100 jig/L by adding
1.00 mL of QC check sample concentrate to
each of four 1-L aliquots of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according- to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in ng/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 3. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Talbe 3 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.2.
80
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Environmental Protection Agency
Pt. 136, App. A, Meth. 604
8.2,6.2 Beginning with Section 8.2.2, repeat
tie test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 100 ug/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any, or, if
none, (2) the larger of either 5 times higher
than the expected background concentration
or 100 fig/L.
8.3,2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze It to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100(A-B)%/T, where T Is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 3, These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.8 If spiking was
performed at a concentration lower than 100
WT/L, the analyst must use either the QC ac-
ceptance criteria in Table 3, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 4, substituting
the spike concentration (T) for C; (2) cal-
culate overall precision (S') using the equa-
tion in Table 4, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X7T)±2.44(100 S'/T)%.8
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 3. Only
parameters that failed the test In Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P - 2sp to
P+2sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6. It is recommended that the labora-
tory adopt additional quality assurance
practices for use with this method. The spe-
cific practices that are most productive de-
pend upon the needs of the laboratory and
the nature of the samples. Field duplicates
81
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Pt. 136, App. A, Meth. 604
40 CFR Ch. I (7-1-04 Edition)
may be analyzed to assess the precision of
the environmental measurements. When
doubt exists over the identification of a peak
on the chromatogram, confirmatory tech-
niques such as gas chromatography with a
dissimilar column, specific element detector,
or mass spectrometer must be used. When-
ever possible, the laboratory should analyze
standard reference materials and participate
in relevant performance evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 G-rab samples must be collected in
glass containers. Conventional sampling
practices9 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4 °C from the time of collection
until extraction. Fill the sample bottles and,
if residual chlorine is present, add 80 mg of
sodium thiosulfate per liter of sample and
mix well. EPA Methods 330.4 and 330.5 may
be used for measurement of residual chlo-
rine.10 Field test kits are available for this
purpose.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
10. Sample Extraction
10.1 Mark the water meniscus on the side
of sample bottle for later determination of
sample volume. Pour the entire sample into
a 2-L separatory funnel.
10.2 For samples high in organic content,
the analyst may solvent wash the sample at
basic pH as prescribed in Sections 10.2.1 and
10.2.2 to remove potential method inter-
ferences. Prolonged or exhaustive contact
with solvent during the wash may result in
low recovery of some of the phenols, notably
phenol and 2,4-dimethylphenol. For rel-
atively clean samples, the wash should be
omitted and the extraction, beginning with
Section 10.3, should be followed.
10.2.1 Adjust the pH of the sample to 12.0
or greater with sodium hydroxide solution.
10.2.2 Add 60 mL of methylene chloride to
the sample by shaking the funnel for 1 min
with periodic venting to release excess pres-
sure. Discard the solvent layer. The wash
can be repeated up to two additional times if
significant color is being removed.
10.3 Adjust the sample to a pH of 1 to 2
with sulfuric acid.
10.4 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask.
10.5 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner.
10.6 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.7 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Erlenmeyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.8 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.9 Increase the temperature of the hot
water bath to 95 to 100 °C. Remove the
Synder column and rinse the flask and its
lower joint into the concentrator tube with 1
to 2 mL of 2-propanol. A 5-mL syringe is rec-
ommended for this operation. Attach a two-
ball micro-Snyder column to the concen-
trator tube and prewet the column by adding
about 0.5 mL of 2-propanol to the top. Place
the micro-K-D apparatus on the water bath
so that the concentrator tube is partially
immersed in the hot water. Adjust the
vertical position of the apparatus and the
water temperature as required to complete
82
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Environmental Protection Agency
Pt. 136, App. A, Meth. 604
concentration in 5 to 10 min. At the proper
rate of distillation the balls of the column
will actively chatter but the chambers will
not flood. When the apparent volume of liq-
uid reaches 2.5 mL, remove the K-D appa-
ratus and allow it to drain and cool for at
least 10 min. Add an additional 2 mL of 2-
propanol through the top of the micro-Sny-
der column and resume concentrating as be-
fore. When the apparent volume of liquid
reaches 0.5 mL, remove the K-D apparatus
and allow it to drain and cool for at least 10
min.
10.10 Remove the micro-Snyder column
and rinse its lower joint into the concen-
trator tube with a minimum amount of 2-
propaaol. Adjust the extract volume to 1.0
mL. Stopper the concentrator tube and store
refrigerated at 4 °C if further processing will
not be performed immediately. If the extract
will be stored longer than two days, it should
be transferred to a Teflon-sealed screw-cap
vial. If the sample extract requires no fur-
ther cleanup, proceed with FIDGC analysis
{Section 11). If the sample requires further
cleanup, proceed to Section 12.
10.11 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Flame lonization Detector Gas
Chromatography
11.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograpli. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. An example of the
separations achieved by this column is
shown in Figure 1. Other packed or capillary
(open-tubular) columns, chromatographic
conditions, or detectors may be used if the
requirements of Section 8,2 are met.
11.2 Calibrate the system daily as de-
scribed in Section 7.
11.3 If the internal standard calibration
procedure is used, the internal standard
must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph.
11.4 Inject 2 to 5 nL of the sample extract
or standard into the gas chromatograph
using tie solvent-flush technique." Smaller
(1.0 jiL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 |iL, and the
resulting peak size in area or peak height
units.
11.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample ehromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound may be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
11.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
11.7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, an alternative gas chromatographic
procedure is required. Section 12 describes a
derivatization and column chromatographic
procedure which has been tested and found
to be a practical means of analyzing phenols
in complex extracts.
12. Derivatization and Electron Capture.
Detector Gas Chromatography
12.1 Pipet a 1.0-mL aliquot of the 2-pro-
panol solution of standard or sample extract
into a glass reaction vial. Add 1.0 mL of
derivatizing reagent (Section 6.11). This
amount of reagent is sufficient to derivatize
a solution whose total phenolic content does
not exceed 0.3 mg/mL.
12.2 Add about 3 mg of potassium car-
bonate to the solution and shake gently.
12.3 Cap the mixture and heat it for 4 h at
80 °C in a hot water bath.
12,4 Bemove the solution from the hot
water bath and allow it to cool.
12.5 Add 10 mL of hexane to the reaction
flask and shake vigorously for 1 min. Add 3.0
mL of distilled, deionized water to the reac-
tion flask and shake for 2 min. Decant a por-
tion of the organic layer into a concentrator
tube and cap with a glass stopper.
12.6 Place 4.0 g of silica gel into a
chromatographic column. Tap the column to
settle the silica gel and add about 2 g of an-
hydrous sodium suUate to the top.
12.7 Preelute the column with 6 mL of
hexane. Discard the eluate and just prior to
exposure of the sodium sulfate layer to the
air, pipet onto the column 2.0 mL of the
hexane solution (Section 12.5) that contains
the derivatized sample or standard. Elute the
column with 10.0 mL of hexane and discard
the eluate. Elute the column, in order, with:
10.0 mL of 15% toluene in hexane (Fraction
1); 10.0 mL of 40% toluene in hexane (Frac-
tion 2); 10,0 mL of 75% toluene in hexane
(Fraction 3); and 10.0 mL of 15% 2-propanol
in toluene (Fraction 4). All elution mixtures
are prepared on a volume: volume basis.
Elution patterns for the phenolic derivatives
are shown in Table 2. Fractions may be com-
bined as desired, depending upon the specific
phenols of interest or level of interferences.
12,8 Analyze the fractions by ECDG-C.
Table 2 summarizes the recommended oper-
ating conditions for the gas chromatograph.
Included in this table are retention times
and MDL that can be achieved under these
conditions. An example of the separations
83
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Pt. 136, App. A, Meth. 604
40 CFR Ch. I (7-1-04 Edition)
achieved by this column is shown in Figure
2.
12.9 Calibrate the system daily with a
minimum of three aliquots of calibration
standards, containing each of the phenols of
interest that are derivatized according to
Section 7.5.
12.10 Inject 2 to 5 H.L of the column frac-
tions into the gas chromatograph using the
solvent-flush technique. Smaller (1.0 |iL) vol-
umes can be injected if automatic devices
are employed. Record the volume injected to
the nearest 0.05 nL, and the resulting peak
size in area or peak height units. If the peak
response exceeds the linear range of the sys-
tem, dilute the extract and reanalyze.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample analyzed by
FIDGC (without derivatization) as indicated
below.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (ng/L) =
(A)(Vt)
Equation 2
where:
A=Amount of material injected (ng).
Vi=Volume of extract injected (|J.L).
Vi=Volume of total extract (|J.L).
V5=Volume of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (ng/L) =
(A.XI.)
(A1S)(RF)(V0)
Equation 3
where:
As=Response for the parameter to be meas-
ured.
AiS=Response for the internal standard.
L=Amount of internal standard added to
each extract (ng).
V0=Volume of water extracted (L).
13.2 Determine the concentration of indi-
vidual compounds in the sample analyzed by
derivatization and ECDGC according to
Equation 4.
Concentration (|ig/L) =
(A)(Vt)(B)(D)
Equation 4
where:
A=Mass of underivatized phenol represented
by area of peak in sample chromatogram,
determined from calibration curve in Sec-
tion 7.5.3 (ng).
V;=Volume of eluate injected (nL).
V,=Total volume of column eluate or com-
bined fractions from which V( was taken
Vs=Volume of water extracted in Section
10.10 (mL).
B=Total volume of hexane added in Section
12.5 (mL).
C=Volume of hexane sample solution added
to cleanup column in Section 12.7 (mL).
D=Total volume of 2-propanol extract prior
to derivatization (mL).
E=Volume of 2-propanol extract carried
through derivatization in Section 12.1
(mL).
13.3 Report results in |ig/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in Ta-
bles 1 and 2 were obtained using reagent
water.12 Similar results were achieved using
representative wastewaters. The MDL actu-
ally achieved in a given analysis will vary
depending on instrument sensitivity and ma-
trix effects.
14.2 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked as six concentrations
over the range 12 to 450 ug/L.13 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships for a flame ionization detector are pre-
sented in Table 4.
References
1. 40 CFR part 136, appendix B.
2. "Determination of Phenols in Industrial
and Municipal Wastewaters," EPA 600/4-84-
ABC, National Technical Information Serv-
ice, PBXYZ, Springfield, Virginia 22161, No-
vember 1984.
3. Kawahara, F. K. "Microdetermination of
Derivatives of Phenols and Mercaptans by
84
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 604
11. Burke, J. A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
12. "Development of Detection Limits, EPA
Method 604, Phenols," Special letter report
for EPA Contract 68-03-2625, U.S. Environ-
mental Protection Agency, Environmental
Monitoring and Support Laboratory, Cin-
cinnati, Ohio 45268.
13. "EPA Method Study 14 Method 604-Phe-
nols," EPA 600/4-84-044, National Technical
Information Service, PB84-196211, Spring-
field, Virginia 22161, May 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMITS
Means of Electron Capture Gas Chroma-
tography," Analytical Chemistry, 40, 1009
(1968).
4. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
5. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
6. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
7. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
8. Provost, L. P., and Elder, R. S. "Inter-
pretation of Percent Recovery Data," Amer-
ican Laboratory, 15, 58-63 (1983). (The value
2.44 used in the equation in Section 8.3.3 is
two times the value 1.22 derived in this re-
port.)
9. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
10. "Methods 330.4 (Titrimetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methmds for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979.
TABLE 2—SILICA GEL FRACTIONATION AND ELECTRON CAPTURE GAS CHROMATOGRAPHY OF PFBB
DERIVATIVES
Parameter
2-Nitrophenol
Phenol
2,4-Dimethylphenol
2,4,6-Trichlorophenol
4-Chloro-3-methylphenol
2,4-Dinitrophenol
2-Methyl-4,6-dinitrophenol
4-Nitrophenol
Retention
time (min)
1 70
2.00
3.01
4.03
430
6.05
7.50
10.00
10.24
1242
24.25
Method de-
tection limit
(H9/L)
031
0.45
0.14
0.32
039
0.64
0.36
13.0
16.0
74
2.8
Column conditions: Supelcoport (80/100 mesh) coated with
1% SP-1240DA packed in a 1.8 m long x 2 mm ID glass col-
umn with nitrogen carrier gas at 30 mL/min flow rate. Column
temperature was 80 °C at injection, programmed immediately
at 8 °C/min to 150 °C final temperature. MDL were deter-
mined with an FID.
Parent compound
2-Chlorophenol
2-Nitrophenol
Phenol
2,4,6-Trichlorophenol
4-Nitroohenol
Percent recovery by frac-
tion a
1
50
75
2
90
90
95
95
50
84
20
3
1
9
10
7
1
14
1
4
90
90
Retention
time (min)
3.3
9.1
1.8
2.9
5.8
7.0
4.8
28.8
14.0
Method
detection
limit (ng/L)
0.58
0.77
2.2
0.63
0.68
0.58
1.8
0.59
0.70
Column conditions: Chromosorb W-AW-DMCS (80/100 mesh) coated with 5% OV-17 packed in a 1.8 m long x 2.0 mm ID
glass column with 5% methane/95% argon carrier gas at 30 mL/min flow rate. Column temperature held isothermal at 200 °C.
MDL were determined with an ECD.
aEluant composition:
Fraction 1—15% toluene in hexane.
Fraction 2—40% toluene in hexane.
Fraction 3—75% toluene in hexane.
Fraction 4—15% 2-propanol in toluene.
85
-------
Pt. 136, App. A, Meth. 604
40 CFRCh. I (7-1-04 Edition)
TABLE 3—QC ACCEPTANCE CRITERIA—METHOD 604
Parameter
2-Chloropheno!
2,4-Dichlorophenol
4,6-Dinitro-2-methylphenol
Phenol
2.4.6-TrichloroDhenol
Test
cone.
(H9/L)
100
100
100
100
100
100
100
100
100
100
100
Limit for s
(H9/L)
166
27.0
25.1
333
25.0
360
22.5
19.0
324
14.1
16.6
Range for X
(ra/L)
56 7-1134
54.1-110.2
59.7-103.3
50 4-1 00 0
42.4-123.6
31 7-125 1
56.6-103.8
22.7-100.0
56 7-1 1 3 5
32.4-100.0
60.8-110.4
Range for
P, P, (per-
cent)
49-122
38-126
44-119
24-1 1 8
30-1 36
12-145
43-117
13-110
36-134
23-108
53-119
s—Standard deviation of four recovery measurements, in (ig/L (Section 8.2.4).
X—Average recovery for four recovery measurements, in |ig/L (Section 8.2.4).
P, Ps—Percent recovery measured (Section 8.3.2, Section 8.4.2}.
NOTE: These criteria are based directly upon the method performance data in Table 4. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 4.
TABLE 4—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 604
Parameter
2-Chlorophenol
4,6-Dinitro-2-methylphenol
4-Nitrophenol
Phenol
2,4,6-Trichlorophenol
Accuracy, as re-
covery, X' (|ag/L)
0 87C-1 97
0.83C-0.84
081C+048
0 62C-1 64
0.84C-1.01
080C-1.58
081C-076
0.46C+0.18
0.83C+2.07
0 43C+0 1 1
0.86C-0.40
Single Analyst
precision, sr' (ng/
L)
0 11X-021
0.18X+0.20
0 17X-002
0 30X-0 89
0.15X+1.25
0.27X-1.15
0 1 5X+0 44
0.17X+2.43
0.22X-0.58
0 20X-0 88
0.10X+0.53
Overall precision,
S' (ng/L)
0 16X+1 41
021X+0.75
0 18X+062
0 25X+0 48
0.19X+5.85
0 29X+4 51
0 14X+384
0.19X+4.79
0 23X+0 57
0 1 7X+0 77
0.13X+2.40
X'=Expected recovery for one or more measurements of a sample containing a concentration of C, in \ig/L.
sr'=Expected single analyst standard deviation of measurements at an average concentration found of X, in n
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
C=True value for the concentration, in ng/L
X=Average recovery found for measurements of samples containing a concentration of C, in ng/L.
86
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 604
o
5
LLJ
=iO TZ
COLUMN: 1% SP-1240DA ON SUPELCOPORT
PROGRAM: 80°C AT INJECTION. IMMEDIATE 8°C/MIN TO 150°C
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i
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CN
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i
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1
1
1
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i
DETECTOR: FLAME IONIZATION
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i £
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I2 J _,Z
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-------
Pt. 136, App. A, Meth. 605
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 5% OV-17 ON CHROMOSORB W-AW-DMCS
TEMPERATURE: 200'C.
DETECTOR: ELECTRON CAPTURE
0
z
o
5
LLJ
a.
8 12 16 20 24 28
RETENTION TIME, MIN.
32
Figure 2. Gas chromatogram of PFB derivatives of phenols.
METHOD 605—BBNZIDINBS
1. Scope and Application
1.1 This method covers the determination
of certain benzidines. The following param-
eters can be determined by this method:
Parameter
3.3'-Dichlorobenzidine
Storet No
39120
34631
CAS No.
92-87-5
91-94-1
1.2 This is a high performance liquid chro-
matography (HPLC) method applicable to
the determination of the compounds listed
above in municipal and industrial discharges
as provided under 40 CFR 136.1. When this
method is used to analyze unfamiliar sam-
ples for the compounds above, identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes electrochemical conditions at a
second potential which can be used to con-
firm measurements made with this method.
Method 625 provides gas chromatograph/mass
spectrometer (GC/MS) conditions appro-
priate for the qualitative and quantitative
confirmation of results for the parameters
listed above, using the extract produced by
this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)' for each parameter is
88
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 605
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of the interferences
in the sample matrix.
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of HPLC instrumentation
and in the interpretation of liquid
chromatograms. Each analyst must dem-
onstrate the ability to generate acceptable
results with this method using the procedure
described in Section 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with chloro-
form using liquid-liquid extractions in a
separatory funnel. The chloroform extract is
extracted with acid. The acid extract is then
neutralized and extracted with chloroform.
The final chloroform extract is exchanged to
methanol while being concentrated using a
rotary evaporator. The extract is mixed with
buffer and separated by HPLC. The benzidine
compounds are measured with an electro-
chemical detector.2
2.2 The acid back-extraction acts as a
general purpose cleanup to aid in the elimi-
nation of interferences.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as
possible after use by rinsing with the last
solvent used in it. Solvent rinsing should be
followed by detergent washing with hot
water, and rinses with tap water and
distilled water. The glassware should then be
drained dry, and heated in a muffle furnace
at 400 °C for 15 to 30 min. Some thermally
stable materials may not be eliminated by
this treatment. Solvent rinses with acetone
and pesticide quality hexane may be substi-
tuted for the muffle furnace heating. Vol-
umetric ware should not be heated in a muf-
fle furnace. After drying and cooling, glass-
ware should be sealed and stored in a clean
environment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedures that are in-
herent in the extraction step are used to
overcome many of these interferences, but
unique samples may require additional
cleanup approaches to achieve the MDL list-
ed in Table 1.
3.3 Some dye plant effluents contain large
amounts of components with retention times
closed to benzidine. In these cases, it has
been found useful to reduce the electrode po-
tential in order to eliminate interferences
and still detect benzidine. (See Section 12.7.)
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health harzard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified 4-6 for
the information of the analyst.
4.2 The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens: benzidine and 3,3'-
dichlorobenzidine. Primary standards of
these toxic compounds should be prepared in
a hood. A NIOSH/MESA approved toxic gas
respirator should be worn when the analyst
handles high concentrations of these toxic
compounds.
4.3 Exposure to chloroform should be
minimized by performing all extractions and
extract concentrations in a hood or other
well-ventiliated area.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
89
-------
Pt. 136, App. A, Meth. 605
40 CFR Ch. I (7-1-04 Edition)
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4°C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested):
5.2.1 Separatory funnels—2000, 1000, and
250-mL, with Teflon stopcock.
5.2.2 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.2.3 Rotary evaporator.
5.2.4 Flasks—Round bottom, 100-mL, with
24/40 joints.
5.2.5 Centrifuge tubes—Conical, grad-
uated, with Teflon-lined screw caps.
5.2.6 Pipettes—Pasteur, with bulbs.
5.3 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.4 High performance liquid chro-
matograph (HPLC)—An analytical system
complete with column supplies, high pres-
sure syringes, detector, and compatible re-
corder. A data system is recommended for
measuring peak areas and retention times.
5.4.1 Solvent delivery system—With pulse
damper, Altex 110A or equivalent.
5.4.2 Injection valve (optional)—Waters
U6K or equivalent.
5.4.3 Electrochemical detector—
Bioanalytical Systems LC-2A with glassy
carbon electrode, or equivalent. This detec-
tor has proven effective in the analysis of
wastewaters for the parameters listed in the
scope (Section 1.1), and was used to develop
the method performance statements in Sec-
tion 14. Guidelines for the use of alternate
detectors are provided in Section 12.1.
5.4.4 Electrode polishing kit—Princeton
Applied Research Model 9320 or equivalent.
5.4.5 Column—Lichrosorb RP-2, 5 micron
particle diameter, in a 25 cm x 4.6 mm ID
stainless steel column. This column was used
to develop the method performance state-
ments in Section 14. Guidelines for the use of
alternate column packings are provided in
Section 12.1.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium hydroxide solution (5 N>—Dis-
solve 20 g of NaOH (ACS) in reagent water
and dilute to 100 mL.
6.3 Sodium hydroxide solution (1 M)—Dis-
solve 40 g of NaOH (ACS) in reagent water
and dilute to 1 L.
6.4 Sodium thiosulfate—(ACS) Granular.
6.5 Sodium tribasic phosphate (0.4 M)—
Dissolve 160 g of trisodium phosphate deca-
hydrate (ACS) in reagent water and dilute to
1L.
6.6 Sulfuric acid (1+1)—Slowly, add 50 mL
of H2SO4 (ACS, sp. gr. 1.84) to 50 mL of rea-
gent water.
6.7 Sulfuric acid (1 M)—Slowly, add 58 mL
of H2SO4 (ACS, sp. gr. 1.84) to reagent water
and dilute to 1 L.
6.8 Acetate buffer (0.1 M, pH 4.7)—Dissolve
5.8 mL of glacial acetic acid (ACS) and 13.6 g
of sodium acetate trihydrate (ACS) in rea-
gent water which has been purified by filtra-
tion through a RO-4 Millipore System or
equivalent and dilute to 1 L.
6.9 Acetonitrile, chloroform (preserved
with 1% ethanol), methanol—Pesticide qual-
ity or equivalent.
6.10 Mobile phase—Place equal volumes of
filtered acetonitrile (Millipore type FH filter
or equivalent) and filtered acetate buffer
(Millipore type GS filter or equivalent) in a
narrow-mouth, glass container and mix thor-
oughly. Prepare fresh weekly. Degas daily by
sonicating under vacuum, by heating an stir-
ring, or by purging with helium.
6.11 Stock standard solutions (1.00 ng/
HD—Stock standard solutions may be pre-
pared from pure standard materials or pur-
chased as certified solutions.
6.11.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in methanol
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.11.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.11.3 Stock standard solutions must be
replaced after six months, or sooner if com-
parison with check standards indicates a
problem.
6.12 Quality control check sample con-
centrate—See Section 8.2.1.
90
-------
Environmental Protection Agency
Pt. T36, App. A, Meth. 605
7. Calibration
7.1 Establish chromatographie operating
conditions equivalent to those given in Table
1. The HPLC system can be calibrated using
the external standard technique (Section 7,2)
or the internal standard technique (Section
7.3).
7.2 External standard calibration proce-
dure;
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
mobile phase. One of the external standards
should be at a concentration near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2.2 Using syringe injections of 5 to 25 (iL
or a constant volume injection loop, analyze
each calibration standard according: to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, BSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with mobile phase. One of the standards
should be at a concentration near, but above.
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using syringe injections of 5 to 25 (iL
or a constant volume injection loop, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (RF) for each compound using
Equation 1.
RP= (A,)(Cj,) (Ai«)(C,)
Equation 1
where:
As=Response for the parameter to be meas-
ured.
AjS=Response for the internal standard.
C,s=Concentration of the internal standard
(Hg/L).
C5=Concentration of the parameter to be
measured (jig/L).
If the RF value over the working range is
a constant (<10% RSD), the RF can be as-
sumed to be invariant and the average RF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, AJAis, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound. If serious loss of response occurs.
polish the electrode and recalibrate.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
S. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method, When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial.
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.9, 11.1, and 12,1) to improve the sepa-
rations or lower the cost of measurements,
Each time such a modification is made to
91
-------
Pt. 136, App. A, Meth. 605
40 CFRCh. I (7-1-04 Edition)
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing benzidine
and/or 3,3'-dichlorobenzidine at a concentra-
tion of 50 ng/mL each in methanol. The QC
check sample concentrate must be obtained
from the U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory in Cincinnati, Ohio, if avail-
able. If not available from that source, the
QC check sample concentrate must be ob-
tained from another external source. If not
available from either source above, the QC
check sample concentrate must be prepared
by the laboratory using stock standards pre-
pared independently from those used for cali-
bration.
8.2.2 Using a pipet, prepare QC check sam-
ples at a concentration of 50 ng/L by adding
1.00 mL of QC check sample concentrate to
each of four 1-L-L aliquots of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in ng/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter. Locate and
correct the source of the problem and repeat
the test for all parameters of interest begin-
ning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 50 ng/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or 50
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100(A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1. 7 If spiking was
performed at a concentration lower than 50
Hg/L, the analyst must use either the QC ac-
ceptance criteria in Table 2, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 3, substituting
92
-------
Environmental Protection Agency
Pt. 136, App. A.Meth. 605
the spike concentration (T) for C; (2) cal-
culate overall precision {S') using the equa-
tion in Table 3, substituting X' for X; (3) cal-
culate tie range for recovery at the spike
concentration as (100 X7T)±2.44(1« S7T)%.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing' each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8,4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed,
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters heing simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Sections 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8,4,3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P - 2sp to
P+2sP. If F=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method, The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such as
HPLC with a dissimilar column, gas chroma-
tography, or mass spectrometer must be
used. Whenever possible, the laboratory
should analyze standard reference materials
and participate in relevant performance
evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices8 should be followed, except that the
bottle must not be prerinsed with sample be-
fore collection. Composite samples should be
collected in refrigerated glass containers in
accordance with the requirements of the pro-
gram. Automatic sampling equipment must
be as free as possible of Tygon tubing and
other potential sources of contamination.
9.2 All samples must be iced or refrig-
erated at 4°C and stored in the dark from the
time of collection until extraction. Both
benzidine and 3,3'-dichlorohenzidine are eas-
ily oxidized. Pill the sample bottles and, if
residual chlorine is present, add 80 mg of so-
dium thiosulfate per liter of sample and mix
well. EPA Methods 330.4 and 330.5 may be
used for measurement of residual chlorine.8
Field test kits are available for this purpose.
After mixing, adjust the pH of the sample to
a range of 2 to 7 with sulfuric acid.
9.3 If 1,2-diphenylhydrazine is likely to be
present, adjust the pH of the sample to 4.0+
0.2 to prevent rearrangement to benzidine.
9.4 All samples must he extracted within 7
days of collection. Extracts may be held up
to 7 days before analysis, if stored under an
inert (oxidant free) atmosphere.2 The extract
should be protected from light.
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel. Check the pH
of the sample with wide-range pH paper and
adjust to within the range of 6.5 to 7.5 with
sodium hydroxide solution or sulfuric acid,
10.2 Add 100 mL of chloroform to the sam-
ple bottle, seal, and shake 30 s to rinse the
inner surface. (Caution: Handle chloroform
in a well ventilated area.) Transfer the sol-
vent to the separatory funnel and extract
the sample by shaking the funnel for 2 min
with periodic venting to release excess pres-
sure. Allow the organic layer to separate
from the water phase for a minimum of 10
min. If the emulsion interface between lay-
ers is more than one-third the volume of the
solvent layer, the analyst must employ me-
chanical techniques to complete the phase
separation. The optimum technique depends
upon the sample, but may include stirring,
filtration of the emulsion through glass
93
-------
Pt. 136, App. A, Meth. 605
40 CFR Ch. I (7-1-04 Edition)
wool, centrifugation, or other physical meth-
ods. Collect the chloroform extract in a 250-
mL separatory funnel.
10.3 Add a 50-mL volume of chloroform to
the sample bottle and repeat the extraction
procedure a second time, combining the ex-
tracts in the separatory funnel. Perform a
third extraction in the same manner.
10.4 Separate and discard any aqueous
layer remaining in the 250-mL separatory
funnel after combining the organic extracts.
Add 25 mL of 1 M sulfuric acid and extract
the sample by shaking the funnel for 2 min.
Transfer the aqueous layer to a 250-mL beak-
er. Extract with two additional 25-mL por-
tions of 1 M sulfuric acid and combine the
acid extracts in the beaker.
10.5 Place a stirbar in the 250-mL beaker
and stir the acid extract while carefully add-
ing 5 mL of 0.4 M sodium tribasic phosphate.
While monitoring with a pH meter, neu-
tralize the extract to a pH between 6 and 7 by
dropwise addition of 5 N sodium hydroxide
solution while stirring the solution vigor-
ously. Approximately 25 to 30 mL of 5 N so-
dium hydroxide solution will be required and
it should be added over at least a 2-min pe-
riod. Do not allow the sample pH to exceed 8.
10.6 Transfer the neutralized extract into
a 250-mL separatory funnel. Add 30 mL of
chloroform and shake the funnel for 2 min.
Allow the phases to separate, and transfer
the organic layer to a second 250-mL sepa-
ratory funnel.
10.7 Extract the aqueous layer with two
additional 20-mL aliquots of chloroform as
before. Combine the extracts in the 250-mL
separatory funnel.
10.8 Add 20 mL of reagent water to the
combined organic layers and shake for 30 s.
10.9 Transfer the organic extract into a
100-mL round bottom flask. Add 20 mL of
methanol and concentrate to 5 mL with a ro-
tary evaporator at reduced pressure and 35
°C. An aspirator is recommended for use as
the source of vacuum. Chill the receiver with
ice. This operation requires approximately 10
min. Other concentration techniques may be
used if the requirements of Section 8.2 are
met.
10.10 Using a 9-in. Pasteur pipette, trans-
fer the extract to a 15-mL, conical, screw-cap
centrifuge tube. Rinse the flask, including
the entire side wall, with 2-mL portions of
methanol and combine with the original ex-
tract.
10.11 Carefully concentrate the extract to
0.5 mL using a gentle stream of nitrogen
while heating in a 30 °C water bath. Dilute to
2 mL with methanol, reconcentrate to 1 mL,
and dilute to 5 mL with acetate buffer. Mix
the extract thoroughly. Cap the centrifuge
tube and store refrigerated and protected
from light if further processing will not be
performed immediately. If the extract will
be stored longer than two days, it should be
transferred to a Teflon-sealed screw-cap vial.
If the sample extract requires no further
cleanup, proceed with HPLC analysis (Sec-
tion 12). If the sample requires further clean-
up, proceed to Section 11.
10.12 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1,000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst first
must demonstrate that the requirements of
Section 8.2 can be met using the method as
revised to incorporate the cleanup proce-
dure.
12. High Performance Liquid Chromatography
12.1 Table 1 summarizes the recommended
operating conditions for the HPLC. Included
in this table are retention times, capacity
factors, and MDL that can be achieved under
these conditions. An example of the separa-
tions achieved by this HPLC column is
shown in Figure 1. Other HPLC columns,
chromatographic conditions, or detectors
may be used if the requirements of Section
8.2 are met. When the HPLC is idle, it is ad-
visable to maintain a 0.1 mL/min flow
through the column to prolong column life.
12.2 Calibrate the system daily as de-
scribed in Section 7.
12.3 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the instrument.
12.4 Inject 5 to 25 pL of the sample extract
or standard into the HPLC. If constant vol-
ume injection loops are not used, record the
volume injected to the nearest 0.05 H.L, and
the resulting peak size in area or peak
height units.
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract with mobile phase and reanalyze.
12.7 If the measurement of the peak re-
sponse for benzidine is prevented by the pres-
ence of interferences, reduce the electrode
94
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 605
potential to +0.6 V and reanalyze. If the ben-
zidine peak is still obscured by interferences,
further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (|ig/L) =
(A)(Vt)
Equation 2
where:
A=Amount of material injected (ng).
Vi=Volume of extract injected (|iL).
V,=Volume of total extract (jiL).
V,=Volume of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (|ig/L) =
(Ais)(RF)(V0)
Equation 3
where:
As=Response for the parameter to be meas-
ured.
Als=Response for the internal standard.
Is=Amount of internal standard added to
each extract (|Jg).
V0=Volume of water extracted (L).
13.2 Report results in jig/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.10
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 7xMDL to
SOOOxMDL.1"
14.3 This method was tested by 17 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 1.0 to 70 (ig/L.11 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
References
1. 40 CPR part 136, appendix B.
2. "Determination of Benzidines in Indus-
trial and Muncipal Wastewaters," EPA 600/4-
82-022, National Technical Information Serv-
ice, PB82-196320, Springfield, Virginia 22161,
April 1982.
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CPR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
8. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
9. "Methods 330.4 (Titrimetric, DPD-PAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine Total Residual," Methods for Chem-
ical Analysis of Water and Wastes, EPA-600/
4-79-020, U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268,
March 1979.
10. "EPA Method Study 15, Method 605
(Benzidines)," EPA 600/4-84-062, National
Technical Information Service, PB84-211176,
Springfield, Virginia 22161, June 1984.
11. "EPA Method Validation Study 15,
Method 605 (Benzidines)," Report for EPA
Contract 68-03-2624 (In preparation).
95
-------
Pt. 136, App. A, Meth. 605 40 CFR Ch. I (7-1-04 Edition)
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
3.3'-Dichlorobenzidine .„..„..„..„[[[
Retention
time (min)
6.1
12.1
Column ca-
pacity factor
«
1 44
3.84
Method de-
tection limit
(Ma/L)
008
0.13
HPLC Column conditions: Uchrosorb RP-2, 5 micron particie size, in a 25 cmx4.6 mm ID stainless steel column. Mobile
Phase: 0.8 mUnrtin of 50% acetonitrile/50% 0.1 M pH 4.7 acetate buffer. The MDL were determined using an electrochemical de-
tector operated at -t-G.8 V,
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 605
Parameter
3.3'-DichIorobenzidine .«,..............,,..,
Test I
cone, (ng/ i
so!
so!
Limit for s
-------
Environmental Protection Agency
Pt. 136, App, A, Meth, 605
COLUMN: UCHROSORB RP-2
MOBILE PHASE: 50% ACETONITRILE IN ACETATE BUFFER
DETECTOR: ELECTROCHEMICAL AT + 0.8 V
z
5
N
§
ea
O
ec
O
O
6 12
RETENTION TIME, MIN.
Figure 1. Liquid chromatogram
of benzidines.
97
-------
Pt. 136, App. A, Meth. 606
40 CFRCh. I (7-1-04 Edition)
METHOD 606—PHTHALATE ESTER
1. Scope and Application
1.1 This method covers the determination
of certain phthalate esters. The following pa-
rameters can be determined by this method:
Parameter
Bis(2-ethylhexyl) phthalate
Di-n-butyl phthalate
Diethyl phthalate
Dimethyl phthalate
Di-n-octyl phthalate
STORE!
No.
39100
34292
39110
34336
34341
34596
CAS No.
117-81-7
85-68-7
84-74-2
84-66-2
131-11-3
117-84-0
1.2 This is a gas chromatographic (GC)
method applicable to the determination of
the compounds listed above in municipal and
industrial discharges as provided under 40
CFR 136.1. When this method is used to ana-
lyze unfamiliar samples for any or all of the
compounds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes analytical conditions for a second
gas chromatographic column that can be
used to confirm measurements made with
the primary column. Method 625 provides gas
chromatograph/mass spectrometer (GC/MS)
conditions appropriate for the qualitative
and quantitative confirmation of results for
all of the parameters listed above, using the
extract produced by this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 608, 609, 611, and 612.
Thus, a single sample may be extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. The analyst is allowed the lati-
tude, under Section 12, to select
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and ex-
changed to hexane during concentration to a
volume of 10 mL or less. The extract is sepa-
rated by gas chromatography and the
phthalate esters are then measured with an
electron capture detector.2
2.2 Analysis for phthalates is especially
complicated by their ubiquitous occurrence
in the environment. The method provides
Florisil and alumina column cleanup proce-
dures to aid in the elimination of inter-
ferences that may be encountered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Phthalate esters are contaminants in
many products commonly found in the lab-
oratory. It is particularly important to avoid
the use of plastics because phthalates are
commonly used as plasticizers and are easily
extracted from plastic materials. Serious
phthalate contamination can result at any
time, if consistent quality control is not
practiced. Great care must be experienced to
prevent such contamination. Exhaustive
cleanup of reagents and glassware may be re-
quired to eliminate background phthalate
contamination.4-5
98
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Environmental Protection Agency
Pt. 136, App. A, Meth. 606
3.3 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedures in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining- a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified 6-8 for
the information of the analyst.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling-.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with TeHon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from lig-ht. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrig-erated at 4 °C and protected from
lig-ht during- compositing. If the sampler uses
a peristaltic pump, a minimum leng-th of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing- should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only).
5.2.1 Separatory funnel—2-L, with Teflon
stopcock.
5.2.2 Drying column—Chromatographic
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Chromatographic column—300 mm
long x 10 mm ID, with Teflon stopcock and
coarse frit filter disc at bottom (Kontes K-
420540-0213 or equivalent).
5.2.4 Concentrator tube, Kuderna-Dan-
ish—10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.6 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.7 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5.2.8 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with gas chromatograph
suitable for on-column injection and all re-
quired accessories including syringes, ana-
lytical columns, gases, detector, and strip-
chart recorder. A data system is rec-
ommended for measuring peak areas.
5.6.1 Column 1—1.8 m long x 4 mm ID
glass, packed with 1.5% SP-2250/1.95% SP-
2401 Supelcoport (100/120 mesh) or equivalent.
This column was used to develop the method
performance statemelts in Section 14. Guide-
lines for the use of alternate column
packings are provided in Section 12.1.
5.6.2 Column 2—1.8 m long x 4 mm ID
glass, packed with 3% OV-1 on Supelcoport
(100/120 mesh) or equivalent.
5.6.3 Detector—Electron capture detector.
This detector has proven effective in the
analysis of wastewaters for the parameters
listed in the scope (Section 1.1), and was used
to develop the method performance state-
ments in Section 14. Guidelines for the use of
alternate detectors are provided in Section
12.1.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Acetone, hexane, isooctane, methylene
chloride, methanol—Pesticide quality or
equivalent.
6.3 Ethyl ether—nanograde, redistilled in
glass if necessary.
6.3.1 Ethyl ether must be shown to be free
of peroxides before it is used as indicated by
99
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Pt. 136, App. A, Meth. 606
40 CFR Ch. I (7-1-04 Edition)
EM Laboratories Quant test strips. (Avail-
able from Scientific Products Co., Cat. No.
P1126-8, and other suppliers.)
6.3.2 Procedures recommended for re-
moval of peroxides are provided with the test
strips. After cleanup, 20 mL of ethyl alcohol
preservative must be added to each liter of
ether.
6.4 Sodium sulfate—(ACS) Granular, an-
hydrous. Several levels of purification may
be required in order to reduce background
phthalate levels to an acceptable level: 1)
Heat 4 h at 400 °C in a shallow tray, 2) Heat
16 h at 450 to 500 °C in a shallow tray, 3)
Soxhlet extract with methylene chloride for
48 h.
6.5 Florisil—PR grade (60/100 mesh). Pur-
chase activated at 1250 °F and store in the
dark in glass containers with ground glass
stoppers or foil-lined screw caps. To prepare
for use, place 100 g of Florisil into a 500-mL
beaker and heat for approximately 16 h at 40
°C. After heating transfer to a 500-mL rea-
gent bottle. Tightly seal and cool to room
temperature. When cool add 3 mL of reagent
water. Mix thoroughly by shaking or rolling
for 10 min and let it stand for at least 2 h.
Keep the bottle sealed tightly.
6.6 Alumina—Neutral activity Super I,
W200 series (ICN Life Sciences Group, No.
404583). To prepare for use, place 100 g of alu-
mina into a 500-mL beaker and heat for ap-
proximately 16 h at 400 °C. After heating
transfer to a 500-mL reagent bottle. Tightly
seal and cool to room temperature. When
cool add 3 mL of reagent water. Mix thor-
oughly by shaking or rolling for 10 min and
let it stand for at least 2 h. Keep the bottle
sealed tightly.
6.7 Stock standard solutions (1.00 ug/uL)—
Stock standard solutions can be prepared
from pure standard materials or purchased
as certified solutions.
6.7.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in isooctane
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.7.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7.3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with check standards indicates a
problem.
6.8 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas chromatograph oper-
ating conditions equivalent to those given in
Table 1. The gas chromatographic system
can be calibrated using the external standard
technique (Section 7.2) or the internal stand-
ard technique (Section 7.3).
7.2 External standard calibration proce-
dure:
7.2.1 Prepared calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
isooctane. One of the external standards
should be at a concentration near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2.2 Using injections of 2 to 5 uL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flash. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with isooctane. One of the standards
should be at a concentraton near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
100
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Environmental Protection Agency
Pt. 136, App. A, Meth. 606
7.3.2 Using injections of 2 to 5 uL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (BF) for each compound using
Equation 1.
RF= (As)(Cis) (Ais)(Cs)
Equation 1
where:
As=Response for the parameter to be meas-
ured.
Ais=Response for the internal standard.
Cis=Concentration of the internal standard
(Hg/L).
C5=Concentration of the parameter to be
measured (^g/L).
If the RF value over the working range is
a constant (<10% RSD), the RF can be as-
sumed to be invariant and the average RF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, AJA-,,, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, and 12.1) to improve the sepa-
rations or lower the cost of measurements.
Each time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality contrml (QC) check sample
concentrate is required containing each pa-
rameter of interest at the following con-
centrations in acetone: butyl benzyl phthal-
ate, 10 M.g/mL; bis(2-ethylhexyl) phthalate, 50
ug/mL; di-n-octyl phthalate, 50 ^.g/mL; any
other phthlate, 25 ug/mL. The QC check sam-
ple concentrate must be obtained from the
U.S. Environmental Protection Agancy, En-
vironmental Monitoring and Support Lab-
oratory in Cincinnati, Ohio, if available. If
not available from that source, the QC check
sample concentrate must be obtained from
another external source. If not available
from either source above, the QC check sam-
ple concentrate must be prepared by the lab-
oratory using stock standards prepared inde-
pendently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at the test concentrations shown in
Table 2 by adding 1.00 mL of QC check sam-
ple concentrate to each of four 1-L aliquots
of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in ^g/L, for each parameter using
the four results.
101
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Pt. 136, App. A, Meth. 606
40 CFR Ch. I (7-1-04 Edition)
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter. Locate and
correct the source of the problem and repeat
the test for all parameters of interest begin-
ning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at the test con-
centration in Section 8.2.2 or 1 to 5 times
higher than the background concentration
determined in Section 8.3.2, whichever con-
centration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
the test concentration in Section 8.2.2.
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100(A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.9 If spiking was
performed at a concentration lower than the
test concentration in Section 8.2.2, the ana-
lyst must use either the QC acceptance cri-
teria in Table 2, or optional QC acceptance
criteria calculated for the specific spike con-
centration. To calculate optional acceptance
criteria for the recovery of a parameter: (1)
Calculate accuracy (X') using the equation in
Table 3, substituting the spike concentration
(T) for C; (2) calculate overall precision (S')
using the equation in Table 3, substituting X'
for X; (3) calculate the range for recovery at
the spike concentration as (100 X'/T)±2.44(100
S7T)%.9
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P-2sp to
P+2sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
102
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Environmental Protection Agency
Pt. 136, App. A, Meth, 606
Update the accuracy assessment tor each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements),
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the ehro-
matogram, confirmatory techniques such as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices10 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 1 °C from the time of collection
until extraction.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel.
10.2 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the Inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phrase separa-
tion. The optimum technique depends upon
the sample, but may include stirring, filtra-
tion of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Brlenmeyer flask.
10.3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Brlenmeyer
flask. Perform a third extraction in the same
manner.
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask,
Other concentrator devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Brlenmeyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 CC) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.7 Increase the temperature of the hot
water bath to about 80 °C. Momentarily re-
move the Snyder column, add 50 mL of
hexane and a new boiling' chip, and reattach
the Snyder column. Concentrate the extract
as in Section 10.6, except use hexane to
prewet the column. The elapsed time of con-
centration should be 5 to 10 min.
10.8 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of hexane. A 6-mI_<
syringe is recommended for this operation.
Adjust the extract volume to 10 mL. Stopper
the concentrator tube and store refrigerated
if further processing will not be performed
immediately. If the extract will be stored
longer than two days, it should be trans-
ferred to a Teflon-sealed screw-cap vial. If
the sample extract requires no further clean-
up, proceed with gas chromatographic anal-
ysis (Section 12). If the sample requires fur-
ther cleanup, proceed to Section 11.
10.9 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11, Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
103
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Pt. 136, App. A, Meth. 606
40 CFR Ch. I (7-1-04 Edition)
of a cleanup procedure, the analyst may use
either procedure below or any other appro-
priate procedure. However, the analyst first
mast demonstrate that the requirements of
Section 8.2 can be met using the method as
revised to incorporate the cleanup proce-
dure.
11.2 If the entire extract is to be cleaned
up by one of the following procedures, it
must be concentrated to 2.0 mL. To the con-
centrator tube in Section 10.8, add a clean
boiling chip and attach a two-ball micro-
Snyder column. Prewet the column by add-
ing about 0.5 mL of hexane to the top. Place
the micro-K-D apparatus on a hot water bath
(80 °C) so that the concentrator tube is par-
tially immersed in the hot water. Adjust the
vertical position of the apparatus and the
water temperature as required to complete
the concentration in 5 to 10 min. At the prop-
er rate of distillation the balls of the column
will actively chatter but the chambers will
not flood. When the apparent volume of liq-
uid reaches about 0.5 mL, remove the K-D
apparatus and allow it to drain and cool for
at least 10 min. Remove the micro-Snyder
column and rinse its lower joint into the
concentrator tube with 0.2 mL of hexane. Ad-
just the final volume to 2.0 mL and proceed
with one of the following cleanup procedures.
11.3 Florisil column cleanup for phthalate
esters:
11.3.1 Place 10 g of Plorisil into a
chromatographio column. Tap the column to
settle the Florisil and add 1 cm of anhydrous
sodium sulfate to the top.
11.3.2 Preelute the column with 40 mL of
hexane. The rate for all elutions should be
about 2 mL/min. Discard the eluate and just
prior to exposure of the sodium sulfate layer
to the air, quantitatively transfer the 2-mL
sample extract onto the column using an ad-
ditional 2 mL of hexane to complete the
transfer. Just prior to exposure of the so-
dium sulfate layer to the air, add 40 mL of
hexane and continue the elution of the col-
umn. Discard this hexane eluate.
11.3.3 Next, elute the column with 100 mL
of 20% ethyl ether in hexane (V/V) into a 500-
mL K-D flask equipped with a 10-mL concen-
trator tube. Concentrate the collected frac-
tion as in Section 10.6. No solvent exchange
is necessary. Adjust the volume of the
cleaned up extract to 10 mL in the concen-
trator tube and analyze by gas chroma-
tography (Section 12).
11.4 Alumina column cleanup for phthal-
ate esters:
11.4.1 Place 10 g of alumina into a
chromatographic column. Tap the column to
settle the alumina and add 1 cm of anhy-
drous sodium sulfate to the top.
11.4.2 Preelute the column with 40 mL of
hexane. The rate for all elutions should be
about 2 mL/min. Discard the eluate and just
prior to exposure of the sodium sulfate layer
to the air, quantitatively transfer the 2-mL
sample extract onto the column using" an ad-
ditional 2 mL of hexane to complete the
transfer. Just prior to exposure of the so-
dium sulfate layer to the air, add 35 mL of
hexane and continue the elution of the col-
umn. Discard this hexane eluate.
11,4.3 Next, elute the column with 140 mL
of 20% ethyl ether in hexane (V/V) into a 500-
mL K-D flask equipped with a 10-mL concen-
trator type. Concentrate the collected frac-
tion as in Section 10,6. No solvent exchange
is necessary. Adjust the volume of the
cleaned up extract to 10 mL in the concen-
trator tube and analyze by gas chroma-
tography (Section 12).
12. Gas Chromatography
12.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Examples of the sep-
arations achieved by Column 1 are shown in
Figures 1 and 2, Other packed or capillary
(open-tubular) columns, chromatographic
conditions, or detectors may be used if the
requirements of Section 8,2 are met,
12.2 Calibrate the system daily as de-
scribed in Section 7,
12.3 If the internal standard calibration
procedure is being used, the internal staldard
must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph,
12.4 Inject 2 to 5 jiL of the sample extract
or standard into the gas-chromatograph
using the solvent-flush technique.11 Smaller
(1.0 uL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 uL, and the
resulting peak size in area or peak height
units,
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms,
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
12.7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
104
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Environmental Protection Agency
Pt. 136, App, A, Meth. 606
13,1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2, The con-
centration in the sample can be calculated
from Equation 2,
Concentration (jig/L) =
(A)(Vt)
Equation 2
where:
A=Amotmt of material injected (ng),
V,=Volume of extract injected ((iL).
V,=Volume of total extract (nD.
V,=Volume of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample usinir the response factor
(BF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (|ig/L) =
(A.XI.)
(Ais)(RF)(V0)
Equation 3
where:
A5=Response for the parameter to be meas-
ured.
Ais=Besponse for the internal standard.
I«=Amount of internal standard added to
each extract (ng).
V,,=Volume of water extracted (L).
13.2 Report results in tig/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.12
Similar results were achieved using" rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 5 x MDL
to 1000 x MDL with the following exceptions:
dimethyl and diethyl phthalate recoveries at
1000 x MDL were low (70%); bis-2-ethylhexyl
and di-n-octyl phthalate recoveries at 5 x
MDL were low (60%).12
14.3 This method was tested by 16 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 0.7 to 106 |ig/L.13 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
References
1. 40 CPE part 136, appendix B.
2. "Determination of Phthalates in Indus-
trial and Muncipal Wastewaters," EPA 600/4-
81-063, National Technical Information Serv-
ice, PB81-232167, Springfield. Virginia 22161,
July 1981.
3, ASTM Annual Book of Standards, Part
31, D3884-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. Qiam, C.S., Chan, H.S., and Nef, G.S,
"Sensitive Method for Determination of
Phthalate Ester Plasticizers in Open-Ocean
Biota Samples," Analytical Chemistry, 47, 2225
(1975).
5. Giam, C.S., and Chan, H.S. "Control of
Blanks in the Analysis of Phthalates in Air
and Ocean Biota Samples," U.S. National Bu-
reau of Standards, Special Publication 442,
pp. 701-708, 1976.
6, "Carcinogens—Working with Carcino-
gens." Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health. Publication No.
77-206, August 1977.
7. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
8. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
9. Provost L.P., and Elder, R.S. "Interpre-
tation of Percent Recovers' Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
10. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
11. Burke, J.A. "Gas Cnromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
12. "Method Detection Limit and Analyt-
ical Curve Studies, EPA Methods 606, 607,
and 608," Special letter report for EPA Con-
tract 68-03-2606, U.S. Environmental Protec-
tion Agency, Environmental Monitoring and
Support Laboratory, Cincinnati, Ohio 45268,
June 1980.
105
-------
Pt. 136, App. A, Meth. 606
40 CFR Ch. I (7-1-04 Edition)
13, "EPA Method Study 16 Method 606
(Phthalate Esters)," EPA 600/4-84-056, Na-
tional Technical Information Service, PB84-
211275, Springfield, Virginia 22161, June 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
Di-n-butyl phthalate
Bis(2-ethylhexyl) phthalate
Di-n-octvl ohthalate
Retention time (min)
Column 1
2.03
2,82
8.65
»6.94
"8.92
•16.2
Column 2
0.95
1.27
3.SO
•5.11
•10.5
•18.0
Method de-
tection limit
(v-gii)
0.29
0,49
0.36
0.34
2.0
3.0
Column 1 conditions; Supelcoport 000/120 mesh) coated with 1,5% SP-2250/1,95% SP-2401 packed in a 1.8 m long x 4 mm
ID glass column with 5% methane/95% argon carrier gas at 60 mL/min flow rate. Column temperature held isothermal at 18CFG,
except where otherwise indicated.
Column 2 conditions: Supelcoport (10G/120 mesh) coated with 3% OV-1 packed in a 1.8 m iong x 4 mm ID glass column with
5% methane/95% argon carrier gas at 60 mL/min flow rate. Column temperature held isothermal at 200 CC, except where other-
wise Indicated.
B220 "C column temperature.
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 606
Parameter
Bis{2-ethylhexyl) phthalate
Diethyl phthalate
Di»n-octvl Dhtrialate
Test
cone, (^g/
50
10
25
25
25
50
Limit for s
(ro/u
38.4
4.2
89
9.0
9.5
13.4
Range for
X (ug/L)
1.2-55.9
57-110
10 3-29 6
1 .9-33.4
1 .3-35.5
D-50.0
Range for
P.P.,
(percent)
D-158
30-136
23-136
D-149
D-156
D-114
substandard deviation of four recovery measurements, in pg/L (Section 8,2.4),
X=Average recovery for four recovery measurements, in [ig/L (Section 8,2,4),
P, P,=Percent recovery measured (Section 8,3.2, Section 8.4,2).
D=Detected; result must be greater than zero,
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits for recovery
have teen broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
TABLE 3 — METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION — METHOD 608
Parameter
Bis(2-ethylhexyl) phthalate
Butyl benzyl phthalate
Di-n-butyl phthalate
Di-n-octyl phthalate
Accuracy, as
recovery, X'
(«/l)
0.53C+2.02
0.82C+0.13
0.79C+Q.17
0.70C+0.13
073C+0.17
0.35C-0.71
Single analyst
precision, s/
(WL)
0.80X-2.54
0.26X+0.04
0.23X+0.2Q
0.27X+0.05
0.26X+0.14
0.38X+0.71
Overall preci-
sion, S' (|ig/L)
0.73X-0.17
0.25X+0.07
0.29X+0.06
0.45X+0.11
0.44X+0.31
0.62X+Q.34
X'^Expected recovery for one or more measurements of a sample containing a concentration of C, in ng/L.
s/ssExpected single analyst standard deviation of measurements at an average concentration found of X, in fjg/L.
S'ssExpected interlaboratory standard deviation of measurements at an average concentration found of X, in fig/L.
C=True value for the concentration, in jig/t.
X=Average recovery found for measurements of samples containing a concentration of C: in fig/L.
106
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Environmental Protection Agency
Pt. 136,App. A, Meth. 606
COLUMN: 1.5% SP-2250/1.95% SP- 2401 ON SUPELCOPORT
TEMPERATURE: 180"C
DETECTOR; aECTRON CAPTURE
ui t-
52
-«<
<
X
1
o
0 2 4 6 8 10 12
RETENTION TIME, MIN.
Figure 1. Gas chromatogram of phthalates.
107
-------
Pt. 136, App. A, Meth. 606
40 CFR Ch, I (7-1-04 Edition)
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 220*C
DETECTOR: ELECTRON CAPTURE
BO 00
u
9
0 4 8 12 16 18
RETENTION TIME, MIN,
Figure 2. Gas chromatogram of phthalates.
108
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Environmental Protection Agency
Pt. 136, App. A, Meth. 607
METHOD 607—NITROSAMINES
1. Scope and Application
1.1 TMs method covers the determination
of certain nitrosaraines. The following pa-
rameters can be determined by this method:
Parameter
N-Nitrosodimethylamine
N-Nitrosodi-n-propylamirie
Store! No.
34438
34433
34428
CAS No,
62-75-9
86-30-6
621-64-7
1,2 This is a gas chromatographic (GC)
method applicable to the determination of
the parameters listed above in municipal and
industrial discharges as provided under 40
CFR 136.1, When this method is used to ana-
lyze unfamiliar samples for any or all of the
eompmunds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes analytical conditimns for a second
gas chromatographic column that can be
used to confirm measurements made with
the primary column. Method 625 provides gas
chromatograph/mass spectrometer (GC/MS)
conditions appropriate for the qualitative
and quantitative confirmation of results for
N-nitrosodi-n-propylamine. In order to con-
firm the presence of N-
nitrosodiphenylamine, the cleanup procedure
specified in Section 11.3 or 11.4 must be used.
In order to confirm the presence of K-
nitrosodimethylamlne by GC/MS, Column 1
of this method must be substituted for the
column recommended in Method 625. Con-
firmation of these parameters using GC-high
resolution mass spectrometry or a Thermal
Energy Analyzer is also recommended. '-
1.3 The method detection limit (MDL, de-
fined in Section 14.1)3 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences In
the sample matrix.
1.4 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 aad 136,5.
1.5 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described In Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is washed with
dilute hydrochloric acid to remove free
amines, dried, and concentrated to a volume
of 10 mL or less. After the extract has been
exchanged to methanol, it is separated by
gas chromatography and the parameters are
then measured with a nitrogen-phosphorus
detector.4
2,2 The method provides Florlsil and alu-
mina column cleanup procedures to separate
diphenylamine from the nitrosamines and to
aid in the elimination of interferences that
may be encountered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from Interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3,
3.1.1 Glassware must be scrupulously
cleaned.5 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Solvent rinses with acetone
and pesticide quality hexane may be sub-
stituted for the muffle furnace heating. Vol-
umetric ware should not be heated in a muf-
fle furnace. After drying and cooling, glass-
ware should be sealed and stored in a clean
environment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize Interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3,2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedures in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
3.3 N-Nitrosodiphenylamine is reported6-9
to undergo transnitrosation reactions. Care
must be exercised in the heating or concen-
trating of solutions containing this com-
pound in the presence of reactive amines.
3.4 The sensitive and selective Thermal
Energy Analyzer and the reductive Hall de-
tector may be used in place of the nitrogen-
phosphorus detector when interferences are
encountered. The Thermal Energy Analyzer
offers the highest selectivity of the non-MS
detectors.
109
-------
Pt. 136, App. A, Meth. 607
40 CFR Ch. I (7-1-04 Edition)
4, Safety
4,1 The toxicity or careinogenieity of
eaoli reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the sale han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified'0-12 for
the information of the analyst.
4.2 These nitrosamines are known car-
cinogens 13-'7' therefore, utmost care must be
exercised in the handling of these materials.
Nitrosamine reference standards and stand-
ard solutions should he handled and prepared
in a ventilated glove box within a properly
ventilated room,
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
8.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4 °C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flowmeter Is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog- numbers are included for il-
lustration only.):
5.2.1 Separatory runnels—2-L and 250-mL,
with Teflon stopcock.
5.2.2 Drying column—Chromatographic
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Concentrator tube, Kuderna-Dan-
ish—10-mLi, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.4 Evaporative flask, Kuderna-Danish—
500-rnL (Kontes K-570001-OSOO or equivalent).
Attach to concentrator tube with springs.
5.2.5 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5,2.8 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5.2.7 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap,
5.2.8 Chromatographic column—Approxi-
mately 400 mm long x 22 mm ID, with Teflon
stopcock and coarse frit filter disc at bottom
(Kontes K-42054Q-0234 or equivalent), for use
in Florisil column cleanup procedure.
5.2.9 Chromatographic column—Approxi-
mately 300 mm long x 10 mm ID, with Teflon
stopcock and coarse frit filter disc at bottom
(Kontes K--J20540-0213 or equivalent), for use
in alumina column cleanup procedure,
5,8 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5,6 Gas chromatograph—An analytical
system complete with gas chromatograph
suitable for on-column Injection and all re-
quired accessories including syringes, ana-
lytical columns, gases, detector, and strip-
chart recorder. A data system is rec-
ommended for measuring peak areas.
5.6.1 Column 1—l.B m long x 4 mm ID
glass, packed with 10% Carbowax 20 M/2%
KOH on Chromosorb W-AW (80/100 mesh) or
equivalent. This column was used to develop
the method performance statements in Sec-
tion 14. Guidelines for the use of alternate
column packings are provided in Section
12.2.
5.6.2 Column 2—1.8 m long x 4 mm ID
glass, packed with 10% SP-2250 on Supel-
coport (100/120 mesh) or equivalent.
5.8.3 Detector—Nitrogen-phosphorus, re-
ductive Hall, or Thermal Energy Analyzer
detector.1'2 These detectors have proven ef-
fective in the analysis of wastewaters for the
parameters listed in the scope (Section 1.1).
A nitrogen-phosphorus detector was used to
develop the method performance statements
in Section 14. Guidelines for the use of alter-
nate detectors are provided in Section 12.2.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6,2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 ml.
110
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Environmental Protection Agency
Pt. 136, App. A, Meth. 607
6.3 Sodium tMosulfate—(ACS) Granular.
6.4 Sulfuric acid (1+1)—Slowly, add 50 mL
of H2SO4 (ACS, sp. gr. 1.84) to 50 mL of rea-
gent water.
6.5 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 °C for 4 h
in a shallow tray.
6.6 Hydrochloric acid (1+9)—Add one vol-
ume of concentrated HC1 (ACS) to nine vol-
umes of reagent water.
6.7 Acetone, methanol, methylene chlo-
ride, pentane—Pesticide quality or equiva-
lent.
6.8 Ethyl ether—Nanograde, redistilled in
glass if necessary.
6.8,1 Ethyl ether must be shown to be free
of peroxides before it is used as indicated by
EM Laboratories Quant test strips. (Avail-
able from Scientific Products Co., Cat No.
P1126-8. and other suppliers.)
6.8.2 Procedures recommended for re-
moval of peroxides are provided with the test
strips. After cleanup, 20 mL of ethyl alcohol
preservative must be added to each liter of
ether.
6.9 Florisil—PR grade (60/100 mesh). Pur-
chase activated at 1250 °F and store in the
dark in glass containers with ground glass
stoppers or foil-lined screw caps. Before use,
activate each batch at least 16 h at 130 °C in
a foil-covered glass container and allow to
cool.
6.10 Alumina—Basic activity Super I,
W200 series (ICN Life Sciences Group, No.
404571, or equivalent). To prepare for use,
place 100 g of alumina into a 500-mL reagent
bottle and add 2 mL of reagrent water. Mix
the alumina preparation thoroughly by
shaking or rolling for 10 min and let it stand
for at least 2 h. The preparation should be
homogeneous before use. Keep the bottle
sealed tightly to ensure proper activity.
6.11 Stock standard solutions (1,00 jig/
uL)—Stock standard solutions can be pre-
pared from pure standard materials or pur-
chased as certified solutions.
6.11.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in methanol
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6,11.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.11.3 Stock standard solutions must be
replaced after six months, or sooner if com-
parison with check standards indicates a
problem.
6.12 Quality control check sample con-
centrate—See Section 8.2.1.
7, Calibration
7.1 Establish gas chromatographie oper-
ating conditions equivalent to those given in
Table 1. The gas chromatographic system
can be calibrated using the external standard
technique (Section 7.2) or the internal stand-
ard technique (Section 7.3),
7.2 External standard calibration proce-
dure:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
methanol. One of the external standards
should be at a concentraton near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working: range of
the detector.
7.2.2 Using injections of 2 to 5 uL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve,
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard Is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with methanol. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
Ill
-------
Pt. 136, App. A, Meth. 607
40 CFR Ch. I (7-1-04 Edition)
7.3,2 Using injections of 2 to 5 |£L, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (BF) for each compound using
Equation 1.
EP= (AS)(C«) (Ais)(C,)
Equation 1
where:
As=Response for the parameter to be meas-
ured.
Ato=Response for the internal standard.
Cu=Coneentration of the internal standard
(M-er/L).
C,=Concentration of the parameter to be
measured (ng/L).
If the RP value over the working range is
a constant (<10% BSD), the RF can be as-
sumed to be invariant and the average RF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, A,/Ais, vs. BF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options {detailed in Sec-
tions 10.4, 11.1, and 12.2) to improve the sepa-
rations or lower the cost of measurements.
Each time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 20
jig/mL in methanol. The QC check sample
concentrate must be obtained from the U.S.
Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at a concentration of 20 ng/L by adding
1.00 mL of QC check sample concentrate to
each of four 1-L aliquots of reagent water,
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
|ig/L, and the standard deviation of the re-
covery (s) in (ig/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
112
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Environmental Protection Agency
Pt. 136, App, A, Meth. 607
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter. Locate and
correct the source of the problem and repeat
the test for all parameters of interest begin-
ning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy, For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8,3,1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 20 ng/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger,
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or 20
W/L.
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QO check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100(A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were caluclated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 6:1.18 If spiking was
performed at a concentration lower than 20
^ig/L. the analyst must use either the QC ac-
ceptance criteria in Table 2, or optional QC
acceptance criteria caluclated for the spe-
cific spike concentration. To calculate op-
tional acceptance crtieria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 3, substituting
the spike concentration (T) for C; (2) cal-
culate overall precision (S') using the equa-
tion in Table 3, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X*/T) ± 2.44(100 S'/T)%,1»
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria, A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8,4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8,3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (P,) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (P..)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for waste water
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P-2sp to
P+2sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
113
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Pt. 136, App. A, Meth. 607
40 CFR Ch. I (7-1-04 Edition)
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such as
gas chromatography with a dissimilar
column, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
9, Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices19 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing'
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4 °C from the time of collection
until extraction. Fill the sample bottles and,
if residual chlorine is present, add 80 mg of
sodium thiosulfate per liter of sample and
mix well. EPA Methods 330.4 and 330,5 may
be used for measurement of residual chlo-
rine.20 Field test kits are available for this
purpose. If N-nltrosodiphenylamine is to be
determined, adjust the sample pH to 1 to 10
with sodium hydroxide solution or sulfuric
acid.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.4
9,4 Nitrosamines are known to be light
sensitive.7 Samples should be stored in
amber or foil-wrapped bottles In order to
minimize photolytic decomposition.
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel. Check the pH
of the sample with wide-range pH paper and
adjust to within the range of 5 to 9 with so-
dium hydroxide solution or sulfuric acid.
10.2 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask.
10,3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner.
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL
concentrator tube to a 500-mL evaporative
flask. Other concentration devices or tech-
niques may be used in place of the K-D con-
centrator if the requirements of Section 8.2
are met.
10.5 Add 10 mL of hydrochloric acid to the
combined extracts and shake for 2 min.
Allow the layers to separate. Pour the com-
bined extract through a solvent-rinsed dry-
ing column containing about 10 cm of anhy-
drous sodium sulfate, and collect the extract
in the K-D concentrator. Rinse the Erlen-
meyer flask and column with 20 to 30 mL of
methylene chloride to complete the quan-
titative transfer,
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column, Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65°C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 rain.
10,7 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of methylene
chloride. A 5-rnL syringe is recommended for
this operation. Stopper the concentrator
tube and store refrigerated if further proc-
essing will not be performed immediately. If
the extract will be stored longer than two
days, it should be transferred to a Teflon-
sealed screw-cap vial. If N-nitrosodiphe-
nylamine is to be measured by gas chroma-
tography, the analyst must first use a clean-
up column to eliminate diphenylamine inter-
ference (Section 11). If N-
nitrosodiphenylamine is of no interest, the
analyst may proceed directly with gas
chromatographic analysis (Section 12).
114
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Environmental Protection Agency
Pt. 136, App. A, Meth. 607
10.8 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11, Cleanup and Separation
11,1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
either procedure below or any other appro-
priate procedure. However, the analyst first
must demonstrate that the requirements of
Section 8.2 can be met using- the method as
revised to incorporate the cleanup proce-
dure. Diphenylamine, if present in the origi-
nal sample extract, must be separated from
the nitrosamines if N-nitrosodiphenylamine
is to be determined by this method,
11.2 If the entire extract is to be cleaned
up by one of the following procedures, it
must be concentrated to 2.0 mL. To the con-
centrator tube in Section 10.7, add a clean
boiling chip and attach a two-ball micro-
Snyder column. Prewet the column by add-
ing about 0.5 mL of methylene chloride to
the top. Place the micr-K-D apparatus on a
hot water bath (60 to 65 °C) so that the con-
centrator tube is partially immersed in the
hot water. Adjust the vertical position of the
apparatus and the water temperature as re-
quired to complete the concentration in 5 to
10 min. At the proper rate of distillation the
balls of the column will actively chatter but
the chambers will not flood. When the appar-
ent volume of liquid reaches about 0.5 mL,
remove the K-D apparatus and allow it to
drain and cool for at least 10 min. Remove
the micro-Snyder column and rinse its lower
joint into the concentrator tube with 0.2 mL
of methylene chloride. Adjust the final vol-
ume to 2.0 mL and proceed with one of the
following cleanup procedures.
11.3 Plorisil column cleanup for nitro-
samines:
11.3.1 Place 22 g of activated Plorisil into
a 22-mm ID chromatographic column. Tap
the column to settle the Plorisil and add
about 5 mrn of anhydrous sodium sulfate to
the top.
11.3.2 Preelute the column with 40 mL of
ethyl ether/pentane (15+85XV/V). Discard the
eluate and just prior to exposure of the so-
dium sulfate layer to the air, quantitatively
transfer the 2-mL sample extract onto the
column using an additional 2 mL of pentane
to complete the transfer.
11.3.3 Elute the column with 90 mL of
ethyl ether/pentane (15+85XVAO and discard
the eluate. This fraction will contain the
diphenylamine, if it is present in the extract.
11.3.4 Next, elute the column with 100 mL
of acetone/ethyl ether (5+95)(V/V) into a 500-
mL K-D flask equipped with a 10-mL concen-
trator tube. This fraction will contain all of
the nitrosamines listed in the scope of the
method.
11.3.5 Add 15 mL of methanol to the col-
lected fraction and concentrate as in Section
10.6, except use pentane to prewet the col-
umn and set the water bath at 70 to 75°C.
When the apparatus Is cool, remove the Sny-
der column and rinse the flask and its lower
joint into the concentrator tube with 1 to 2
mL of pentane. Analyze by gas caroma-
tography (Section 12).
11.4 Alumina column cleanup for nitro-
samines:
11.4.1 Place 12 g of the alumina prepara-
tion (Section 6.10) Into a 10-mm ID
chromatographic column. Tap the column to
settle the alumina and add 1 to 2 cm of anhy-
drous sodium sulfate to the top.
11.4.2 Preelute the column with 10 mL of
ethyl ether/pentane (3+7)(V/V). Discard the
eluate (about 2 mL) and just prior to expo-
sure of the sodium sulfate layer to the air,
quantitatively transfer the 2 mL sample ex-
tract onto the column using an additional 2
mL of pentane to complete the transfer.
11.4.3 Just prior to exposure of the sodium
sulfate layer to the air, add 70 mL of ethyl
ether/pentane (3+7)(V/V). Discard the first 10
mL of eluate. Collect the remainder of the
eluate in a 500-mL K-D flask equipped with
a 10 mL concentrator tube. This fraction
contains N-nitrosodiphenylamine and prob-
ably a small amount of N-nitrosodi-n-propyl-
amine.
11.4.4 Next, elute the column with 60 mL
of ethyl ether/pentane (1+1XV/V), collecting
the eluate in a second K-D flask equipped
with a 10-mL concentrator tube. Add 15 mL
of mettanol to the K-D flask. This fraction
will contain N-nitrosodimethylamine, most
of the N-nitrosodi-n-propylamine and any
diphenylamine that is present.
11.4.5 Concentrate both fractions as in
Section 10.6, except use pentane to prewet
the column. When the apparatus is cool, re-
move the Snyder column and rinse the flask
and its lower joint into the concentrator
tube with 1 to 2 mL of pentane. Analyze the
fractions by gas chromatogrraphy (Section
12).
12. Oas Chromatography
12.1 N-nitrosodiphenylamine completely
reacts to form diphenylamine at the normal
operating temperatures of a GC injection
port (200 to 250°C). Thus, N-nitrosodi-
phenylamine is chromatographed and de-
tected as diphenylamine. Accurate deter-
mination depends on removal of diphenyla-
mine that may be present in the original ex-
tract prior to GC analysis (See Section 11).
12.2 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Examples of the sep-
arations achieved by Column 1 are shown in
115
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Pt. 136, App. A, Meth. 607
40 CFR Ch. I (7-1-04 Edition)
Figures 1 and 2. Other packed or capillary
(open-tubular) columns, ehromatographic
conditions, or detectors may be used if the
requirements of Section 8.2 are met.
12.3 Calibrate the system daily as de-
scribed in Section 7.
12.4 If the extract has not been subjected
to one of the cleanup procedures in Section
11; it is necessary to exchange the solvent
from methylene chloride to methanol before
the thermionic detector can be used. To a 1
to 10-mL volume of methylene chloride ex-
tract in a concentrator tube, add 2 mL of
methanol and a clean boiling chip. Attach a
two-ball micro-Snyder column to the con-
centrator tube. Prewet the column by adding
about 0.5 mL of methylene chloride to the
top. Place the micro-K-D apparatus on a
boiling (100 °C) water bath so that the con-
centrator tube is partially immersed in the
hot water. Adjust the vertical positioa of the
apparatus and the water temperature as re-
quired to complete the concentration in 5 to
10 min. At the proper rate of distillation the
balls of the column will actively chatter but
the chambers will not flood. When the appar-
ent volume of liquid reaches about 0.5 mL,
remove the K-D apparatus and allow it to
drain and cool for at least 10 min. Remove
the micro-Snyder column and rinse its lower
joint into the concentrator tube with 0.2 mL
of methanol. Adjust the final volume to 2.0
mL.
12.5 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph.
12.6 Inject 2 to 5 ^iL of the sample extract
or standard into the gas ehromatograph
using the solvent-flush technique,21 Smaller
(1.0 nL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 |*L, and the
resulting peak size in area or peak height
units.
12.7 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
12.8 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
12.9 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined In Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (M-g/L) =
(A)(Vt)
Equation 2
where:
A=Amount of material injected (ng).
Vi=Volume of extract injected (jiL).
Vt=Volume of total extract (jiL).
Vs=Volnme of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RP) determined in Section 7.3.2 and Equa-
tion 3.
RF =
(AS)(C1S)
(Ais)(Cs)
Equation 3
where:
A,=Response for the parameter to be meas-
ured.
Ah=Response for the internal standard.
Lj=Amount of internal standard added to
each extract (jig),
V0=Volume of water extracted (L).
13.2 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.3 The MDL concentrations listed in
Table 1 were obtained using reagent water.22
Similar results were achieved nsing rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 4 x MDL
to 1000 x MDL.22
14.3 This method was tested by 17 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
116
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Environmental Protection Agency
Pt. 136, App. A, Meth. 607
over the range 0.8 to 55 ng/L.23 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
References
1. Fine, D.H., Lieb, D., and Rufeh, R.
"Principle of Operation of the Thermal En-
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Volatile and Non-volatile N-nitroso Com-
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(1975).
2. Fine, D.H., Hoffman, F., Rounbehler,
D.P., and Belcher, N.M. "Analysis of N-nitro-
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pounds—Analysis and Formation, Lyon,
International Agency for Research on Cancer
(IARC Scientific Publications No. 14), pp. 43-
50 (1976).
3. 40 CFR part 136, appendix B.
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6. Buglass, A.J., Challis, B.C., and Osborn,
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Ivankovic, S., and Schmahl, D. "Organotrope
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N-NitrosoVerbindungen an BD-Ratten." Z.
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77-206, August 1977.
11. "OSHA Safety and Health Standards,
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Edition, 1979.
13. Lijinsky, W. "How Nitrosamines Cause
Cancer," New Scientist, 73, 216 (1977).
14. Mirvish, S.S. "N-Nitroso compounds:
Their Chemical and in vivo Formation and
Possible Importance as Environmental Car-
cinogens," J. Toxicol. Environ. Health, 3, 1267
(1977).
15. "Reconnaissance of Environmental Lev-
els of Nitrosamines in the Central United
States," EPA-330/1-77-001, National Enforce-
ment Investigations Center, U.S. Environ-
mental Protection Agency (1977).
16. "Atmospheric Nitrosamine Assessment
Report," Office of Air Quality Planning and
Standards, U.S. Environmental Protection
Agency, Research Triangle Park, North
Carolina (1976).
17. "Scientific and Technical Assessment
Report on Nitrosamines," EPA-660/6-7-001,
Office of Research and Development, U.S.
Environmental Protection Agency (1976).
18. Provost, L.P., and Elder, R.S. "Inter-
pretation of Percent Recovery Data," Amer-
ican Laboratory, 15, 58-63 (1983). (The value
2.44 used in the equation in Section 8.3.3 is
two times the value of 1.22 derived in this re-
port.)
19. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
20. "Methods 330.4 (Titrimetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979.
21. Burke, J. A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
22. "Method Detection Limit and Analyt-
ical Curve Studies EPA Methods 606, 607, and
608," Special letter report for EPA Contract
68-03-2606, U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268,
June 1980.
23. "EPA Method Study 17 Method 607—
Nitrosamines," EPA 600/4-84-051, National
Technical Information Service, PB84-207646,
Springfield, Virginia 22161, June 1984.
117
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Pt. 136, App. A, Meth. 607
40 CFR Ch. I (7-1-04 Edition)
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
N-Nitrosodimethylamine
N-Nitrosodi-n-propylamine
N-Nitrosodiphenylaminea
Retention time (min)
Column 1
4.1
12.1
"12.8
Column 2
0.88
4.2
= 6.4
Method de-
tection limit
(ti9/L)
0.15
.46
.81
Column 1 conditions: Chromosorb W-AW (80/100 mesh) coated with 10% Carbowax 20 M/2% KOH packed in a 1.8 m long x
4mm ID glass column with helium carrier gas at 40 mL/min flow rate. Column temperature held isothermal at 110 °C, except
where otherwise indicated.
Column 2 conditions: Supelcoport (100/120 mesh) coated with 10% SP-2250 packed in a 1.8 m long x 4 mm ID glass column
with helium carrier gas at 40 mL/min flow rate. Column temperature held isothermal at 120 °C, except where otherwise indicated.
a Measured as diphenylamine.
b 220 °C column temperature.
C210 °C column temperature.
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 607
Parameter
N-Nitrosodimethylamine
N-Nitrosodiphenyl
N-Nitrosodi-n-propylamine
Test cone.
(ti9/L)
20
20
20
Limit for s
(ti9/L)
34
6.1
5.7
Range for X
(tig/L)
46-200
2.1-24.5
11.5-26.8
Range for
P, P, (per-
cent)
13-109
D-139
45-146
s=Standard deviation for four recovery measurements, in jig/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in jig/L (Section 8.2.4).
P, Ps=Percent recovery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero.
NOTE: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 607
Parameter
N-Nitrosodimethylamine
N-Nitrosodiphenylamine
N-Nitrosodi-n-propylamine
Accuracy, as
recovery, X'
Oig/L)
0.37C+0.06
0.64C+0.52
0.96C-0.07
Single analyst
precision, s/
(tig/L)
0.25X-0.04
0.36X-1.53
0.15X+0.13
Overall preci-
sion, S' (ng/L)
0.25X+0.11
0.46X-0.47
0.21X+0.15
X'=Expected recovery for one or more measurements of a sample containing a concentration of C, in jig/L.
s/=Expected single analyst standard deviation of measurements at an average concentration found of X, in |ig/L.
S'=Expected intelaboratory standard deviation of measurements at an average concentration found of X, in ng/L
C=True value for the concentration, in jig/L.
X=Average recovery found for measurements of samples containing a concentration of C, in jig/L.
118
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Environmental Protection Agency
Pt. 136, App. A, Meth. 607
COLUMN: 10% CARBOWAX 20M / 2% KOH ON CHROMOSORB W-AW
TEMPERATURE: 11Q°C
DETECTOR: PHOSPHORUS/NITROGEN
UJ
Z
111
5
5
o
«
O
ff
H
_
Z
UJ
Z
a.
O
cc
a.
O
O
(fl
O
cc
H
Z
Z
24 6 8 10 12 14
RETENTION TIME, MIN.
Figure 1. Gas chromatogram of nitrosamines.
119
203-160 D-5
-------
Pt. 136, App. A, Mefh. 607
40 CFR Ch. I (7-1-04 idiflon)
COLUMN: 10% CARBQWAX 20M/2% KOH ON CHROMOSQRB W-AW
TEMPERATURE: 220°C
DETECTOR: PHOSPHORUS/NITROGEN
0 2 4 6 8 10 12 14 16 18
RETENTION TIME, MIN.
Figure 2. Gas chromatogram of IM-nitrosodiphenylamine
as diphenylamine.
120
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Environmental Protection Agency
Pt. 136, App. A, Meth. 608
METHOD 608—OEBANOCHLOEINB PESTICIDES
AND PCBS
I. Scope and Application
1.1 This method covers the determination
of certain organoehlorine pesticides and
PCBs. The following parameters can tie de-
termined by this method:
Parameter
CAS No-
Aldrin ,
a-BHC
|)-BHC
8-BHC
T^BHC
Chlordane
4,4'-DDD
44'-DDE
4 4'-DDT
Dieldrin
Endosulfan 1
Endosulfan li
Endosulfan sulfate
Eldrin
Endrin aldehyde
Heptachlor
Heptachlor epoxide
Toxaphene
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254
PCB-1260
39330
39337
39338
34259
39340
39350
39310
39320
39300
39380
34361
34356
34351
39390
34366
39410
39420
39400
34671
39488
39492
39496
39500
39504
39508
309-00-2
319-B4-6
319-85-7
319-88-8
58-89-8
57-74-9
72-54-8
72-55-9
50-29-3
60-57-1
959-98-8
33212-65-9
1031-07-8
72-20-8
7421-93^1
76-44-8
1024-57-3
8001-35-2
12674-11-2
1104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
1.2 This is a gas chromatographic (GO)
method applicable to the determination of
the compounds listed above in municipal and
industrial discharges as provided under 40
CFB 136.1. When this method is used to ana-
lyze unfamiliar samples for any or all of the
compounds above, compound Identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes analytical conditions for a second
gas chromatographic column that can be
used to confirm measurements made with
the primary column. Method 625 provides gas
ehromatograph/mass spectrometer (GC/MS)
conditions appropriate for the qualitative
and quantitative confirmation of results for
all of the parameters listed above, using the
extract produced by this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 606, 609, 611, and 612.
Thus, a single sample may he extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. The analyst Is allowed the lati-
tude, under Section 12, to select
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136,4 and 136.5,
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Bach analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2,1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and ex-
changed to hexane during concentration to a
volume of 10 mL or less. The extract is sepa-
rated by gas chromatography and the param-
eters are then measured with an electron
capture detector.2
2.2 The method provides a Plorisil column
cleanup procedure and an elemental sulfur
removal procedure to aid in the elimination
of interferences that may be encountered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
121
-------
Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Interferences by phthalate esters can
pose a major problem in pesticide analysis
when using the electron capture detector.
These compounds generally appear in the
chronratogram as large late eluting peaks,
especially in the 15 and 80% fractions from
Florisil. Common flexible plastics contain
varying amounts of phthalates. These
phthalates are easily extracted or leached
from such materials during laboratory oper-
ations. Cross contamination of clean glass-
ware routinely occurs when plastics are han-
dled during extraction ateps, especially when
solvent-wetted surfaces are handled. Inter-
ferences from phthalates can best be mini-
mized by avoiding the use of plastics in the
laboratory. Exhaustive cleanup of reagents
and glassware may be required to eliminate
background phthalate contamination.4-5 The
interferences from phthalate esters can be
avoided by using a microcoulometric or elec-
trolytic conductivity detector,
3.3 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedures in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
4, Safety
4.1 The toxicity or careinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified6-8 for
the information of the analyst.
4.2 The following- parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens: 4,4'-DDT, 4,4'-DDD, the
BHGs, and the PCBs. Primary standards of
these toxic compounds should be prepared in
a hood. A NIQSH/MESA approved toxic gas
respirator should be wora when the analyst
handles high concentrations of these toxic
compounds.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling'.
5.1.1 Grab sample bottle—1-L or 1-q.t,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5,1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 nxL of sample. Sample containers must be
kept refrigerated at 4 "C and protected from
light during composting. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating-
flow meter is required to collect flow propor-
tional composites.
5.2. Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2~L, with Teflon
stopcock.
5,2.2 Drying column—Chromatograpblc
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Chroniatographic column—400 mm
long x 22 mm ID, with Teflon stopcock and
coarse frit filter disc (Kontes K-42054 or
equivalent),
6.2.4 Concentrator tube, Kuderna-Dan-
ish— 10-mL, graduated (Kontes K-57Q050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.6 Snyder column, Kuderna'Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.7 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.3 Boiling chips—Approximately 10/40
inesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with gas chromatograph
suitable for on-column injection and all re-
quired accessories including syringes, ana-
lytical columns, gases, detector, and strip-
122
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Environmental Protection Agency
Pt. 136, App, A, Meth. 608
chart recorder. A data system is rec-
ommended for measuring1 peak areas,
5.6.1 Column 1—1.8 m long x 4 inm ID
glass, packed with 1.5% SP-2250/1.95% SP-
2401 on Supelcoport (100/120 inesh) or equiva-
lent. This column was used to develop the
method performance statements in Section
14. Guidelines for the use of alternate col-
umn packings are provided in Section 12.1.
5.6.2 Column 2—1.8 m long x 4 mm ID
glass, packed with 3% OV-1 on Supelcoport
(100/120 mesh) or equivalent.
5.6.3 Detector—Electron capture detector.
This detector has proven effective in the
analysis of wastewaters for the parameters
listed in the scope (Section 1.1), and was used
to develop the method performance state-
ments in Section 14. Guidelines for the use of
alternate detectors are provided in Section
12.1.
6, Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 mL.
6.3 Sodium thiosulfate—(ACS) Granular.
6.4 Sulfurie acid (1+1)—Slowly, add 50 mL
to H2SO4 (ACS, sp. gr. 1.84) to 50 mL of rea-
gent water.
6.5 Acetone, hexane, isooctane, methylene
chloride—Pesticide quality or equivalent.
6,6 Ethyl ether—Nanograde, redistilled in
glass if necessary.
6.6,1 Ethyl ether must be shown to be free
of peroxides before it is used as indicated by
EM Laboratories Quant test strips. (Avail-
able from Scientific Products Co., Cat. No.
P1126-8, and other suppliers.)
6,6.2 Procedures recommended for re-
moval of peroxides are provided with the test
strips. After cleanup, 20 mL of ethyl alcohol
preservative must be added to each liter of
ether.
6.7 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating- at 400 °C for 4 h
in a shallow tray.
6.8 Plorisil—PR grade (60/100 mesh). Pur-
chase activated at 1250 °P and store in the
dark in glass containers with ground grlass
stoppers or foil-lined screw caps. Before use,
activate each batch at least 16 h at 130 °C in
a foil-covered glass container and allow to
cool,
6.9 Mercury—Triple distilled.
6.10 Copper powder—Activated.
6.11 Stock standard solutions (1.00 p.g/
pi)—Stock standard solutions can be pre-
pared from pure standard materials or pur-
chased as certified solutions.
6.11.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in isooctane
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.11.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.11.3 Stock standard solutions must be
replaced after six months, or sooner if com-
parison with check standards indicates a
problem.
6.12 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas chromatographic oper-
ating conditions equivalent to those given in
Table 1. The gas chromatographic system
can be calibrated using the external standard
technique (Section 7.2) or the Internal stand-
ard technique (Section 7,3),
7,2 External standard calibration proce-
dure:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
isooctane. One of the external standards
should be at a concentration near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2,2 Using injections of 2 to 5 |£L, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
123
-------
Pt. 136, App. A, Meth, 608
40 CFR Ch. I (7-1-04 Edition)
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with isooctane. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 2 to 5 |iL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (BF) for each compound using
Equation 1.
(At)(Cis)
O EE _- * s A is '
(Ah)(CJ
Equation 1
where:
As=Response for the parameter to be meas-
ured.
A,v=Response for the Internal standard.
Ci,=Concentration of the internal standard
(jig/L).
Cs=Concentraton of the parameter to be
measured (|ig/L).
If the RF value over the working range is
a constant (<10% BSD), the EF can be as-
sumed to be invariant and the average BF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, A/Ai,, vs. EF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, the
test must be repeated using a fresh calibra-
tion standard. Alternatively, a new calibra-
tion curve must be prepared for that com-
pound,
7.5 The cleanup procedure in Section 11
utilizes Florisil column ehromatography.
Florisil from different batches or sources
may vary in adsorptive capacity. To stand-
ardize the amount of Florisil which is used,
the use of lauric acid value9 is suggested.
The referenced procedure determines the ad-
sorption from kexane solution of lauric acid
(mg) per g of Florisil. The amount of Florisil
to be used for each column is calculated by
dividing 110 by this ratio and multiplying by
20 g.
7.6 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, and 12,1) to improve the sepa-
rations or lower the cost of measurements.
Bach time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Bach time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5,
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
124
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Environmental Protection Agency
Pt, 136, App. A, Meth. 608
8.2.1 A quality control {QO check sample
concentrate is required containing each sin-
gle-component parameter of Interest at the
following concentrations in acetone: 4,4'-
DDD, 10 ug/mL; 4,4'-DDT, 10 pg/mL;
endosulfan II, 10 jig/mL; endosulfan sulfate,
10 jig/mL: endrin, 10 (igr/mL; any other single-
component pesticide, 2 ug/mL. If this method
is only to be used to analyze for PCBs,
chlordane, or toxaphene, the QC check sam-
ple concentrate should contain the most rep-
resentative multicornponent parameter at a
concentration of 50 (jg/mL in acetone. The QC
check sample concentrate must be obtained
from the U.S. Environmental Protection
Agency, Environmental Monitoring- and Sup-
port Laboratory in Cincinnati, Ohio, if avail-
able. If not available from that source, tlie
QC check sample concentrate must be ob-
tained from another external source. If not
available from either source above, the QC
check sample concentrate must be prepared
by the laboratory using stock standards pre-
pared independently from those used for cali-
bration.
8.2.2 Using a pipet, prepare QC check sam-
ples at the test concentrations. shown in
Table 3 by adding 1.00 rnL of QC check, sam-
ple concentrate to each of four 1-L aliquots
of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/mL; and the standard deviation of the re-
covery (s) in jig/mL, for each parameter
using the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 3. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE; The large number of parameters in
Table 3 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.2.
8.2.8.2 Beginning with Section 8.2.2, repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compmunds of in-
terest beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at the test con-
centration in Section 8.2.2 or 1 to 5 times
higher than the background concentration
determined in Section 8.3.2, whichever con-
centration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
the test concentration in Section 8.2.2.
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1,0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100(A-B)%/T. where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 3. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.10 If spiking was
performed at a concentration lower than the
test concentration in Section 8.2.2, the ana-
lyst must use either the QC acceptance cri-
teria in Table 3, or optional QC acceptance
criteria calculated for the specific spike con-
centration. To calculate optional acceptance
criteria for the recovery of a parameter: (1)
Calculate accuracy (X') using- the equation in
Table 4, substituting the spike concentration
(T) for C; (2) calculate overall precision (S')
using the equation in Table 4, substituting X'
125
-------
Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
for X; (3) calculate the range for recovery at
the spike concentration as (100 X'/T)±2,44(100
8.3.4 If any Individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory. If the entire list of parameters in Table
3 must be measured in the sample in Section
8.3, the probability that the analysis of a QC
check standard will be required is high. In
this case the QC check standard should be
routinely analyzed with the spike sample.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QO check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standards to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 3. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P-2 sp to
P+2 sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8,6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the ehro-
matogram, confirmatory techniques such as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies,
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices11 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4 °C from the time of collection
until extraction. If the samples will not be
extracted within 72 h of collection, the aam-
ple should be adjusted to a pH range of 5.0 to
9.0 with sodium hydroxide solution or sul-
furic acid. Record the volume of acid or base
used. If aldrin is to be determined, add so-
dium thiosulfate when residual chlorine is
present. EPA Methods 330.4 and 330.5 may be
used for measurement of residual chlorine.12
Field test kits are available for this purpose.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-Li separatory funnel.
10.2 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optium technique depends upon the sam-
ple, but may include stirring, filtration of
the emulsion through glass wool, eentrifuga-
tion, or other physical methods. Collect the
methylene chloride extract in a 250-mL Er-
lenmeyer flask.
126
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Environmental Protection Agency
Pt, 136, App. A, Meth. 608
10.3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenrneyer
flask. Perform a third extraction in the same
manner.
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate.
and collect the extract in the K-D concen-
trator. Rinse the Erlenineyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed In the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.7 Increase the temperature of the hot
water bath to about 80 °C. Momeltarily re-
move the Snyder column, add 50 mL of
hexane and a new boiling' chip, and reattach
the Snyder column. Concentrate the extract
as in Section 10.6, except use hexane to
prewet the column. The elapsed time of con-
centration should be 5 to 10 min.
10.8 Bemove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of hexane. A 5-mL
syringe is recommended for this operation.
Stopper the concentrator tube and store re-
frigerated if further processing will not be
performed immediately. If the extract will
be stored longer than two days, it should be
transferred to a Teflon-sealed screw-cap vial.
If the sample extract requires no further
cleanup, proceed with gas chromatographic
analysis (Section 12). If the sample requires
further cleanup, proceed to Section 11,
10.9 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring- the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
either procedure below or any other appro-
priate procedure. However, the analyst first
must demonstrate that the requirements of
Section 8.2 can be met using- the method as
revised to incorporate the cleanup proce-
dure. The Florisil column allows for a select
fractlonation of the compounds and will
eliminate polar interferences. Elemental sul-
fur, which interferes with the electron cap-
ture gas ehromatography of certain pes-
ticides, can be removed by the technique de-
scribed in Section 11.3.
11.2 Florisil column cleanup:
11.2.1 Place a weight of Florisil (nomi-
nally 20 g) predetermined by calibration
(Section 7.5), into a chromatographic col-
umn, Tap the column to settle the Florisil
and add 1 to 2 cm of anhydrous sodium sul-
fate to the top.
11.2.2 Add 60 mL of hexane to wet and
rinse the sodium sulfate and Florisil. Just
prior to exposure of the sodium sulfate layer
to the air, stop the elution of the hexane by
closing the stopcock on the chromatographic
column. Discard the eluate.
11.2.3 Adjust the sample extract volume
to 10 mL with hexane and transfer it from
the K-D concentrator tube onto the column.
Rinse the tube twice with 1 to 2 mL of
hexane, adding each rinse to the column.
11.2.4 Place a 500-mL K-D flask and clean
concentrator tube uader the chroma-
tographic column. Drain the column into the
flask until the sodium sulfate layer is nearly
exposed. Blute the column with 200 mL of 6%
ethyl ether in hexane (V/V) (Fraction 1) at a
rate of about 5 mL/min. Bemove the K-D
flask and set it aside for later concentration.
Elute the column again, using 200 mL of 15%
ethyl ether in hexane (V/V) (Fraction 2), into
a second K-D flask, Perform the third
elution using 200 mL of 50% ethyl ether in
hexane (V/V) (Fraction 3). The elution pat-
terns for the pesticides and PCBs are shown
in Table 2.
11.2.5 Concentrate the fractions as in Sec-
tion 10.6, except use hexane to prewet the
column and set the water bath at about 85
°C. When the apparatus is cool, remove the
Snyder column and rinse the flask and its
lower joint into the concentrator tube with
hexane. Adjust the volume of each fraction
to 10 mL with hexane and analyze by gas
ehromatography (Section 12).
11.3 Elemental sulfur will usually elute
entirely In Fraction 1 of the Florisil column
cleanup, To remove sulfur interference from
this fraction or the original extract, pipet
1.00 mL of the concentrated extract into a
clean concentrator tube or Teflon-sealed
vial. Add one to three drops of mercury and
127
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Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
seal.13 Agitate the contents of the vial for 15
to 30 s. Prolonged shaking (2 h) may be re-
quired. If so, this may be accomplished with
a reciprocal shaker. Alternatively, activated
copper powder may be used for sulfur re-
moval.14 Analyze by gas chromatography,
12. Gas Ckromatography
12.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Examples of the sep-
arations achieved by Column 1 are shown in
Figures 1 to 10, Other packed or capillary
(open-tubular) columns, chromatographic
conditions, or detectors may be used if the
requirements of Section 8.2 are met.
12.2 Calibrate the system daily as de-
scribed in Section 1,
12.3 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph.
12.4 Inject 2 to 5 nL of the sample extract
or standard into the gas chromatograph
using the solvent-flush technique.15 Smaller
(1.0 uL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 |iL, the total
extract volume, and the resulting peak size
in area or peak height units,
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample ctoomatograin with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
12.7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7,2,2, The con-
centration in the sample can be calculated
from Equation 2.
Concentration (|J.g/L) =
(A)(Vt)
Equation 2
where:
A=Amount of material injected (ng).
Vi=Volume of extract injected (jiL).
V,=Volume of total extract (tiL).
Vs=Volume of water extracted (niL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3,
Concentration (jig/L) =
(Ais)(RF)(V0)
Equation 3
where:
As=Response for the parameter to be meas-
ured.
A,s=Besponse for the internal standard.
Is=Amount of internal standard added to
each extract (ng).
V0=Volume of water extracted (L).
13.2 When it is apparent that two or more
PCS (Aroclor) mixtures are present, the
Webb and McCall procedure16 may be used to
identify and quantify the Aroclors,
13,3 For multicomponent mixtures
(chlordane, toxaphene, and POBs) match re-
tention times of peaks in the standards with
peaks in the sample. Quantitate every iden-
tifiable peak unless interference with indi-
vidual peaks persist after cleanup. Add peak
height or peak area of each identified peak
in the chromatogram. Calculate as total re-
sponse in the sample versus total response in
the standard.
13.4 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method, Performance
14,1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero,1 The MDL concentrations listed in
Table 1 were obtained using reagent water.17
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 4xMDL to
lOOOxMDL with the following exceptions:
Chlordane recovery at 4xMDL was low (60%);
128
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Environmental Protection Agency
Pt. 136, App. A, Meth. 608
Toxaphene recovery was demonstrated linear
over the range of lOxMDL to lOOOxMDL.17
14.3 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations.18
Concentrations used in the study ranged
from 0.5 to 30 |ig/L for single-component pes-
ticides and from 8.5 to 400 |ig/L for multi-
component parameters. Single operator pre-
cision, overall precision, and method accu-
racy were found to be directly related to the
concentration of the parameter and essen-
tially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 4.
REFERENCES
1. 40 CFR part 136, appendix B.
2. "Determination of Pesticides and PCBs
in Industrial and Municipal Wastewaters,"
EPA 600/4-82-023, National Technical Infor-
mation Service, PB82-214222, Springfield,
Virginia 22161, April 1982.
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. Giam, C.S., Chan, H.S., and Nef, G.S.,
"Sensitive Method for Determination of
Phthalate Ester Plasticizers in Open-Ocean
Biota Samples," Analytical Chemistry, 47, 2225
(1975).
5. Giam, C.S., Chan, H.S. "Control of
Blanks in the Analysis of Phthalates in Air
and Ocean Biota Samples," U.S. National Bu-
reau of Standards, Special Publication 442,
pp. 701-708, 1976.
6. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
7. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
8. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
9. Mills, P.A. "Variation of Florisil Activ-
ity: Simple Method for Measuring Absorbent
Capacity and Its Use in Standardizing
Florisil Columns," Journal of the Association
of Official Analytical Chemists, 51, 29, (1968).
10. Provost, L.P., and Elder, R.S. "Inter-
pretation of Percent Recovery Data," Amer-
ican Laboratory, 15, 58-63 (1983). (The value
2.44 used in the equation in Section 8.3.3 is
two times the value 1.22 derived in this re-
port.)
11. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
12. "Methods 330.4 (Titrimetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979.
13. Goerlitz, D.F., and Law, L.M. Bulletin
for Environmental Contamination and Toxi-
cology, 6, 9 (1971).
14. "Manual of Analytical Methods for the
Analysis of Pesticides in Human and Envi-
ronmental Samples," EPA-600/8-80-038, U.S.
Environmental Protection Agency, Health
Effects Research Laboratory, Research Tri-
angle Park, North Carolina.
15. Burke, J.A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
16. Webb, R.G., and McCall, A.C. "Quan-
titative PCB Standards for Election Capture
Gas Chromatography," Journal of
Chromatographic Science, 11, 366 (1973).
17. "Method Detection Limit and Analyt-
ical Curve Studies, EPA Methods 606, 607.
and 608," Special letter report for EPA Con-
tract 68-03-2606, U.S. Environmental Protec-
tion Agency, Environmental Monitoring and
Support Laboratory, Cincinnati, Ohio 45268,
June 1980.
18. "EPA Method Study 18 Method 608—
Organochlorine Pesticides and PCBs," EPA
600/4-84-061, National Technical Information
Service, PB84-211358, Springfield, Virginia
22161, June 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
a-BHC
•y-BHC
(3-BHC
5-BHC
Heptachlor epoxide
Endosulfan I
Retention time (min)
Col. 1
1.35
1.70
1.90
2.00
2.15
2.40
3.50
4.50
Col. 2
1.82
2.13
1.97
3.35
2.20
4.10
5.00
6.20
Method detec-
tion limit
(H9/L)
0.003
0.004
0.006
0.003
0.009
0.004
0.083
0.014
129
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Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS—Continued
Parameter
4S4'-DDE .„ ,.,.,.,............,...,.,.,..,..,.,.,„.,...„..„„„„., ... . , „ M ,
Dieldrin [[[
4.4'-DDD
4,4'-DDT ..
Endrin aldehyde
Chlordane
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254 , . , , ,
PCB-1260
Retention time (min)
Col. 1
5.13
5.45
6.55
7.83
8.00
9.40
11.82
14.22
mr
mr
mr
mr
ml
mr
mr
rnr
mr
Col. 2
7.15
7.23
8.10
9.08
8.2B
11.75
9.30
10.70
m
m
m
m
m
m
m
m
m
Method detec-
tion limit
(ngrt-)
0.004
0.002
0.006
0.011
0.004
0,012
0.023
0.066
0.014
0.24
nd
nd
nd
0.085
nd
nd
nd
ACoiumn 1 conditions: Supalcoport (100/120 mesh) coated with 1.5% SP-2250/1.95% SP-2401 packed in a 1.8 m long x 4
mm ID glass column with 5% methane/95% argon carrier gas at 60 mUmin flow rate. Column temperature held isothermal at
200 °C, except for PCB-1018 through PCB-1248, should be measured at 160 "C.
AColumn 2 conditions: Supeleoporl (100/120 mesh| coated with 3% OV-1 packed in a 1.8 m long x 4 mm ID glass column
with 5% methane/95% argon carrier gas at 60 mL/min flow rate. Column temperature held isothermal at 200 °C for the pes-
ticides; at 140 °C for PCB-1221 and 1232; and at 170 °C for PCB-1016 and 1242 to 1268.
Amr^Multiple peak response. See Figures 2 thru 10.
And=Not determined.
TABLE 2—DISTRIBUTION OF CHLORINATED PESTICIDES AND RGBs INTO FLORISIL COLUMN
FRACTIONS 2
Percent recovery by fraction •
ot-BHC
p-BHC
S-BHC
4,4'-DDD
4,4'-DDE
44'-DDT ..
Heptachlor
PCB-1016 . .. .
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254
PCB-1260
1
100
100
97
98
100
100
99
98
100
0
37
0
0
100
100
96
97
97
95
97
103
90
95
2
100
64
7
0
96
68
4
3
91
106
26
* Eluant composition:
Fraction 1-6% ethyl ether in hexane,
Fraction 2-15% ethyl ether in hexane.
Fraction 3-50% ethyl ether in hexane.
TABLE 3—QC ACCEPTANCE CRITERIA—METHOD 608
Parameter
a-BHC
Test cone.
(ng/L)
20
2.0
Limit for s
(Hfl/L)
0.42
0.48
Range for
-------
Environmental Protection Agency
Pt. 136, App, A, Meth. 608
TABLE 3—QC ACCEPTANCE CRITERIA—METHOD 608—Continued
Parameter
p-BHC
J-BHC
•fBHC
4 4 '-ODD
4,4 '-DDE
4 4'-~DDT
Dieldrin
Endosulfan 11
Heptachlor
PCB-1016
PCB-123Z
PCB-1242 ....
PCB-1254
PCB-1260
Test cone.
(M9/L)
20
2.0
20
50
10
2.0
10
20
2.0
10
10
10
2.0
2.0
50.0
50
SO
so
50
SO
50
50
Limit for s
(W/U
064
072
046
10.0
28
0.55
3.6
076
0.49
6.1
2.7
37
0.40
0.41
127
10.0
24.4
179
12.2
15.9
138
10.4
Range for
X (ng/L)
0 78-2 60
1 01-237
0 86-2 32
27.6-54.3
48-126
1.08-2.60
4.6-137
1 15-249
1 14-2 82
2.2-17.1
3.8-132
5 1-126
0.86-2.00
1.13-2.63
278-556
30,5-51 .5
22 1-752
140-985
24.8-69.6
29 0-70 2
22 2-57 9
18.7-54.9
Range for
P, PsS%)
17-147
19-140
32-1 27
45-119
31-141
30-145
25-160
36-146
45-1 53
D-202
26-144
30-147
34-111
37-142
41-126
50-114
15-178
10-215
39-150
38-158
29-131
8-127
s=Standard deviation of four recovery measurements, in ng/L (Section 8.2.4).
X=Average recovery for tour recovery measurements, in tig/L (Section 8.2.4).
P, P..=Percent recovery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero.
NOTE: These criteria are based directly upon the method performance data in Table 4. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used lo develop Table 4.
TABLE 4—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 608
Parameter
Aidrcn
a-BHC
p-BHC
8-BHC
y-BHC
Chlordane
4,4'-DDD
4,4'-DDE
4,4'-DDT
Dieldrin
Endosullan I
Endosuifan II
Endosulfan SuKate .
Endrin
Heptaehtor
Hepiachior epoxide
Toxaphene
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254
PCB-1260
Accuracy, as recov-
ery, X' ftigfl.)
0.81C+0.04
0.84C+0.03
0.81C+0.07
0.81C+0.07
0.82C-O.OS
0.82C-Q.04
Q.84C+Q.30
0.8SC+0.14
0.93C-0.13
0.90C+0.02
0.97C+0.04
0.93C+0.34
0.89C-0.37
0.89C-0.04
0.69C+0.04
0.89C+0.10
0.80C+1.74
0.81C+0.50
0.96C+0.65
0.91 C+1 0.79
0.93C+0.70
0.97C+1.06
0.76C+-2.07
0.66C+3.76
Single analyst pre-
cision. Sr' (jig/L)
0.16X-0.04
0.13X+0.04
0.22X-0.02
0.18X+0.09
0,12X+0.06
0.13X+0.13
0.20X-0.18
0.13X+0.06
0.17X+0.39
0.12X+0.19
0.10X+0.07
0.41 X— 0.65
0.13X+0.33
0.20X+0.25
0.06X+0.13
0.18X-0.11
0.09X+3.20
0.13X+0.15
0.29X-0.76
0.21X--1.93
0.11X+1.40
0.17X^0.41
0.15X-1.66
0.22X-2.37
Overall precision,
S' itig/L)
0.20X-0.01
0.23X-0.00
0.33X-0.05
0.25X+0.03
0.22X+0.04
0.18X+0.18
0.27X 0.14
0.28X 0.09
0.31 X- 0.21
0.16X+0.16
0-18X+0.08
0.47X-0.20
0.24X+0.3S
0.24X+0.25
0.16X+0.08
0.25X-0.08
0.20X^0.22
0.15X^0.45
0.35X-0.62
0.31X+3.50
0.21X+1.52
0-25X-0.37
0.17X+3.62
039X-4.86
X'=Expscted recovery for one or more measurements of a sample containing a concentration of Cs in niJ/L.
s/=Expected single analyst standard deviation of measurements at an average concentration found of X, in gg/L.
S'=Expected trrferiaboratory standard deviation of measurements at an average concentration found of X, in pg/L.
G=True value for the concentration, in gg/L,
X=Average recovery found for measurements of samples containing a concentration of C, in fig/L
131
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Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 200°C.
DETECTOR: ELECTRON CAPTURE
Q
x
O
0 4 8 12 16
RETENTION TIME, MIN.
Figure 1. Gas chromatogram of pesticides.
132
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Environmental Protection Agency
Pt. 136, App. A, Meth. 608
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 200eC.
DETECTOR: ELECTRON CAPTURE
0
16
4 8 12
RETENTION TIME, MIN,
Figure 2. Gas chromatogram of chlordane.
133
-------
Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 1.5% SP-2250/1.95% SP-2401
ON SUPELCOPORT
TEMPERATURE: 200°C.
DETECTOR: ELECTRON CAPTURE
2 6 10 14 18 22
RETENTION TIME, MIN.
Figure 3. Gas chromatogram of toxaphene.
26
134
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Environmental Protection Agency
Ft. 136, App. A, Meth. 608
10LUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 160"C.
DETECTOR; ELECTRON CAPTURE
6 10 14
RETENTION TIME, MIN.
18
22
Figure 4. Gas chromatogram of PCB-1016.
135
-------
Pt. 136, App. A, Meth, 608
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE; 160eC.
DETECTOR: ELECTRON CAPTURE
2 6 10 14 18 22
RETENTION TIME, MIN.
Figure 5. Gas chromatogram of PCB-1221.
136
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Environmental Protection Agency
Pt. 136, App. A, Meth. 608
COLUMN: 1.5% SP-2250/1.95% SP-24Q1 ON SUPELCOPORT
TEMPERATURE: 160'C.
DETECTOR: ELECTRON CAPTURE
2 6 10 14 18
RETENTION TIME, MIN.
Figure 6. Gas chromatogram of PCB-1232.
22
24
137
-------
Pt, 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 fdiflon)
COLUMN: 1.5% SP-2250/1,95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 160°C,
DETECTOR: aECTRON CAPTURE
2 6 10 14 18
RETENTION TIME, MIN.
Figure 7, Gas chromatogram of PCB-1242.
22
138
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Environmental Protection Agency
Pt. 136, App. A, Meth. 608
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 160*0.
DETECTOR: ELECTRON CAPTURE
2 6 10 14 18
RETENTION TIME, MIN.
Figure 8. Gas chromatogram of PCB-1248.
22
26
139
-------
Pt. 136, App. A, Meth. 608
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 1,5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 200aC.
DETECTOR: ELECTRON CAPTURE
6 10 14
RETENTION TIME, MIN .
18
22
Figure 9. Gas chromatogram of PCB-1254.
140
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Environmental Protection Agency
Pt. 136, App. A, Meth. 609
COLUMN: 1.5% SP-2250/1.95% SP-2401 ON SUPELCOPORT
TEMPERATURE: 200°C.
DETECTOR: ELECTRON CAPTURE
JL
JL
JL
10 14 18
RETENTION TIME, MiN.
22
26
Figure 10. Gas chromatogram of PCB-1260.
METHOD 609—NITROAKOMATICS AND
ISOPHOBONE
1, Scope and Application
1.1 This method covers the determination
of certain nitroaromatlcs and isophoroae,
The following parameters may be deter-
mined by this method:
Parameter
2,4-Dinitrotoluene
2,6-Dinitrotoluene
tsophorone -
Nitrobenzene
STORE!
No.
34611
34626
34408
34447
CAS No.
121-14-2
606-20-2
78-59-1
98-95-3
1.2 This is a gas chromatographio (GO)
method applicable to the determination of
141
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Pt. 136, App. A, Meth. 609
40CFRCh. I (7-1-04 Edition)
the compounds listed above in municipal and
industrial discharges as provided under 40
CPR 136.1. When this method is used to ana-
lyze unfamiliar samples for any or all of the
compounds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes analytical conditions for a second
gas chromatographic column that can be
used to confirm measurements made with
the primary column. Method 625 provides gas
chromatograph/mass spectrometer (GC/MS)
conditions appropriate for the qualitative
and quantitative confirmation of results for
all of the parameters listed above, using the
extract produced by this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 606, 608, 611, and 612.
Thus, a single sample may be extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. The analyst is allowed the lati-
tude, under Section 12, to select
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5.
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately l-Ii, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and ex-
changed to hexane during concentration to a
volume of 10 mL or less. Isophorone and
nitrobenzene are measured by flame ioniza-
tion detector gas chromatography (FIDGC).
The dinitrotoluenes are measured by elec-
tron capture detector gas chromatography
(ECDGC).2
2.2 The method provides a Plorisil column
cleanup procedure to aid in the elimination
of interferences that may be encountered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baseliles in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedure in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. Prom this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified4-6 for
the information of the analyst.
142
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Environmental Protection Agency
Pt. 136, App. A, Meth. 609
5. Apparatus and Materials
5.1 Sampling- equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4°C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2-L, with Teflon
stopcock.
5.2.2 Drying column—Chromatographic
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Chromatographic column—100 mm
long x 10 mm ID, with Teflon stopcock.
5.2.4 Concentrator tube, Kuderna-Dan-
ish—10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.6 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.7 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5.2.8 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2°C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with gas chromatograph
suitable for on-column injection and all re-
quired accessories including syringes, ana-
lytical columns, gases, detector, and strip-
chart recorder. A data system is rec-
ommended for measuring peak areas.
5.6.1 Column 1—1.2 m long x 2 or 4 mm ID
glass, packed with 1.95% QF-1/1.5% OV-17 on
Gas-Chrom Q (80/100 mesh) or equivalent.
This column was used to develop the method
performance statements given in Section 14.
Guidelines for the use of alternate column
packings are provided in Section 12.1.
5.6.2 Column 2—3.0 m long x 2 or 4 mm ID
glass, packed with 3% OV-101 on Gas-Chrom
Q (80/100 mesh) or equivalent.
5.6.3 Detectors—Flame ionization and
electron capture detectors. The flame ioniza-
tion detector (FID) is used when determining
isophorone and nitrobenzene. The electron
capture detector (ECD) is used when deter-
mining the dinitrotoluenes. Both detectors
have proven effective in the analysis of
wastewaters and were used in develop the
method performance statements in Section
14. Guidelines for the use to alternate detec-
tors are provided in Section 12.1.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 mL.
6.3 Sulfuric acid (1+1)—Slowly, add 50 mL
of H2SO4 (ACS, sp. gr. 1.84) to 50 mL of rea-
gent water.
6.4 Acetone, hexane, methanol, methylene
chloride—Pesticide quality or equivalent.
6.5 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 °C for 4 h
in a shallow tray.
6.6 Florisil—PR grade (60/100 mesh). Pur-
chase activated at 1250 °F and store in dark
in glass containers with ground glass stop-
pers or foil-lined screw caps. Before use, acti-
vate each batch at least 16 h at 200 °C in a
foil-covered glass container and allow to
cool.
6.7 Stock standard solutions (1.00 ng/M-L)—
Stock standard solutions can be prepared
from pure standard materials or purchased
as certified solutions.
6.7.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in hexane
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.7.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
143
-------
Pt. 136, App. A, Meth. 609
40 CFR Ch. I (7-1-04 Edition)
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7.3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with check standards indicates a
problem.
6.8 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas chromatographic oper-
ating conditions equivalent to those given in
Table 1. The gas chromatographic system
can be calibrated using the external standard
technique (Section 7.2) or the internal stand-
ard technique (Section 7.3).
7.2 External standard calibration proce-
dure:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
hexane. One of the external standards should
be at a concentration near, but above, the
MDL (Table 1) and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.2.2 Using injections of 2 to 5 |iL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD) linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flash. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with hexane. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 2 to 5 |iL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (RF) for each compound using
Equation 1.
Equation 1.
RF =
(As)(Cis)
(Ais)(CS)
where:
As=Response for the parameter to be meas-
ured.
Ais=Response for the internal standard.
Cis=Concentration of the internal standard
((ig/L).
Cs=Concentration of the parameter to be
measured ((ig/L).
If the RF value over the working range is
a constant (<10% RSD), the RF can be as-
sumed to be invariant and the average RF
can be used for calculations. Alternatively,
the results can be used to plot a calibration
curve of response ratios, AJAis, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
144
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Environmental Protection Agency
Pt. 136, App. A, Meth. 609
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, and 12.1) to improve the sepa-
rations or lower the cost of measurements.
Each time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1,5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest in acetone at a con-
centration of 20 ng/mL for each dinitro-
toluene and 100 ng/mL for isophorone and
nitrobenzene. The QC check sample con-
centrate must be obtained from the U.S. En-
vironmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at the test concentrations shown in
Table 2 by adding 1.00 mL of QC check sam-
ple concentrate to each of four 1-L aliquots
of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
|ig/L, and the standard deviation of the re-
covery (s) in ng/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter. Locate and
correct the source of the problem and repeat
the test for all parameters of interest begin-
ning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at the test con-
centration in Section 8.2.2 or 1 to 5 times
higher than the background concentration
determined in Section 8.3.2, whichever con-
centration would be larger.
8.3.1.3 If it is impractical to determile
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
the test concentration in Section 8.2.2.
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100 (A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
145
-------
Pt. 136, App. A, Meth. 609
40 CFR Ch. I (7-1-04 Edition)
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.7 If spiking was
performed at a concentration lower than the
test concentration in Section 8,2.2, the ana-
lyst must use either the QC acceptance cri-
teria in Table 2, or optional QC acceptance
criteria calculated for the specific spike con-
centration. To calculate optional acceptance
criteria for the recovery of a parameter: (1)
Calculate accuracy (X') using the equation in
Table 3, substituting the spike concentration
(T) for C; (2) calculate overall precision (S')
using the equation in Table 3, substituting X'
for X8; (3) calculate the range for recovery at
the spike concentration as (100 XVT) ±2.44
(100 S7T)%.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria, A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4. If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2.1 or 8,3,2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Pa) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test In Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8,5 As part of QC program for the labora-
tory, method accuracy for wastewater sam-
ples must be assessed and records must be
maintained. After the analysis of five spiked
wastewater samples as in Section 8,3, cal-
culate the average percent recovery (P) and
the standard deviation of the percent recov-
ery (sp). Express the accuracy assessment as
a percent_recovery interval from P-2sp to
P+2sp, If P=90% and sp = 10%, for example,
the accuracy interval is expressed as 70-
110%, Update the accuracy assessment for
each parameter on a regular basis (e.g. after
each five to ten new accuracy measure-
ments),
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matograrn, confirmatory techniques such as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
9, Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices8 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4 °C from the time of collection
until extraction.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
JO. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel. Check the pH
of the sample with wide-range pH paper and
adjust to within the range of 5 to 9 with so-
dium hydroxide solution or sulfuric acid.
10,2 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
146
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 609
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask.
10.3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner.
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Erlenmeyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.6 Sections 10.7 and 10.8 describe a pro-
cedure for exchanging the methylene chlo-
ride solvent to hexane while concentrating
the extract volume to 1.0 mL. When it is not
necessary to achieve the MDL in Table 2, the
solvent exchange may be made by the addi-
tion of 50 mL of hexane and concentration to
10 mL as described in Method 606, Sections
10.7 and 10.8.
10.7 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.8 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of methylene
chloride. A 5-mL syringe is recommended for
this operation. Add 1 to 2 mL of hexane and
a clean boiling chip to the concentrator tube
and attach a two-ball micro-Snyder column.
Prewet the column by adding about 0.5 mL of
hexane to the top. Place the micro-K-D ap-
paratus on a hot water bath (60 to 65 °C) so
that the concentrator tube is partially im-
mersed in the hot water. Adjust the vertical
position of the apparatus and the water tem-
perature as required to complete the con-
centration in 5 to 10 min. At the proper rate
of distillation the balls of the column will
actively chatter but the chambers will not
flood. When the apparent volume of liquid
reaches 0.5 mL, remove the K-D apparatus
and allow it to drain and cool for at least 10
min.
10.9 Remove the micro-Snyder column
and rinse its lower joint into the concen-
trator tube with a minimum amount of
hexane. Adjust the extract volume to 1.0 mL.
Stopper the concentrator tube and store re-
frigerated if further processing will not be
performed immediately. If the extract will
be stored longer than two days, it should be
transferred to a Teflon-sealed screw-cap vial.
If the sample extract requires no further
cleanup, proceed with gas chromatographic
analysis (Section 12). If the sample requires
further cleanup, proceed to Section 11.
10.10 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
the procedure below or any other appropriate
procedure. However, the analyst first must
demonstrate that the requirements of Sec-
tion 8.2 can be met using the method as re-
vised to incorporate the cleanup procedure.
11.2 Florisil column cleanup:
11.2.1 Prepare a slurry of 10 g of activated
Florisil in methylene chloride/hexane
(1+9)(V/V) and place the Florisil into a
chromatographic column. Tap the column to
settle the Florisil and add 1 cm of anhydrous
sodium sulfate to the top. Adjust the elution
rate to about 2 mL/min.
11.2.2 Just prior to exposure of the sodium
sulfate layer to the air, quantitatively trans-
fer the sample extract onto the column using
an additional 2 mL of hexane to complete the
transfer. Just prior to exposure of the so-
dium sulfate layer to the air, add 30 mL of
methylene chloride/hexane (1 + 9)(V/V) and
continue the elution of the column. Discard
the eluate.
11.2.3 Next, elute the column with 30 mL
of acetone/methylene chloride (1 + 9)(V7V)
into a 500-mL K-D flask equipped with a 10-
mL concentrator tube. Concentrate the col-
lected fraction as in Sections 10.6, 10.7, 10.8,
and 10.9 including the solvent exchange to 1
mL of hexane. This fraction should contain
the nitroaromatics and isophorone. Analyze
by gas chromatography (Section 12).
12. Gas Chromatography
12.1 Isophorone and nitrobenzene are ana-
lyzed by injection of a portion of the extract
into an FIDGC. The dinitrotoluenes are ana-
lyzed by a separate injection into an ECDGC.
147
-------
Pt. 136, App. A, Meth. 609
40 CFR Ch. I (7-1-04 Edition)
Table 1 summarizes the recommended oper-
ating conditions for the gas chromatograph.
Included in this table are retention times
and MDL that can be achieved under these
conditions. Examples of the separations
achieved by Column 1 are shown in Figures 1
and 2. Other packed or capillary (open-tubu-
lar) columns, chromatographic conditions,
or detectors may be used if the requirements
of Section 8.2 are met.
12.2 Calibrate the system daily as de-
scribed in Section 7.
12.3 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the same extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph.
12.4 Inject 2 to 5 pL of the sample extract
or standard into the gas chromatograph
using the solvent-flush technique.9 Smaller
(1.0 M.L) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 nL, the total
extract volume, and the resulting peak size
in area or peak height units.
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
12.7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (|0.g/L) =
K)(vs)
Equation 2
Vs=Volume of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (|J.g/L) =
(AS)(IS)
(Ais)(RF)(V0)
where:
A=Amount of material injected (ng).
Vi=Volume of extract injected (pL).
V,=Volume of total extract (
Equation 3
where:
As=Response for the parameter to be meas-
ured.
Als=Response for the internal standard.
Is=Amount of internal standard added to
each extract (ng).
V0=Volume of water extracted (L).
13.2 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero. ' The MDL concentrations listed
in Table 1 were obtained using reagent
water.10 Similar results were achieved using
representative wastewaters. The MDL actu-
ally achieved in a given analysis will vary
depending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 7xMDL to
lOOOxMDL.i"
14.3 This method was tested by 18 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 1.0 to 515 ng/L.11 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
REFERENCES
1. 40 CFR part 136, appendix B.
2. "Determination of Nitroaromatic Com-
pounds and Isophorone in Industrial and Mu-
nicipal Wastewaters," EPA 600/ 4-82-024, Na-
tional Technical Information Service, PB82-
208398, Springfield, Virginia 22161, May 1982.
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
148
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 609
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
VV-206, August 19VV.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
8. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
9. Burke, J.A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
10. "Determination of Method Detection
Limit and Analytical Curve for EPA Method
609—Nitroaromatics and Isophorone," Special
letter report for EPA Contract 68-03-2624,
U.S. Environmental Protection Agency, En-
vironmental Monitoring and Support Lab-
oratory, Cincinnati, Ohio 45268, June 1980.
11. "EPA Method Study 19, Method 609
(Nitroaromatics and Isophorone)," EPA 600/4-
84-018, National Technical Information Serv-
ice, PB84-176908, Springfield, Virginia 22161,
March 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
2.4-Dinitrotoluene
Retention time (min)
Col. 1
3.31
3.52
4.49
5.35
Col. 2
4.31
4.75
5.72
6.54
Method detection limit (ug/L)
ECDGC
13.7
0.01
15.7
0.02
FIDGC
3.6
5.7
AAColumn 1 conditions: Gas-Chrom Q (80/100 mesh) coated with 1.95% QF-1/1.5% OV-17 packed in a 1.2 m long x 2 mm
or 4 mm ID glass column. A 2 mm ID column and nitrogen carrier gas at 44 mL/min flow rate were used when determining
isophorone and nitrobenzene by FIDGC. The column temperature was held isothermal at 85 °C. A 4 mm ID column and 10%
methane/90% argon carrier gas at 44 mL/min flow rate were used when determining the dinitrotoluenes by ECDGC. The column
temperature was held isothermal at 145 °C.
AAColumn 2 conditions: Gas-Chrom Q (80/100 mesh) coated with 3% OV-101 packed in a 3.0 m long x 2 mm or 4 mm ID
glass column. A 2 mm ID column and nitrogen carrier gas at 44 mL/min flow rate were used when determining isophorone and
nitrobenzene by FIDGC. The column temperature was held isothermal at 100 °C. A 4 mm ID column and 10% methane/90%
argon carrier gas at 44 mL/min flow rate were used when determining the dinitrotoluenes by ECDGC. The column temperature
was held isothermal at 150 °C.
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 609
Parameter
Nitrobenzene
Test Cone.
(ng/U
20
20
100
100
Limit for s
(i*g/L)
5 1
48
323
33.3
Range for X
(ug/L)
3 6 22 8
3 8 23 0
80-1000
25.7-100.0
Range for
P, P, (%)
6-125
8-126
D-117
6-118
5=Standard deviation of four recovery measurements, in ug/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in |ig/L (Section 8.2.4).
P, P,=Percent recovery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero.
NOTE: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 609
Parameter
2,4-Dinitro-
2,6-Dinitro-
toluene
Nitrobenzene
Accuracy, as re-
covery, X' (fig/L)
0 65C+0 22
0.66C+0.20
0 49C+2 93
0.60C+2.00
Single analyst pre-
cision, s/ (ug/L)
0 20X+0 08
0 19X+006
0 28X+2 77
0.25X+2.53
Overall precision,
S' (ug/L)
0 37X 0 07
0 36X - 0 00
0 46X+0 31
0.37X-0.78
X'=Expected recovery for one or more measurements of a sample containing a concentration of C, in ^g/L
sr'=Expected single analyst standard deviation of measurements at an average concentration found of X, in (ig/L.
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in jig/L.
C=True value for the concentration, in jig/L
X=Average recovery found for measurements of samples containing a concentration of C, in |jg/L
149
-------
Pt. 136, App. A, Meth. 609
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 1,5% OV-17/1.95% QF-1 ON GAS CHROM Q
TEMPERATURE: 85°C.
DETECTOR: FLAME IONIZAT1ON
u
Z
tu
m
O
in
z
O
K
O
I
O-
o
ta
24 6 8 10 12
RETENTION TIME, WIN.
Figure 1. Gas chromatogram
of nitrobenzene
and isophorone.
150
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 609
COLUMN: 1.5% OV-17/1.95% QF-1 ON GAS CHROM Q
TEMPERATURE: 145°C.
DETECTOR: ELECTRON CAPTURE
Ul
01
1 I
s i
9
to
2468
RETENTION TIME, MIN.
Figure 2. Gas chromatogram
of dinitrotoluenes.
151
203-160 D-6
-------
Pt. 136, App. A, Meth. 610
40 CFR Ch. I (7-1-04 Edition)
METHOD 610—POLYNUCLBAR AROMATIC
HYDROCARBONS
1. Scope and Application
1.1 This method covers the determination
of certain polynuclear aromatic hydro-
carbons (PAH). The following parameters
can be determined by this method:
Parameter
Acenaphthene
Acenaphthylene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(ghi)perytene
Benzo(k)fluoranthene
Chrysene
Dibenzo(a,h)anthracene
lndeno(1,2,3-cd)pyrene
Naphthalene
STORE! No.
34205
34200
34220
34526
34247
34230
34521
34242
34320
34556
34376
34381
34403
34696
34461
34469
CAS No.
83-32-9
208-96-8
120-12-7
56-55-3
50-32-8
205-99-2
191-24-2
207-08-9
218-01-9
53-70-3
206-44-0
86-73-7
193-39-5
91-20-3
85-01-8
129-00-0
1.2 This is a chromatographic method ap-
plicable to the determination of the com-
pounds listed above in municipal and indus-
trial discharges as provided under 40 CFR
136.1. When this method is used to analyze
unfamiliar samples for any or all of the com-
pounds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. Method 625 pro-
vides gas chromatograph/mass spectrometer
(GC/MS) conditions appropriate for the qual-
itative and quantitative confirmation of re-
sults for many of the parameters listed
above, using the extract produced by this
method.
1.3 This method provides for both high
performance liquid chromatographic (HPLC)
and gas chromatographic (G-C) approaches
for the determination of PAHs. The gas
chromatographic procedure does not ade-
quately resolve the following four pairs of
compounds: Anthracene and phenanthrene;
chrysene and benzo(a)anthracene;
benzo(b)fluoranthene and
benzo(k)fluoranthene; and dibenzo(a.h) an-
thracene and indeno (l,2,3-cd)pyrene. Unless
the purpose for the analysis can be served by
reporting the sum of an unresolved pair, the
liquid chromatographic approach must be
used for these compounds. The liquid
chromatographic method does resolve all 16
of the PAHs listed.
1.4 The method detection limit (MDL, de-
fined in Section 15.1)l for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.5 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 606, 608, 609, 611, and 612.
Thus, a single sample may be extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. Selection of the aliquots must be
made prior to the solvent exchange steps of
this method. The analyst is allowed the lati-
tude, under Sections 12 and 13, to select
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.6 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5.
1.7 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of HPLC and GC systems
and in the interpretation of liquid and gas
chromatograms. Each analyst must dem-
onstrate the ability to generate acceptable
results with this method using the procedure
described in Section 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and con-
centrated to a volume of 10 mL or less. The
extract is then separated by HPLC or GC. Ul-
traviolet (UV) and fluorescence detectors are
used with HPLC to identify and measure the
PAHs. A flame ionization detector is used
with GC.2
2.2 The method provides a silica gel col-
umn cleanup procedure to aid in the elimi-
nation of interferences that may be encoun-
tered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardward
that lead to discrete artifacts and/or ele-
vated baselines in the chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
152
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Pt. 136, App. A, Meth. 610
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedure in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
3.3 The extent of interferences that may
be encountered using liquid chromatographic
techniques has not been fully assessed. Al-
though the HPLC conditions described allow
for a unique resolution of the specific PAH
compounds covered by this method, other
PAH compounds may interfere.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method have not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified4-6 for
the information of the analyst.
4.2 The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens: benzo(a)anthracene,
benzo(a)pyrene, and dibenzo(a,h)-anthracene.
Primary standards of these toxic compounds
should be prepared in a hood. A NIOSH/
MESA approved toxic gas respirator should
be worn when the analyst handles high con-
centrations of these toxic compounds.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4°C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2-L, with Teflon
stopcock.
5.2.2 Drying column—Chromatographic
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Concentrator tube, Kuderna-Dan-
ish—10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.4 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.5 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.6 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5.2.7 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.2.8 Chromatographic column—250 mm
long x 10 mm ID, with coarse frit filter disc
at bottom and Teflon stopcock.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 High performance liquid chro-
matograph (HPLC)—An analytical system
complete with column supplies, high pres-
sure syringes, detectors, and compatible
strip-chart recorder. A data system is rec-
ommended for measuring peak areas and re-
tention times.
5.6.1 Gradient pumping system—Constant
flow.
153
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Pt. 136, App. A, Meth. 610
40 CFR Ch. I (7-1-04 Edition)
5.6.2 Reverse phase column—HC-ODS Sil-
X, 5 micron particle diameter, in a 25 cm x
2.6 mm ID stainless steel column (Perkin
Elmer No. 089-0716 or equivalent). This col-
umn was used to develop the method per-
formance statements in Section 15. Guide-
lines for the use of alternate column
packings are provided in Section 12.2.
5.6.3 Detectors—Fluorescence and/or UV
detectors. The fluorescence detector is used
for excitation at 280 nm and emission greater
than 389 nm cutoff (Corning 3-75 or equiva-
lent). Pluorometers should have dispersive
optics for excitation and can utilize either
filter or dispersive optics at the emission de-
tector. The UV detector is used at 254 nm
and should be coupled to the fluorescence de-
tector. These detectors were used to develop
the method performance statements in Sec-
tion 15. Guidelines for the use of alternate
detectors are provided in Section 12.2.
5.7 Gas chromatograph—An analytical
system complete with temperature program-
mable gas chromatograph suitable for on-
column or splitless injection and all required
accessories including syringes, analytical
columns, gases, detector, and strip-chart re-
corder. A data system is recommended for
measuring peak areas.
5.7.1 Column—1.8 m long x 2 mm ID glass,
packed with 3% OV-17 on Chromosorb W-
AW-DCMS (100/120 mesh) or equivalent. This
column was used to develop the retention
time data in Table 2. Guidelines for the use
of alternate column packings are provided in
Section 13.3.
5.7.2 Detector—Flame ionization detector.
This detector has proven effective in the
analysis of wastewaters for the parameters
listed in the scope (Section 1.1), excluding
the four pairs of unresolved compounds list-
ed in Section 1.3. Guidelines for the use of al-
ternate detectors are provided in Section
13.3.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium thiosulfate—(ACS) Granular.
6.3 Cyclohexane, methanol, acetone,
methylene chloride, pentane—Pesticide qual-
ity or equivalent.
6.4 Acetonitrile—HPLC quality, distilled
in glass.
6.5 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 °C for 4 h in
a shallow tray.
6.6 Silica gel—100/200 mesh, desiccant,
Davison, grade-923 or equivalent. Before use,
activate for at least 16 h at 130 °C in a shal-
low glass tray, loosely covered with foil.
6.7 Stock standard solutions (1.00 |ig/|iL)—
Stock standard solutions can be prepared
from pure standard materials or purchased
as certified solutions.
6.7.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in acetoni-
trile and dilute to volume in a 10-mL volu-
metric flask. Larger volumes can be used at
the convenience of the analyst. When com-
pound purity is assayed to be 96% or greater,
the weight can be used without correction to
calculate the concentration of the stock
standard. Commercially prepared stock
standards can be used at any concentration
if they are certified by the manufacturer or
by an independent source.
6.7.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7.3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with check standards indicates a
problem.
6.8 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish liquid or gas chromatogra-
phic operating conditions equivalent to
those given in Table 1 or 2. The
chromatographic system can be calibrated
using the external standard technique (Sec-
tion 7.2) or the internal standard technique
(Section 7.3).
7.2 External standard calibration proce-
dure:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
acetonitrile. One of the external standards
should be at a concentration near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2.2 Using injections of 5 to 25 |iL for
HPLC and 2 to 5 nL for GC, analyze each cali-
bration standard according to Section 12 or
13, as appropriate. Tabulate peak height or
area responses against the mass injected.
The results can be used to prepare a calibra-
tion curve for each compound. Alternatively,
if the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
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Pt. 136, App. A, Meth. 610
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with acetonitrile. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 5 to 25 |iL for
HPLC and 2 to 5 |iL for GC, analyze each cali-
bration standard according to Section 12 or
13, as appropriate. Tabulate peak height or
area responses against concentration for
each compound and internal standard. Cal-
culate response factors (RF) for each com-
pound using Equation 1.
RF =
(As)(cls)
(Ais)(cs)
Equation 1
where:
A 5=Response for the parameter to be meas-
ured.
Als=Response for the internal standard.
Cis=Concentration of the internal standard
Cs=Concentration of the parameter to be
measured (|ig/L).
If the RF value over the working range is a
constant (<10% RSD), the RF can be assumed
to be invariant and the average RF can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, A/Ajs, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, the
test must be repeated using a fresh calibra-
tion standard. Alternatively, a new calibra-
tion curve must be prepared for that com-
pound.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, 12.2, and 13.3) to improve the
separations or lower the cost of measure-
ments. Each time such a modification is
made to the method, the analyst is required
to repeat the procedure in Section 8.2.
8.1.3 Before processing any samples the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at the following con-
centrations in acetonitrile: 100 |ig/mL of any
155
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Pt. 136, App. A, Meth. 610
40 CFR Ch. I (7-1-04 Edition)
of the six early-eluting PAHs (naphthalene,
acenaphthylene, aoenaphthene, fluorene,
phenanthrene, and anthracene); 5 |ig/mL of
benzo(k)fluoranthene; and 10 |ig/mL of any of
the other PAHs. The QC check sample con-
centrate must be obtained from the U.S. En-
vironmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at the test concentrations shown in
Table 3 by adding 1.00 mL of QC check sam-
ple concentrate to each of four 1-L aliquots
of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
|ig/L, and the standard deviation of the re-
covery (s) in |ig/L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 3. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Table 3 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.2.
8.2.6.2 Beginning with Section 8.2.2, repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at the test con-
centration in Section 8.2.2 or 1 to 5 times
higher than the background concentration
determined in Section 8.3.2, whichever con-
centration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if
none, (2) the larger of either 5 times higher
than the expected background concentration
or the test concentration in Section 8.2.2.
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100 (A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 3. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.7 If spiking was
performed at a concentration lower than the
test concentration in Section 8.2.2, the ana-
lyst must use either the QC acceptance cri-
teria in Table 3, or optional QC acceptance
criteria calculated for the specific spike con-
centration. To calculate optional acceptance
criteria for the recovery of a parameter: (1)
Calculate accuracy (X') using the equation in
Table 4, substituting the spike concentration
(T) for C; (2) calculate overall precision (S')
using the equation in Table 4, substituting X'
for X; (3) calculate the range for recovery at
the spike concentration as (100 X'/T)±2.44(100
S7T)%.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
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Environmental Protection Agency
Pt. 136, App. A, Meth. 610
that failed the critiera must be analyzed as
described In Section 8.4.
8.4 If any parameter falls the acceptance
criteria for recovery In Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory. If the entire list of parameters in Table
3 must be measured in the sample in Section
8.3, the probability that the analysis of a QC
check standard will be required is high. In
this case the QC check standard should be
routinely analyzed with the spike sample.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (P,) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 3. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (Sp). Express the accuracy assessment
as a percent recovery interval from P-2s,, to
P+2sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in rel-
evant performance evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices8 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4°C from the time of collection
until extraction. PAHs are known to be light
sensitive; therefore, samples, extracts, and
standards should be stored in amber or foil-
wrapped bottles in order to minimize photo-
lytic decomposition. Fill the sample bottles
and, if residual chlorine is present, add 80 mg
of sodium thiosulfate per liter of sample and
mix well. EPA Methods 330.4 and 330.5 may
be used for measurement of residual chlo-
rine.9 Field test kits are available for this
purpose.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel.
10.2 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask.
10.3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner.
157
-------
Pt. 136, App. A, Meth. 610
40 CFR Ch. I (7-1-04 Edition)
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Erlenmeyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the cdfccen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.7 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of methylene
chloride. A 5-mL syringe is recommended for
this operation. Stopper the concentrator
tube and store refrigerated if further proc-
essing will not be performed immediately. If
the extract will be stored longer than two
days, it should be transferred to a Teflon-
sealed screw-cap vial and protected from
light. If the sample extract requires no fur-
ther cleanup, proceed with gas or liquid
chromatographic analysis (Section 12 or 13).
If the sample requires further cleanup, pro-
ceed to Section 11.
10.8 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
the procedure below or any other appropriate
procedure. However, the analyst first must
demonstrate that the requirements of Sec-
tion 8.2 can be met using the methods as re-
vised to incorporate the cleanup procedure.
11.2 Before the silica gel cleanup tech-
nique can be utilized, the extract solvent
must be exchanged to cyclohexane. Add 1 to
10 mL of the sample extract (in methylene
chloride) and a boiling chip to a clean K-D
concentrator tube. Add 4 mL of cyclohexane
and attach a two-ball micro-Snyder column.
Prewet the column by adding 0.5 mL of
methylene chloride to the top. Place the
micro-K-D apparatus on a boiling (100 °C)
water bath so that the concentrator tube is
partially immersed in the hot water. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete concentration in 5 to 10 min. At the
proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood. When the apparent vol-
ume of the liquid reaches 0.5 mL, remove the
K-D apparatus and allow it to drain and cool
for at least 10 min. Remove the micro-Sny-
der column and rinse its lower joint into the
concentrator tube with a minimum amount
of cyclohexane. Adjust the extract volume to
about 2 mL.
11.3 Silica gel column cleanup for PAHs:
11.3.1 Prepare a slurry of 10 g of activiated
silica gel in methylene chloride and place
this into a 10-mm ID chromatographic col-
umn. Tap the column to settle the silica gel
and elute the methylene chloride. Add 1 to 2
cm of anhydrous sodium sulfate to the top of
the silica gel.
11.3.2 Preelute the column with 40 mL of
pentane. The rate for all elutions should be
about 2 mL/min. Discard the eluate and just
prior to exposure of the sodium sulfate layer
to the air, transfer the 2-mL cyclohexane
sample extract onto the column using an ad-
ditional 2 mL cyclohexane to complete the
transfer. Just prior to exposure of the so-
dium sulfate layer to the air, add 25 mL of
pentane and continue the elution of the col-
umn. Discard this pentane eluate.
11.3.3 Next, elute the column with 25 mL
of methylene chloride/pentane (4+6)(V/V)
into a 500-mL K-D flask equipped with a 10-
mL concentrator tube. Concentrate the col-
lected fraction to less than 10 mL as in Sec-
tion 10.6. When the apparatus is cool, remove
the Snyder column and rinse the flask and
its lower joint with pentane. Proceed with
HPLC or GC analysis.
12. High Performance Liquid Chromatography
12.1 To the extract in the concentrator
tube, add 4 mL of acetonitrile and a new
boiling chip, then attach a two-ball micro-
Snyder column. Concentrate the solvent as
in Section 10.6, except set the water bath at
95 to 100 °C. When the apparatus is cool, re-
move the micro-Snyder column and rinse its
lower joint into the concentrator tube with
about 0.2 mL of acetonitrile. Adjust the ex-
tract volume to 1.0 mL.
12.2 Table 1 summarizes the recommended
operating conditions for the HPLC. Included
in this table are retention times, capacity
factors, and MDL that can be achieved under
158
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 610
these conditions. The UV detector is rec-
ommended for the determination of naph-
thalene, acenaphthylene, aeenapthene, and
fluorene and the fluorescence detector is rec-
ommended for the remaining PAHs. Exam-
ples of the separations achieved by this
HPLC column are shown in Figures 1 and 2.
Other HPLC columns, chromatographic con-
ditions, or detectors may be used if the re-
quirements of Section 8.2 are met.
12.3 Calibrate the system daily as de-
scribed in Section 7.
12.4 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the instrument.
12.5 Inject 5 to 25 \iL of the sample extract
or standard into the HPLC using a high pres-
sure syringe or a constant volume sample in-
jection loop. Record the volume injected to
the nearest 0.1 uL, and the resulting peak
size in area or peak height units. Re-equili-
brate the HPLC column at the initial gra-
dient conditions for at least 10 min between
injections.
12.6 Identify the parameters in the sample
by comparing the retention time of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
12.7 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract with acetonitrile and reanalyze.
12.8 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
75. Gas Chromatography
13.1 The packed column OC procedure will
not resolve certain Isomerie pairs as indi-
cated in Section 1.3 and Table 2, The liquid
chromatographic procedure (Section 12)
must be used for these parameters.
13.2 To achieve maximum sensitivity with
this method, the extract must be con-
centrated to 1.0 mL. Add a clean boiling chip
to the methylene chloride extract in the con-
centrator tube. Attach a two-ball micro-Sny-
der column. Prewet the micro-Snyder col-
umn by adding about 0.5 mL of methylene
chloride to the top. Place the micro-K-D ap-
paratus on a hot water bath (60 to 65 °C) so
that the concentrator tube is partially im-
mersed in the hot water. Adjust the vertical
position of the apparatus and the water tem-
perature as required to complete the con-
centration in 5 to 10 min. At the proper rate
of distillation the balls will actively chatter
but the chambers will not flood. When the
apparent volume of liquid reaches 0.5 mL, re-
move the K-D apparatus and allow it to
drain and cool for at least 10 min. Remove
the micro-Snyder column and rinse its lower
joint into the concentrator tube with a min-
imum amount of methylene chloride. Adjust
the final volume to 1.0 mL and stopper the
concentrator tube.
13.3 Table 2 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times that were obtained under these
conditions. An example of the separations
achieved by this column is shown in Figure
3. Other packed or capillary (open-tubular)
columns, chromatographic conditions, or de-
tectors may be used if the requirements of
Section 8.2 are met.
13.4 Calibrate the gas chromatographic
system daily as described in Section 7.
13.5 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas chromatograph.
13.6 Inject 2 to 5 |J.L of the sample extract
or standard into the gas chromatograph
using the solvent-flush technique.10 Smaller
(1.0 uL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 uL, and the
resulting peak size in area or peak height
units.
13.7 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of chromatograms.
13.8 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
13.9 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
14, Calculations
14.1 Determine the concentration of indi-
vidual compounds in the sample.
14.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration In the sample can be calculated
from Equation 2.
159
-------
Pt. 136,App. A,Meth, 610
40 CFR Ch. 1 (7-1-04 Edition)
Concentration (Hg/L) =
(A)(Vt)
Equation 2
where:
A=Amount of material injected (ng),
Vj=Volume of extract injected (jiL).
V,=Volume of total extract (|J,L).
Vs=Volume of water extracted (mL).
13.1,2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7,3.2 and Equa-
tion 3.
Concentration (Hg/L) =
(A.XI.)
(Ai5)(RF)(V0)
Equation 3
where:
As=Besponse for the parameter to be meas-
ured.
AiS=Response for the internal standard.
I,=Amount of internal standard added to
each extract (ng).
V0=Volume of water extracted (L).
14.2 Report results in ug/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
15. Method Performance
15,1 The method detection limit (MDL) is
defined as the minimum concentration ol a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.11
Similar results were achieved using rep-
resentative wastewaters. MDL for the GC ap-
proach were not determined. The MDL actu-
ally achieved in a given analysis will vary
depending on instrument sensitivity and ma-
trix effects,
15.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 8 x MDL
to 800 x MDL11 with the following exception:
benzo(ghi)perylene recovery at 80 x and 800 x
MDL were low (35% and 45%, respectively).
15.3 This method was tested by 16 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 0.1 to 425 ug/L.12 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially Independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 4.
REFERENCES
1. 40 CPU part 136, appendix B.
2. "Determination of Polynuclear Aromatic
Hydrocarbons in Industrial and Municipal
Wastewaters," EPA 600/4-82-025, National
Technical Information Service, PB82-258799,
Springfield, Virginia 22161, June 1982.
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
8. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
9. "Methods 330.4 (Titrirnetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979.
10. Burke, J.A. "Gas Chrornatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48,1037 (1965).
11. Cole, T., Riggin, E., and Glaser, J.
"Evaluation of Method Detection Limits and
Analytical Curve for EPA Method 610—
PNAs," International Symposium on
Polynuclear Aromatic Hydrocarbons, 5th,
Battelle's Columbus Laboratories, Colum-
bus, Ohio (1980).
12. "EPA Method Study 20, Method 610
(PNA's)," EPA 600/4-84-063, National Tech-
nical Information Service, PB84-211614,
Springfield, Virginia 32161, June 1984.
160
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 610
TABLE 1—HIGH PERFORMANCE LIQUID CHROMATOGRAPHY CONDITIONS AND METHOD DETECTION
LIMITS
Naphthalene
Acenaphthylene ...............
Acenaphthene .................
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene ..,,..
Benzo(a)anthracene
Chrysene
Benz0(b)ffuoranthene ......
Benzo{k)fluoranthene
6enzo(a)pyr@ne
Dibenzoia,h)anthracene .,
Benzo(ghi)peryiene .„.,„.,
Indeno(1,2,3-cd)pyrene .-.
Retention
lime (min)
Column
capacity
factor (k')
16.6 ! 12,2
18.5 ! 13.7
20,5 i 15.2
21.2
22.1
23.4
24.5
25.4
28.5
29.3
31-6
32.9
33.9
35.7
36.3
37-4
15.8
16.6
17.6
18.5
19.1
21.6
22.2
24.0
25.1
25.9
27.4
27.8
28.7
Method
detection
limit (u,g/
Ms
1.8
2.3
1.8
0.21
0.64
0.66
0.21
0,27
0.013
0.15
0.018
0.017
0,023
0.030
0,076
0,043
AAAHPLG column conditions; Reverse phase HC-ODS Sil-X, 5 micron particle size, in a 25 cm x 2.6 mm ID stainless steel
column. Isocratic elution for 5 rnin. using acetortitrile/water (4+6), then linear gradient elution to 100% acetonrtrile over 25 min. at
0.5 mL'min flow rate. If columns having other internal diameters are used, the flow rate should be adjusted to maintain a linear
velocity of 2 mm/sec.
"The MDL for naphthalene, acenaphthylene, acenaphthene, and fluorene were determined using a UV detector. All others
were determined using a fluorescence detector.
TABLE 2—GAS CHROMATOGRAPHIC CONDITIONS
AND RETENTION TIMES
TABLE 2—GAS CHROMATOGRAPHIC CONDITIONS
AND RETENTION TIMES—Continued
Parameter
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene ...
Chrysene
Benzo(b)fluoranthene .
Retention
time (min)
4.5
10.4
10.8
12.6
15.9
15.9
19.8
20.6
24.7
24,7
28.0
Parameter
Benzo(k)fiuoranthene ..... .,,,.,,,.,,..., ,
Benzo(a)pyrene ,.,.,.„.,„.,.,.,.,...,..,...,.,.,...,...,........
Indeno(1,2,3-cd)pyrene .,,,.,,,,,,.,,,.,„.„„,.„.,.,.,...,,
Benzofahiloervlene .„.,.,.,...,...,......,.......... ,.,
Retention
time (rnin)
28.0
29.4
382
36^2
38.6
GC Column conditions: Chromosorb W-AW-DCMS (100/
120 mesh) coated with 3% OV-17 packed in a 1.8 x 2 mm ID
glass column with nitrogen carrier gas at 40 mU'min. flow rate.
Column temperature was held al TQQ°C for 4 rnin., then pro-
grammed at 8°C/min. to a final hold at 280 °C.
TABLE 3—QC ACCEPTANCE CRITERIA—METHOD 610
Parameter
Anthracene
Benzo(a)anthracene
Benzo(b)flu0r-anthene
Benzo(k)fluo-rahthene ,
Dibenzo(a,h)an-thracene
lndeno(1.2,3-cd}pyrene ..
Test cone.
(M9-'L)
100
100
100
10
10
10
10
5
10
10
10
100
10
100
100
10
Limit for s
^JM/L)
403
45 1
28.7
4.0
40
3,1
23
25
42
2,0
30
430
30
407
377
3.4
Range for X
(ra'L)
D-105 7
22 1-112 1
11.2-112.3
3.1-11.6
0 2-1 1 0
1.8-13.8
D-107
D-7.0
D-175
0.3-10.0
27-11 1
D-119
1.2-10.0
21 5-1000
8 4-1 33 7
1.4-12.1
Range for
P, P> (%)
D-124
D-139
D-128
12-135
D-128
6-150
D-116
D-159
D-199
D-110
14-123
D-142
D-116
D-122
D-155
D-140
s,=Standard deviation of four recovery measurements, in ^ig/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in $ig/L (Section 8.2.4).
p p^_percenj recOvery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero,
NOTE: These criteria are based directly upon the method performance data in Table 4. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 4,
161
-------
Pt. 136, App. A, Meth. 610
40 CFR Ch. I (7-1-04 Edition)
TABLE 4—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 610
Parameter
Acenaphthene 0.52C+0.54
Acenaphthylene 0.69C-1.89
Anthracene 0.63C- 1.26
Benzo{a)anthracene 0.73C+0.05
Benzoja)pyrene 0,560+0.01
Benzo(b)fluoranthene 0.78C + 0.01
Benzo(ghi)perylene 0.44C+0.30
Benzo(k)fluoranthene 0.59C+O.OQ
Chrysene 0.77C-0.18
Dib8nzo(a,h)anthracene 0.410+0.11
Fluoranthens 0.68C+Q.07
Fluorene O.S6C-O.S2
lndeno(1,2,3-cd)pyrene 0.54C + 0.06
Naphthalene 0.57C - 0.70
Phenanthrene ! 0.72C - 0.95
Pyrene j 0.69C - 0.12
Accuracy, as
recovery, X'
Single analyst
precision, s,'
(Ml/I-)
0.39X
0.36X
0.23X
0.2BX
0.38X -
0.21 X
0.25X
0.44X -
0.32X-
0.24X
0.22X
0.44X-
0.29X
0.39X
Q.29X
0.25X
Overall preci-
sion, S'
0.76
0.29
+ 1.16
0.04
0.01
0.01
0.04
0.00
0.18
0.02
0.08
1.12
0.02
-0.18
+ 0.05
+ 0.14
0.53X + 1.32
Q.42X+Q.52
0.41X+0.45
0.34X + 0.02
0.53X - 0.01
0.38X - 0.00
0.58X+0.10
0.69X + 0.01
0.66X - 0.22
0.4SX+0.03
0.32X + 0.03
0.63X - 0.65
0.42X + 0.01
0.41X + 0.74
0.47X - 0.25
0.42X - 0.00
X'=Expeeted recovery for one or more measurements of a sample containing a concentration of C, in jig/L.
s/sExpeeted single analyst standard deviation of measurements at an average concentration found of X, in jig/L.
S'ssExpected interlaboratory standard deviation of measurements at an average concentration found of X, in &io/L
C=True value for the concentration, in \ig/L.
X=Average recovery found for measurements of samples containing a concentration of C, in u.g/L.
COLUMN: HC-ODS SIL-X
MOBILE PHASE: 40% TO 100% ACETONITRILE IN WATER
DiTiCTOR: ULTRAVIOLET AT 254nm
i
1
i
S 3
< £
I X. at
i s s
I 5 |
III
Jlif'
i
TMRACENE
JE
2 £
H u
z
C
i
li f
I i
!
U
i
I 1
1 !| pi
1 1| If1
UHL
4 8 12 16 20 2« 28 3Z w
RETENTION TIME, WIN .
Figure 1 . Liquid chromatogram of poiynuctear aromatic hydrocarbons.
162
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Environmental Protection Agency
Pt. 136, App. A, Meth. 610
COLUMN: HC-ODS SIL-X
MOBILE PHASE: 40%TO 100% ACETONITRILE
IN WATER
DETECTOR: FLUORESCENCE
RETENTION TIME. MIN.
Figure 2. Liquid chromatogram of polynuclear aromatic hydrocarbons.
163
-------
Pt. 136, App. A, Meth. 611
40 CFRCh. I (7-1-04 Edition)
COLUMN: 3% OV-170N CHROMOSORB W-AW-DCMS
PROGRAM: 100°C FOR 4 WIN. 8°C/MIN TO 280°C
DETECTOR: FLAME IONIZATION
z
<
I z
it
< o
§3
D a:
8S
Z m
8
jjj
5
<9
12
24
28
32
40
RETENTION TIME, MIN.
Figure 3. Gas chromatogram of polynuclear aromatic hydrocarbons.
METHOD 611—HALOETHERS
1. Scope and Application
1.1 This method covers the determination
of certain haloethers. The following param-
eters can be determined by this method:
Parameter
Bis(2-chloroethyl) ether
Bis(2-chloroethoxy) methane ....
Bis(2-chloroisopropyl) ether
4-Bromophenyl phenyl ether
4-Chlorophenyl phenyl either ....
STORE!
No.
34273
34278
34283
34636
34641
CAS No.
111-44-4
111-91-1
108-60-1
101-55-3
7005-72-3
1.2 This is a gas chromatographic (GC)
method applicable to the determination of
the compounds listed above in municipal and
industrial discharges as provided under 40
CFR 136.1. When this method is used to ana-
lyze unfamiliar samples for any or all of the
compounds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes analytical conditions for a second
gas chromatographic column that can be
used to confirm measurements made with
the primary column. Method 625 provides gas
chromatograph/mass spectrometer (GC/MS)
conditions appropriate for the qualitative
and quantitative confirmation of results for
all of the parameters listed above, using the
extract produced by this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)' for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 606, 608, 609, and 612.
Thus, a single sample may be extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. The analyst is allowed the lati-
tude, under Section 12, to select
164
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Environmental Protection Agency
Pt. 136, App. A, Meth. 611
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph and
in the interpretation of gas chromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and ex-
changed to hexane during concentration to a
volume of 10 mL or less. The extract is sepa-
rated by gas chromatography and the param-
eters are then measured with a halide spe-
cific detector.2
2.2 The method provides a Florisil column
cleanup procedure to aid in the elimination
of interferences that may be encountered.
3. Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in gas chromatograms. All of
these materials must be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.1 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed be detergent washing with hot water.
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such a PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCS interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedure in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
3.3 Dichlorobenzenes are known to
coelute with haloethers under some gas
chromatographic conditions. If these mate-
rials are present together in a sample, it
may be necessary to analyze the extract
with two different column packings to com-
pletely resolve all of the compounds.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified46 for
the information of the analyst.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4 °C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
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40 CFR Ch. I (7-1-04 Edition)
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2-L, with Teflon
stopcock.
5.2.2 Drying column—Chromatographic
column, approximately 400 mm long x 19 mm
ID, with coarse frit filter disc.
5.2.3 Chromatographic column—400 mm
long x 19 mm ID, with Teflon stopcock and
coarse frit filter disc at bottom (Kontes K-
420540-0224 or equivalent).
5.2.4 Concentrator tube, Kuderna-Dan-
ish—10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.6 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.7 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2°C). The bath should be used in a hood.
5.5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with temperature program-
mable gas chromatograph suitable for on-
column injection and all required accessories
including syringes, analytical columns,
gases, detector, and strip-chart recorder. A
data system is recommended for measuring
peak areas.
5.6.1 Column 1—1.8 m long x 2 mm ID
glass, packed with 3% SP-1000 on Supelco-
port (100/120 mesh) or equivalent. This col-
umn was used to develop the method per-
formance statements in Section 14. Guide-
lines for the use of alternate column
packings are provided in Section 12.1.
5.6.2 Column 2—1.8 m long x 2 mm ID
glass, packed with 2,6-diphenylene oxide
polymer (60/80 mesh), Tenax, or equivalent.
5.6.3 Detector—Halide specific detector:
electrolytic conductivity or microcoulo-
metric. These detectors have proven effec-
tive in the analysis of wastewaters for the
parameters listed in the scope (Section 1.1).
The Hall conductivity detector was used to
develop the method performance statements
in Section 14. Guidelines for the use of alter-
nate detectors are provided in Section 12.1.
Although less selective, an electron capture
detector is an acceptable alternative.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium thiosulfate—(ACS) Granular.
6.3 Acetone, hexane, methanol, methylene
chloride, petroleum ether (boiling range 30-
60 °C)—Pesticide quality or equivalent.
6.4 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 °C for 4 h
in a shallow tray.
6.5 Florisil—PR Grade (60/100 mesh). Pur-
chase activated at 1250 °F and store in the
dark in glass containers with ground glass
stoppers or foil-lined screw caps. Before use,
activate each batch at least 16 h at 130 °C in
a foil-covered glass container and allow to
cool.
6.6 Ethyl ether—Nanograde, redistilled in
glass if necessary.
6.6.1 Ethyl ether must be shown to be free
of peroxides before it is used as indicated by
EM Laboratories Quant test strips. (Avail-
able from Scientific Products Co., Cat. No.
P1126-8, and other suppliers.)
6.6.2 Procedures recommended for re-
moval of peroxides are provided with the test
strips. After cleanup, 20 mL of ethyl alcohol
preservative must be added to each liter of
ether.
6.7 Stock standard solutions (1.00 ng/nL)—
Stock standard solutions can be prepared
from pure standard materials or purchased
as certified solutions.
6.7.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in acetone
and dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.7.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7.3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with check standards indicates a
problem.
6.8 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas Chromatographic oper-
ating conditions equivalent to those given in
Table 1. The gas Chromatographic system
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Pt. 136, App. A, Meth. 611
can be calibrated using the external standard
technique (Section 7.2) or the internal stand-
ard technique (Section 7.3).
7.2 External standard calibration proce-
dure:
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
hexane. One of the external standards should
be at a concentration near, but above, the
MDL (Table 1) and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7,2,2 Using injections of 2 to 5 jtL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, BSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
be suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding- vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with hexane. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 2 to 5 jiL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (BF) for each compound using
Equation 1.
Equation 1
where:
A ,=Response for the parameter to be
measured,
A,s=Response for the internal standard.
C,s=Concentration of the internal standard
RF =
(A.XC*
Cs=Conoentration of the parameter to be
measured (ug/L).
If the BP value over the working range is a
constant (<10% RSD), the KF can be assumed
to be invariant and the average BF can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, AJ An, vs, BF.
7.4 The working calibration curve, cali-
bration factor, or HP must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±15%, a new
calibration curve must be prepared for that
compound.
7.5 The cleanup procedure in Section 11
utilizes Florisil column chromatography.
Florisil from different batches or sources
may vary in adsorptive capacity. To stand-
ardize the amount of Florisil which is used,
the use of lauric acid value7 is suggested.
The referenced procedure determines the ad-
sorption from hexane solution of lauric acid
(mg) per g of Florisil. The amount of Florisil
to be used for each column is calculated by
dividing 110 by this ratio and multiplying by
20 g,
7.6 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
6. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
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40 CfR Ch. I (7-1-04 Edition)
8.1.2 In recognition of advances that are
occurring in ehromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, and 12.1) to improve the sepa-
rations or lower the cost of measurements.
Each time such a modification ia made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.8 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst mast perform tbe following operations.
8.2,1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 100
ug/mL in acetone. The QC check sample con-
centrate must be obtained from the U.S. En-
vironmental Protection Agency, Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration.
8,2,2 Using a pipet, prepare QC check sam-
ples at a concentration of 100 |ig/L by adding
1.00 mL of QC check sample concentrate to
each of four l-L allquots of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in (ig/L, for each parameter using
tie four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter. Locate and
correct the source of the problem and repeat
the test for all parameters of interest begin-
ning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1. The concentration of the spike in
the sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to S times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 100 pir/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.1.3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate {Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 10Q(A~B)%;T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1, This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.8 If spiking was
performed at a concentration lower than 100
Hg/L, the analyst must use either the QC ac-
ceptance criteria in Table 2, or optional QC
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Pt. 136, App. A, Meth. 611
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria tor the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 3, substituting
the spike concentration (T) for 0; (2) cal-
culate overall precision (S') using the equa-
tion in Table 3, substituting- X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X7T)±2.44(100 S'/T)%,8
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory.
8.4.1 Prepare the QC check standard by
adding 1.0 m/L of QC check sample con-
centrate (Section 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
tmspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P-2sp to
P+2Sp. If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the
chromatogram, confirmatory techniques
such as gas ehromatography with a dis-
similar column, specific element detector, or
mass spectrometer must be used. Whenever
possible, the laboratory should analyze
standard reference materials and participate
in relevant performance evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices* should be followed, except that the
bottle must not be prerinsed with sample be-
fore collection, Composite samples should be
collected in refrigerated glass containers in
accordance with the requirements of the pro-
gram. Automatic sampling equipment must
be as free as possible of Tygon tubing and
other potential sources of contamination,
9.2 All samples must be iced or refrig-
erated at 4 °C from the time of collection
until extraction. Fill the sample bottles and,
if residual chlorine is present, add 80 mg of
sodium thiosulfate per liter of sample and
mix well. EPA Methods 330.4 and 330.5 may
be used for measurement of residual chlo-
rine,'0 Field test kits are available for this
purpose,
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraetion.-
10. Sample Extraction
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel.
10.2 Add 60 niL methylene chloride to the
sample bottle, seal, and shake 30 s to rinse
the inner surface. Transfer the solvent to the
separatory funnel and extract the sample by
shaking the funnel for 2 min with periodic
venting to release excess pressure. Allow the
organic layer to separate from the water
phase for a minimum of 10 min. If the emul-
sion interface between layers is more than
one-third the volume of the solvent layer,
the analyst must employ mechanical tech-
niques to complete the phase separation. The
optimum technique depends upon the sam-
ple, but may include stirring, filtration of
the emulsion through glass wool, centrifuga-
tion, or other physical methods. Collect the
methylene chloride extract in a 250-mL Br-
lenmeyer flask.
10.3 Add a second 80-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Brlenmeyer
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40 CFR Ch. I (7-1-04 Edition)
flask. Perform a third extraction In the same
manner,
10,4 Assemble a Kuderna-Danlsli (K—D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour tie combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Erlenmeyer flask and col-
umn with 20 to 30 mLi of methylene chloride
to complete the quantitative transfer.
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
NOTE: Some of the haloethers are very
volatile and significant losses will occur in
concentration steps if care is not exercised.
It is important to maintain a constant
gentle evaporation rate and not to allow the
liquid volume to fall below 1 to 2 mL before
removing the K-D apparatus from tie hot
water bath.
10,7 Momentarily remove the Snyder col-
umn, add 50 mL of hexane and a new boiling
chip, and reattach the Snyder column. Raise
the temperature of the water bath to 85 to 90
°C. Concentrate the extract as in Section
10.6, except use hexane to prewet the column.
The elapsed time of concentration should be
5 to 10 min.
10.8 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of hexane, A 5-mL
syringe is recommended for this operation.
Stopper the concentrator tube and store re-
frigerated if further processing will not be
performed immediately. If the extract will
be stored longer than two days, it should be
transferred to a Teflon-sealed screw-cap vial.
If the sample extract requires no further
cleanup, proceed with gas chromatographic
analysis (Section 12), If the sample requires
further cleanup, proceed to Section 11.
10.9 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
the procedure below or any other appropriate
procedure. However, the analyst first must
demonstrate that the requirements of Sec-
tion 8.2 can be met using the method as re-
vised to incorporate the cleanup procedure.
11.2 Plorisil column cleanup for
haloethers:
11.2,1 Adjust the sample extract volume
to 10 mL.
11.2.2 Place a weight of Florisil (nomi-
nally 20 g) predetermined by calibration
(Section 7.5), into a chromatographic col-
umn. Tap the column to settle the Florisil
and add 1 to 2 cm of anhydrous sodium sul-
fate to the top.
11.2.3 Preelute the column with 50 to 60
mL of petroleum ether. Discard the eluate
and just prior to exposure of the sodium sul-
fate layer to the air, quantitatively transfer
the sample extract onto the column by de-
cantation and subsequent petroleum ether
washings. Discard the eluate. Just prior to
exposure of the sodium sulfate layer to the
air, begin eluting the column with 300 mL of
ethyl ether/petroleum ether (6+94) (VAT). Ad-
just the elution rate to approximately 5 mL/
min and collect the eluate in a 500-mL K-D
flask equipped with a 10-mL concentrator
tube. This fraction should contain all of the
haloethers.
11.2.4 Concentrate the fraction as in Sec-
tion 10.6, except use hexane to prewet the
column. When the apparatus is cool, remove
the Snyder column and rinse the flask and
its lower joint into the concentrator tube
with hexane. Adjust the volume of the
cleaned up extract to 10 mL with hexane and
analyze by gas chromatography (Section 12).
12. Gas Chromatography
12.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Examples of the sep-
arations achieved by Columns 1 and 2 are
shown in Figures 1 and 2, respectively. Other
packed or capillary (open-tubular) columns,
chromatographic conditions, or detectors
may be used if the requirements of Section
8.2 are met.
12.2 Calibrate the system daily as de-
scribed in Section 7.
12.3 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed thoroughly immediately before injec-
tion into the gas cnromatrograph.
170
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 611
12.4 Inject 2 to 5 |iL of the sample extract
or standard into the gas ehromatograph
using the solvent-flush technique," Smaller
(1,0 uL) volumes may be injected If auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 nL, the total
extract volume, and the resulting peak size
in area or peak height units.
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
chromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weight heavily in the
interpretation of chromatograms.
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze,
12,7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13, Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (fig/L) =
Equation 2
where:
A=Amount of material injected (ng).
Vj=Volume of extract injected (uL),
V,=Volume of total extract (nL).
V.,=Volume of water extracted (mL).
13.1.2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (jJ.g/L):
(Ais)(RF)(V0)
Equation 3
where:
As=Response for the parameter to he meas-
ured.
Ais=Response for the internal standard.
I,=Amount of internal standard added to
each extract (fig).
V0=Volume of water extracted (L).
13.2 Report results in ng/L without correc-
tion for recovery data. All QG data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MEL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.12
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to he applicable
over the concentration range from 4 x MDL
to 1000 x MDL.12
14.3 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 1.0 to 626 ji/L,12 Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
RBFEEENCES
1. 40 CFR part 136, appendix B.
2. "Determination of Haloethers in Indus-
trial and Municipal Wastewaters," EPA 600/4-
81-062, National Technical Information Serv-
ice, PB81-232290, Springfield, Virginia 22161,
July 1981.
3, ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constitutents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. "Carcinogens—Working Carcinogens, "
Department of Health, Education, and Wel-
fare, Public Health Services, Center for Dis-
ease Control, National Institute for Occupa-
tional Safety and Health, Publication No. 77-
206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Mills., P.A. "Variation of Plorisil Activ-
ity: Simple Method for Measuring Absorbent
Capacity and Its Use in Standardizing
171
-------
Pt, 136, App. A,Meth, 611
40 CFR Ch. I (7-1-04 Edition)
Florisil Columns," Journal of the Association
of Official Analytical Chemists, 51, 29 (1968).
8. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983), (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
9. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
10. "Methods 330.4 (Titrimetric, DPD-FAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes.
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979,
11. Burke, J.A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
12. "EPA Method Study 21, Method 611,
Haloethers," EPA 600/4-84-052, National Tech-
nical Information Service, PB84-205939,
Springfield, Virginia 22161, June 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHODS DETECTION LIMITS
Parameters
4-Bromophenyl phenyl ether
Retention time (min)
Column 1 Column 2
8.4
9.3
13.1
19.4
21.2
9.7
9.1
10.0
15.0
18.Z
Method
detection
limit (n/L)
0.8
0.3
0.5
3.9
2.3
AColumn 1 conditions: Supelcoport (100/120 mesh) coated with 3% SP-1000 packed in a 1.8 m long x Z mm ID glass column
with helium carrier gas at 40 mL/min. flow rate. Column temperature held at 60 "C for 2 rnin. after injection then programmed at
8 °C/min. to 230 °C and held for 4 min. Under these conditions the retention time for Aldrin is 22.6 min.
AColumn 2 conditions: Tenax-GC (60/80 mesh) packed in a 1.8 m Jong x 2mm ID glass column with heiium carrier gas at 40
mLJmin. flow rate. Column temperature held at 150 °C for 4 min. after injection then programmed at 16 °C/min. to 310 °C. Under
these conditions the retention time for Aldrin is 18.4 min,
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 611
Parameter
4-Chloropheny! phenyi ether
Test cone.
(|ig/L)
100
100
100
100
100
Limit for s
(TO/L)
263
257
327
393
30.7
Range for X
(ng/L)
26 3-1368
27 3-115 0
264 1 47 Q
7.6-167.5
15.4-152.5
Range for
P, P, per-
cent
1 1-152
12-128
9-165
D-189
D-170
s=Standard deviation of four recovery measurements, in ng/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in (ig/L (Section 8.2.4).
P, P,=Percent recovery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero.
NOTE: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 611
Parameter
4-ChloroDhenvl ohenvl ether
Accuracy, as
recovery, X'
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 611
COLUMN: 3% SP-1000 ON SUPELCOPORT
PR0BRAM 60°C FOR 2 WIN, 8°C/MIN TO 230°C
DETECTOR: HALL ELECTROLYTIC CONDUCTIVITY
ee
UJ
LU
LU
X
a.
O
ce
a.
O
v*
O
ee
O
O
LU
uu
O .-.
I ^M
C^< ^^
3? o
i
LU
i
Q.
O
i
CQ
02 4 6 8 10 12 14 16 18
RETENTION TIME, MIN.
Figure 1. Gas chromatogram of haloethers.
20 22 24
173
-------
Pt. 136,App. A, Meth. 612
40 CFR Ch. 1 (7-1-04 Edition)
COLUMN: TEN AX GC
PROGRAM: 150°C FOR 4 WIN, 16°C/M1N TO 310°C
DETECTOR: HALL ELECTROLYTIC CONDUCTIVITY
1
048 12 16
RETENTION TIME, MIN,
Figure 2. Gas chromatogram of haloethers.
24
METHOD 612—CHLORINATED HYDROCARBONS
1, Scope and Application
1.1 This method covers the determination
of certain chlorinated hydrocarbons. The fol-
lowing parameters can be determined by this
method:
Parameter
2-CMoronaphthaiene ,,-
1 ,2-DichlGrobenzene
1,3-Dichiorobenzene
Hexachloroethane
STORE!
No.
34581
34536
34566
34571
39700
34391
34386
34396
CAS No.
91-58-7
95-50-1
541-73-1
106-46-7
118-74-1
87-68-3
77-47-4
67-72-1
174
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 612
Parameter
STOHET
No.
345S1
CAS No.
120-82-1
1.2 This is a gas ehromatographie (GC)
method applicable to the determination of
the compounds listed above in municipal and
industrial discharges as provided under 40
CFB 136.1. When this method is used to ana-
lyze unfamiliar samples for any or all of the
compounds above, compound identifications
should be supported by at least one addi-
tional qualitative technique. This method
describes a second gas chromatographic col-
umn that can be used to confirm measure-
ments made with the primary column. Meth-
od 625 provides gas ehromatograph/mass
spectrometer (GC/MS) conditions appro-
priate for the qualitative and quantitative
confirmation of results for all of the param-
eters listed above, using the extract pro-
duced by this method.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
wastewater may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.4 The sample extraction and concentra-
tion steps in this method are essentially the
same as in Methods 606, 608, 609, and 611.
Thus, a single sample may be extracted to
measure the parameters included in the
scope of each of these methods. When clean-
up is required, the concentration levels must
be high enough to permit selecting aliquots,
as necessary, to apply appropriate cleanup
procedures. The analyst is allowed the lati-
tude, under Section 12. to select
chromatographic conditions appropriate for
the simultaneous measurement of combina-
tions of these parameters.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5.
1,6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas ehromatograph and
in the interpretation of gas cliromatograms.
Each analyst must demonstrate the ability
to generate acceptable results with this
method using the procedure described in Sec-
tion 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is extracted with meth-
ylene chloride using a separatory funnel. The
methylene chloride extract is dried and ex-
changed to hexane during concentration to a
volume of 10 mL or less. The extract is sepa-
rated by gas chromatography and the param-
eters are then measured with an electron
capture detector.2
2.2 The method provides a Plorisil column
cleanup procedure to aid in the elimination
of interferences that may be encountered.
3, Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and-'or ele-
vated baselines in gas chromatograms. All of
these materials mnst be routinely dem-
onstrated to be free from interferences under
the conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. The cleanup procedure in Section
11 can be used to overcome many of these
interferences, but unique samples may re-
quire additional cleanup approaches to
achieve the MDL listed in Table 1.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. Prom this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
175
-------
Pt. 136, App. A, Meth. 612
40 CFR Ch. I (7-1-04 Edition)
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified4 * for
the information of the analyst.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—IcL or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner rnnst be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4 °C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separatory funnel—2-L. with Teflon
stopcock.
5.2,2 Drying column—ChromatograpMc
column, approximately iQQ mrn long x 19 mm
ID, with coarse frit filter disc.
5.2,3 Chromatographic column—300 long x
10 mm ID, with Teflon stopcock and coarse
frit filter disc at bottom.
5.2.4 Concentrator tube, Kuderna-Dan-
ish 10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.5 Evaporative flask, Knderna-Danish—
500-mLi {Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5,2.6 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-50300M121 or
equivalent).
5.2,7 Vials—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 °C for 30 min or Soxhlet ex-
tract with methylene chloride.
5.4 Water bath—Heated, with concentric
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5,5 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
5.6 Gas chromatograph—An analytical
system complete with gas chromatograph
suitable for on-column injection and all re-
quired accessories including syringes, ana-
lytical columns, gases, detector, and strip-
chart recorder. A data system is rec-
ommended for measuring peak areas.
5.6.1 Column 1—1,8 m long x 2 mm ID
glass, packed with 1% SP-1000 on
Supelcoport (100/120 mesh) or equivalent.
Guidelines for the use of alternate column
packings are provide in Section 12.1.
5.6.2 Column 2—1.8 m long x2 mm ID glass,
packed with 1.5% OV-1/2.4% OV-225 on
Supelcoport (80/100 mesh) or equivalent. This
column was used to develop the method per-
formance statements in Section 14.
5.6.3 Detector— Electron capture detec-
tor. This detector has proven effective in the
analysis of wastewaters for the parameters
listed in the scope (Section 1.1), and was used
to develop the method performance state-
ments in Section 14. Guidelines for the use of
alternate detectors are provided in Section
12.1.
6, Reagents
6.1 Reagent water— Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Acetone, hexane, isooctane, methanol,
methylene chloride, petroleum ether (boiling
range 30 to 60 °C)—Pesticide quality or equiv-
alent.
6.3 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify heating at 400 °C for 4 h in a
shallow tray.
6.4 Plorisil—PE grade (60/100 mesh). Pur-
chase activated at 1250 "F and store in the
dark in glass containers with ground glass
stoppers or foil-lined screw caps. Before use,
activate each batch at least 16 h at 130 °C in
a foil-covered glass container and allow to
cool.
6.5 Stock standard solution (1.00 ng/liD—
Stock standard solutions can be prepared
from pure standard materials or purchased
as certified solutions,
6.5.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material. Dissolve the material in isooctane
and dilute to volume in a 120-rnL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight can be used without correction to cal-
culate the concentration of the stock stand-
ard. Commercially prepared stock standards
can be used at any concentration if they are
certified by the manufacturer or by an inde-
pendent source.
6.5.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
176
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 612
6.5.3 Stock standard solutions must be re-
placed after six months, or sooner if
oomparieion with check standards indicates
a problem.
6.6 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas ehromatographic oper-
ating conditions equivalent to those given in
Table 1. The gas chromatographic system
can be calibrated using the external standard
technique (Section 7.2) or the internal stand-
ard technique (Section 7.3).
7.2 External standard calibration proce-
dure;
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask and diluting to volume with
Isooctane. One of the external standards
should be at a concentration near, but above,
the MDL (Table 1) and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the detector.
7.2.2 Using injections of 2 to 5 jiL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against the mass injected. The re-
sults can be used to prepare a calibration
curve for each compound. Alternatively, if
the ratio of response to amount injected
(calibration factor) is a constant over the
working range (<10% relative standard devi-
ation, RSD), linearity through the origin can
be assumed and the average ratio or calibra-
tion factor can be used in place of a calibra-
tion curve.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select one or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Because of
these limitations, no internal standard can
he suggested that is applicable to all sam-
ples.
7.3.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding vol-
umes of one or more stock standards to a
volumetric flask. To each calibration stand-
ard, add a known constant amount of one or
more internal standards, and dilute to vol-
ume with isooctane. One of the standards
should be at a concentration near, but above,
the MDL and the other concentrations
should correspond to the expected range of
concentrations found in real samples or
should define the working range of the detec-
tor.
7.3.2 Using injections of 2 to 5 nL, analyze
each calibration standard according to Sec-
tion 12 and tabulate peak height or area re-
sponses against concentration for each com-
pound and internal standard. Calculate re-
sponse factors (BP) for each compound using
Equation 1,
RF'
(A5)(Cis)
(Ais)(Cs)
Equation 1
where:
A,.=RespQnse for the parameter to be meas-
ured.
AiB=Response for the internal standard.
C,s=Concentration of the internal standard
(tig/L).
Cs=Concentration of the parameter to be
measured (|tg/L).
If the RF value over the working range is a
constant (<10% RSD), the RP can be assumed
to be invariant and the average RP can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, As/Ai,, vs. RF.
7.4 The working calibration curve, cali-
bration factor, or RF must be verified on
each working day by the measurement of one
or more calibration standards. If the re-
sponse for any parameter varies from the
predicted response by more than ±18%, a new
calibration curve must be prepared for that
compound.
7.5 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
S. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When the results of
sample spikes indicate atypical method per-
formance, a quality control check standard
must be analyzed to confirm that the meas-
urements were performed in an in-control
mode of operation.
8,1,1 The analyst must make an initial,
one-tinie, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
177
-------
Pt. 136, App. A, Meth. 612
CFR Ch. I (7-1-04 Edition)
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.4, 11.1, and 12.1) to improve the sepa-
rations or lower the cost of measurements.
Each time such modification is made to the
method, the analyst is required to repeat the
procedure in Section 8.2.
8.1.3 Before processing' any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Bach time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples to monitor and evaluate lab-
oratory data quality. This procedure is de-
scribed in Section 8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8,4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at the following con-
centrations in acetone: Hexachloro-sub-
stituted parameters, 10 fig/mL; any other
chlorinated hydrocarbon, 100 ng/ml_i. The QC
check sample concentrate must be obtained
from the U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory in Cincinnati, Ohio, if avail-
able. If not available from that source, the
QC check sample concentrate must be ob-
tained from another external source. If not
available from either source above, the QC
check sample concentrate must be prepared
by the laboratory using stock standards pre-
pared independently from those used for cali-
bration,
8.2.2 Using a pipet, prepare QC check sam-
ples at the test concentrations shown in
Table 2 by adding 1.00 mL of QC check sam-
ple concentrate to each of four 1-L aliquots
of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
Hg/L, and the standard deviation of the re-
covery (s) in (ig/Li, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 2. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Table 2 presents a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2,6,1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.2.
8.2.6.2 Beginning with Section 8.2.2, repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spike
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at that limit or 1 to 5 times higher than
the background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter, the spike should be at the test con-
centration in Section 8.2.2 or 1 to 5 times
higher than the background concentration
determined in Section 8.3.2, whichever con-
centration would be larger,
8.3.1,3 If it is impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
by (2) the larger of either 5 times higher than
the expected background concentration or
the test concentration in Section 8.2.2.
178
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Environmental Protection Agency
Pt. 136, App. A, Merh. 612
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. In necessary, prepare a new
QC check sample concentrate (Section 8.2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 100 (A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 2. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.' If spiking was
performed at a concentration lower than the
test concentration in Section 8.2.2, the ana-
lyst must use either the QC acceptance cri-
teria in Table 2, or optional QC acceptance
criteria calculated for the specific spike con-
centration. To calculate optional acceptance
criteria for the recovery of a parameter: (1)
Calculate accuracy (X') using the equation in
Table 3, substituting the spike concentration
(T) for 0; (2) calculate overall precision (S')
using the equation in Table 3, substituting X'
for X; (3) calculate the range for recovery at
the spike concentration as (100 XVT) ± 2.44
<10QS7T)%.7
8,3,4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4. If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory,
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Sections 8.2.1 or 8.3.2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8.3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T Is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (PJ
for each parameter with the corresponding
QC acceptance criteria found in Table 2. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes,
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (Bp). Express the accuracy assessment
as a percent recovery interval from P - 2sp to
P+2sp, If P=90% and sp=10%, for example, the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment for each pa-
rameter on a regular basis (e.g. after each
five to ten new accuracy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. When doubt exists
over the identification of a peak on the chro-
matogram, confirmatory techniques such, as
gas chromatography with a dissimilar col-
umn, specific element detector, or mass
spectrometer must be used. Whenever pos-
sible, the laboratory should analyze standard
reference materials and participate in
relevent performance evaluation studies.
S. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices" should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All samples must be iced or refrig-
erated at 4°C from the time of collection
until extraction.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
10. Sample Extraction
10,1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel.
179
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Pt. 136, App. A, Meth. 612
40 CFR Ch. I (7-1-04 Edition)
10.2 Add 60 mL of methylele chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask.
10.3 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner.
10.4 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used in place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.5 Pour the combined extract through a
solvent-rinsed drying column containing
about 10 cm of anhydrous sodium sulfate,
and collect the extract in the K-D concen-
trator. Rinse the Erlenmeyer flask and col-
umn with 20 to 30 mL of methylene chloride
to complete the quantitative transfer.
10.6 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 mL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 to 2 mL, remove the K-D apparatus and
allow it to drain and cool for at least 10 min.
NOTE: The dichloribenzenes have a suffi-
ciently high volatility that significant losses
may occur in concentration steps if care is
not exercised. It is important to maintain a
constant gentle evaporation rate and not to
allow the liquid volume to fall below 1 to 2
mL before removing the K-D apparatus from
the hot water bath.
10.7 Momentarily remove the Snyder col-
umn, add 50 mL of hexane and a new boiling
chip, and reattach the Snyder column. Raise
the tempeature of the water bath to 85 to 90
°C. Concentrate the extract as in Section
10.6, except use hexane to prewet the column.
The elapsed time of concentration should be
5 to 10 min.
10.8 Remove the Snyder column and rinse
the flask and its lower joint into the concen-
trator tube with 1 to 2 mL of hexane. A 5-mL
syringe is recommended for this operation.
Stopper the concentrator tube and store re-
frigerated if further processing will not be
performed immediately. If the extract will
be stored longer than two days, it should be
transferred to a Teflon-sealed screw-cap vial.
If the sample extract requires no further
cleanup, proceed with gas chromatographic
analysis (Section 12). If the sample requires
further cleanup, proceed to Section 11.
10.9 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 mL.
11. Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
the procedure below or any other appropriate
procedure. However, the analyst first must
demonstrate that the requirements of Sec-
tion 8.2 can be met using the method as re-
vised to incorporate the cleanup procedure.
11.2 Plorisll column cleanup for
chlorinated hydrocarbons:
11.2.1 Adjust the sample extract to 10 mL
with hexane.
11.2.2 Place 12 g of Florisil into a
chromatographic column. Tap the column to
settle the Plorisil and add 1 to 2 cm of anhy-
drous sodium sulfate to the top.
11.2.3 Preelute the column with 100 mL of
petroleum ether. Discard the eluate and just
prior to exposure of the sodium sulfate layer
to the air, quantitatively transfer the sam-
ple extract onto the column by decantation
and subsequent petroleum ether washings.
Discard the eluate. Just prior to exposure of
the sodium sulfate layer to the air, begin
eluting the column with 200 mL of petroleum
ether and collect the eluate in a 500-mL K-D
flask equipped with a 10-mL concentrator
tube. This fraction should contain all of the
chlorinated hydrocarbons.
11.2.4 Concentrate the fraction as in Sec-
tion 10.6, except use hexane to prewet the
column. When the apparatus is cool, remove
the Snyder column and rinse the flask and
its lower joint into the concentrator tube
with hexane. Analyze by gas chroma-
tography (Section 12).
180
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Environmental Protection Agency
Pt. 136,App. A, Meth, 612
12. Gas Chromatography
12.1 Table 1 summarizes the recommended
operating conditions for the gas chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Examples of the sep-
arations achieved by Columl 2 are shown in
Figures 1 and 2. Other packed or capillary
(open-tubular) columns, chromatographic
conditions, or detectors may be used if the
requirements of Section 8.2 are met.
12.2 Calibrate the system daily as de-
scribed in Section 7.
12.3 If the internal standard calibration
procedure is being used, the internal stand-
ard must be added to the sample extract and
mixed throughly Immediately before injec-
tion into the gas chromatograph.
12.4 Inject 2 to 5 uL of the sample extract
or standard into the gas chromatograph
using the solvent-flush techlique,9 Smaller
(1.0 (iL) volumes may be injected if auto-
matic devices are employed. Record the vol-
ume injected to the nearest 0.05 uL, the total
extract volume, and the resulting; peak size
in area or peak height units.
12.5 Identify the parameters in the sample
by comparing the retention times of the
peaks in the sample chromatogram with
those of the peaks in standard
ehromatograms. The width of the retention
time window used to make identifications
should be based upon measurements of ac-
tual retention time variations of standards
over the course of a day. Three times the
standard deviation of a retention time for a
compound can be used to calculate a sug-
gested window size; however, the experience
of the analyst should weigh heavily in the
interpretation of ehromatograms.
12.6 If the response for a peak exceeds the
working range of the system, dilute the ex-
tract and reanalyze.
12.7 If the measurement of the peak re-
sponse is prevented by the presence of inter-
ferences, further cleanup is required.
13. Calculations
13.1 Determine the concentration of indi-
vidual compounds in the sample.
13.1.1 If the external standard calibration
procedure is used, calculate the amount of
material injected from the peak response
using the calibration curve or calibration
factor determined in Section 7.2.2. The con-
centration in the sample can be calculated
from Equation 2.
Concentration (jig/L) =
(A)(Vt)
Vi=Volume of extract injected (uL).
V,=¥olume of total extract (|iL).
V,=Volume of water extracted (mL).
13.1,2 If the internal standard calibration
procedure is used, calculate the concentra-
tion in the sample using the response factor
(RF) determined in Section 7.3.2 and Equa-
tion 3.
Concentration (|ig/L) =
(AS)(IS)
Ais)(RF)(V0)
Equation 2
where:
A=Amount of material injected (ng).
Equation 3
where:
A,,=Response for the parameter to be meas-
ured.
Ais=Besponse for the internal standard.
I4=Amount of internal standard added to
each extract (jjg).
V,,=Volume of water extracted (L).
13.2 Report results in (ig/L without correc-
tion for recovery data. All QO data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.' The MDL concentrations listed in
Table 1 were obtained using reagent water.10
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method has been tested for lin-
earity of spike recovery from reagent water
and has been demonstrated to be applicable
over the concentration range from 4xMDL to
lOOOxMDL.i"
14.3 This method was tested by 20 labora-
tories using reagent water, drinking water,
surface water, and three industrial
wastewaters spiked at six concentrations
over the range 1.0 to 356 ugr/L." Single oper-
ator precision, overall precision, and method
accuracy were found to be directly related to
the concentration of the parameter and es-
sentially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
REFERENCES
1. 40 CPR part 136, appendix B.
2. "Determination of Chlorinated Hydro-
carbons In Industrial and Municipal
Wastewaters, "EPA 6090/4-84-ABC, National
Technical Information Service, PBXYZ,
Springfield, Virginia, 22161 November 1984.
181
-------
Pt. 136, App. A, Meth. 612
40 CFR Ch. i (7-1-04 Edition)
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing- and Materials, Philadel-
phia.
4, "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
"Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206. August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFE part 1910), Occu-
pational Safety and Health. Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data,,"American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8,3.3 is two
times the value 1.22 derived in this report.)
8. ASTM Annual Book of Standards, Part
31, D3370-76. "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
9. Burke, J.A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48, 1037 (1965).
10. "Development of Detection Limits, EPA
Method 612, Chlorinated Hydrocarbons," Spe-
cial letter report for EPA Contract 68-03-
2625, U.S. Environmental Protection Agency,
Environmental Monitoring and Support Lab-
oratory, Cincinnati, Ohio 45268.
11. "EPA Method Study Method 612—
Chlorinated Hydrocarbons," EPA 600/4-84-039,
National Technical Information Service,
PB84-187772, Springfield, Virginia 22161, May
1984.
12. "Method Performance for
Hexachlorocyclopentadiene by Method 612,"
Memorandum from R. Slater, U.S. Environ-
mental Protection Agency, Environmental
Monitoring and Support Laboratory, Cin-
cinnati, Ohio 45268, December 7, 1983.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND METHOD DETECTION LIMITS
Parameter
Hexachlorobenzene
Retention time (min)
Column 1
4.5
4.9
5.2
6.6
7.7
15.5
nd
•2.7
•5.6
Column 2
6.8
8.3
7.6
9.3
20.0
22.3
'16.5
b3.6
»10.1
Method de-
tection limit
WL)
1.19
0.03
1.34
1.14
0.34
0.05
0.40
0.94
0.05
Column 1 conditions: Supelcoport (100/120 mesh) coated with 1% SP-1000 packed in a 1.8 m x 2 mm ID glass column wilh
5% methane/95% argon carrier gas at 25 mUmin. flow rate. Column temperature heid isothermal at 6$ eC, except where other-
wise indicated.
Column 2 conditions: Supelcoport (80/100 mesh) coated with 1.5% OV-1/2.4% OV-225 packed in a 1.8 m x 2 mm ID glass
column with 5% methane/95% argon carrier gas at 25 rnUmin. flow rate. Column temperature held Isothermal at 75 °C, except
where otherwise indicated.
nd=Not determined.
»150 °C column temperature.
" 165 °C column temperature.
c 100 °C coiumn temperature.
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD 612
Parameter
1 ,2,4-Trichlorobenzene
Test
cone, (ug/
L)
100
100
100
100
10
10
10
10
100
Limit for s
(ug/L)
37.3
283
26.4
20.8
24
22
2.5
3.3
31.6
Range for X
(ug/L)
29.5-126.9
23 5-145 1
7.2-138.6
22.7-128.9
26-148
D-12.7
D-10.4
2.4-12.3
20.2-133.7
Range for
P, P»
(percent)
9-148
9-160
D-150
13-137
15-159
D-139
D-111
8-139
5-149
^Standard deviation of four recovery measurements, in \ig/L (Section 8.2,4),
X=Average recovery for four recovery measurements, in \io/L (Section 8.2.4).
P, Ps=Percent recovery measured (Section 8,3.2, Section 8.4.2).
D=Detected; result must be greater than zero,
NOTE: These criteria are based directly upon the method performance data in Table 3. Where necessary, the iirnits for recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 3.
182
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Environmental Protection Agency
Pt, 136, App. A, Meth. 612
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 612
Overall preci-
sion, S' (ng/L.)
2-Chloronaphthatene ..
1,2-Dichlorobenzene ..
1,3-Dichlo.robenzene .........
1,4-Dichlorobenzene ,.,.,.,..
Hexachlorobenzene
Hexachlorobufadiene .,,......
Hexaehlorocyciopentadiene
Hexachloroethane ....,.,.,,,..
1.2,4-TrichIorobenzenfc ......
X'=Expected recovery for one or more measurements of a sample containing a concenirafion of C, in ucj/L
s/=Expected single analyst standard deviation of measurements at an average concentration found of X, ;n pg/'L
S'=Expected interiaboratory standard deviation of measurements at an average concentration found o! X, in ug/L.
C=True value for the concentration, in ^g/L.
X-Average recovery found for measurements of samples containing a concentration of C. in ug-1.
•'Estimates based upon the performance in a single laboratory-12
183
203-160 D-?
-------
Pf. 136, App. A, Meth. 612
40 CFR Ch, I (7-1-04 Edition)
COLUMN: 1.5% 0V-1/2.4% OV-225 ON SUPELCOPORT
TEMPERATURE: 75*t
DETECTOR: ELECTRON CAPTURE
0 4 8 12 16 20 24
RETENTION TIME, IS/UN.
Figure 1. Gas chromatogram of chlorinated hydrocarbons.
184
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Environmental Protection Agency
Pt. 136, App. A.Meth. 612
COLUMN: 1.5% OV-1/2,4% OV-225 ON SUPELCQPORT
TEMPERATURE: 165'C
DETECTOR: ELECTRON CAPTURE
UJ
a.
O
cc
O
O
UJ
5
to
O
O
yj
0 4 8 12
RETENTION TIME, MIN.
Figure 2. Gas chromatogram of chlorinated hydrocarbons.
185
-------
Pt. 136, App. A, Meih. 613
40 CFR Ch. I (7-1-04 Edition)
METHOD 613—2,3,7,8-TETRACHLORODIBBNZO-P-
DlOXIN
1. Scope and Application
1,1 This method covers the determination
of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-
TCDD). The following parameter may be de-
termined by this method:
Parameter
2,3,7,8-TCDD
GAS
1746-01-6
1.2 This is a gas chromatographic/mass
spectrometer (GC/MS) method applicable to
the determination of 2.3,7,8-TCDD in munic-
ipal and industrial discharges as provided
under 40 CPR 136.1. Method 625 may be used
to screen samples for 2,3,7,8-TCDD. When the
screening test is positive, the final quali-
tative confirmation and quantification must
be made using Method 613.
1.3 The method detection limit (MDL, de-
fined in Section 14.1)J for 2,3,7,8-TCDD is
listed in Table 1. The MDL for a specific
wastewater may be different from that list-
ed, depending upon the nature of inter-
ferences in the sample matrix,
1.4 Because of the extreme toxioity of this
compound, the analyst must prevent expo-
sure to himself, of to others, by materials
knows or believed to contain 2,3,7,8-TCDD.
Section 4 of this method contains guidelines
and protocols that, serve as minimum safe-
handling standards in a limited-access lab-
oratory.
1.5 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5.
1.6 TMs method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas ehromatograph/
mass spectrometer and in the interpretation
of mass spectra. Bach analyst must dem-
onstrate the ability to generate acceptable
results with this method using the procedure
described in Section 8.2.
2. Summary of Method
2.1 A measured volume of sample, ap-
proximately 1-L, is spiked with an internal
standard of labeled 2,3,7,8-TCDD and ex-
tracted with methylene chloride using a
separatory funnel. The methylene chloride
extract is exchanged to hexane during con-
centration to a volume of 1.0 mL or less. The
extract is then analyzed by capillary column
GO/MS to separate and measure 2,3.7.8-
TGDD.2-'
2.2 The method provides selected column
cb.romatograpb.ie cleanup proceudres to aid
in the elimination of interferences that may
be encountered.
3, Interferences
3.1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated backgrounds at the masses (m/z) mon-
itored. All of these materials must be rou-
tinely demonstrated to be free from inter-
ferences under the conditions of the analysis
by running laboratory reagent blanks as de-
scribed in Section 8.1.3.
3.1.1 Glassware must be scrupulously
cleaned.1* Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water.
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by the treatment. Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thorough rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to miiiinniize interference
problems. Purification of solvents by dis-
tillation in all-glass systems may be re-
quired.
3.2 Matrix interferences may be caused by
contaminants that are coextracted from the
sample. The extent of matrix interferences
will xrary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled. 2,3,7,8-TCDD is often associated
with other interfering chlorinated com-
pounds which are at concentrations several
magnitudes higher than that of 2,3,7.8-TCDD.
The cleanup producers in Section 11 can be
used to overcome many of these Inter-
ferences, but unique samples may require ad-
ditional cleanup approaches '•'-7 to eliminate
false positives and achieve the MDL listed in
Table 1.
3.3 The primary column, SP-2330 or equiv-
alent, resolves 2,3,7,8-TCDD from the other
21 TCDD insomers. Positive results using
any other gas chromatographic column must
be confirmed using the primary column.
4,1 The toxioity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. Prom this viewpoint, ex-
posure to these chemicals must be reduced to
186
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Environmental Protection Agency
Pt. 136, App. A, Meth. 613
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining' a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od, A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified"-10 for
the information of the analyst. Benzene and
2,3,7,8-TCDD have been identified as sus-
pected human or mammalian carcinogens.
4,2 Each laboratory must develop a strict
safety program for handling 2,3,7,8-TCDD.
The following laboratory practices are rec-
ommended:
4.2.1 Contamination of the laboratory will
be minimized by conducting all manipula-
tions in a hood.
4.2.2 The effluents of sample splitters for
the gas chromatograph and roughing pumps
on the GC/MS should pass through either a
column of activated charcoal or be bubbled
through a trap containing oil or high-boiling
alcohols.
4.2.3 Liquid waste should be dissolved in
methanol or ethanol and irradiated with ul-
traviolet light, with a wavelength greater
than 290 nrn for several days. (Use P 40 BL
lamps or equivalent). Analyze liquid wastes
and dispose of the solutions when 2,3,7,8-
TCDD can no longer be detected.
4.3 Dow Chemical U.S.A. has issued the
following precautimns (revised November
1978) for safe handling of 2,3.7,8-TCDD in the
laboratory:
4.3.1 The following statements on safe
handling are as complete as possible on the
basis of available toxicological information.
The precautions for safe handling and use
are necessarily general in nature since de-
tailed, specific recommendations can be
made only tor the particular exposure and
circumstances of each individual use. Inquir-
ies about specific operations or uses may be
addressed to the Dow Chemical Company.
Assistance in evaluating the health hazards
of particular plant conditions may be ob-
tained from certain consulting laboratories
and from State Departments of Health or of
Labor, many of which have an industrial
health service. 2,3.7.8-TCDD is extremely
toxic to laboratory animals. However, it has
been handled for years without injury in an-
alytical and biological laboratories. Tech-
niques used in handling radioactive and in-
fectious materials are applicable to 2.3.7,8,-
TCDD.
4.3.1.1 Protective equipment ^Throw-
away plastic gloves, apron or lab coat, safety
glasses, and a lab hood adequate for radio-
active work.
4.3.1.2 Training—Workers must be trained
in the proper method of removing contami-
nated gloves and clothing' without con-
tacting the exterior surfaces.
4.3,1.3 Personal hygiene—Thorough wash-
ing of hands and forearms after each manipu-
lation and before breaks (coffee, lunch, and
shift).
4.3.1.4 Confinement—Isolated work area,
posted with signs, segregated glassware and
tools, plastic-backed absorbent paper on
benchtops.
4.3.1.5 Waste—Good technique includes
minimizing contaminated waste. Plastic bag
liners should be used in waste cans. Janitors
must be trained in the safe handling of
waste.
4.3.1.6 Disposal of wastes—2.3,7,8-TCDD
decomposes above 800 °C. Low-level waste
such as absorbent paper, tissues, animal re-
mains, and plastic gloves may be burned in a
good incinerator. Gross quantities (milli-
grams) should be packaged securely and dis-
posed through commercial or governmental
channels which are capable of handling high-
level radioactive wastes or extremely toxic
wastes. Liquids should be allowed to evapo-
rate in a good hood and in a disposable con-
tainer. Residues may then be handled as
above.
4.3.1.7 Decontamination—For personal de-
contamination, use any mild soap with plen-
ty of scrubbing action. For decontamination
of glassware, tools. and surfaces,
Chlorothene NU Solvent (Trademark of the
Dow Chemical Company) is the least toxic
solvent shown to be effective. Satisfactory
cleaning may be accomplished by rinsing
with Chlorothene, then washing with any de-
tergent and water. Dishwater may be dis-
posed to the sewer. It is prudent to minimize
solvent wastes because they may require spe-
cial disposal through commercial sources
which are expensive.
4.3.1.8 Laundry—Clothing- known to be
contaminated should he disposed with the
precautions described under Section 4.3.1.8.
Lab coats or other clothing worn in 2.3.7,8--
TCDD work areas may be laundered.
Clothing should be collected in plastic
bags. Persons who convey the bags and laun-
der the clothing should be advised of the haz-
ard and trained in proper handling. The
clothing may be put into a washer without
contact if the launderer knows the problem.
The washer should be run through a cycle be-
fore being used again for other clothing.
4.3.1.9 Wipe tests—A useful method of de-
termining" cleanliness of work surfaces and
tools is to wipe the surface with a piece of
filter paper. Extraction and analysis by gas
chromatography can achieve a limit of sensi-
tivity of 0,1 ug per wipe. Less than 1 ug of
2.3,7,8-TCDD per sample indicates acceptable
cleanliness: anything higher warrants far-
ther cleaning. More than 10 ug on a wipe
sample constitutes an acute hazard and re-
quires prompt cleaning before further use of
the equipment or work space. A high f>10 ug)
187
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Pt. 136, App. A, Meth. 613
40 CFR Ch. 1 (7-1-04 Edition)
2,3,7,8-TCDD level indicates that unaccept-
able work practices have been employed in
the past.
4.3.1.10 Inhalation—Any procedure that
may produce airborne contamination must
be done with good ventilation. Gross losses
to a ventilation system must not be allowed.
Handling of the dilute solutions normally
used in analytical and animal work presents
no inhalation hazards except in the case of
an accident.
•1.3.1.11 Accidents—Remove contaminated
clothing" immediately, taking precautions
not to contaminate skin or other articles.
Wash exposed skin vigorously and repeatedly
until medical attention is obtained.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composite sampling.
5.1.1 Grab sample bottle—1-L or 1-qt,
amber glass, fitted with a screw cap lined
with Teflon. Poll may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone, or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional)—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 mL of sample. Sample containers must be
kept refrigerated at 4 °C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used. Before use, however, the compressible
tubing should be thoroughly rinsed with
methanol, followed by repeated rinsings with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.1.3 Clearly label all samples as "POI-
SON" and ship according to U.S. Department
of Transportation regulations.
5.2 Glassware (All specifications are sug-
gested. Catalog numbers are included for il-
lustration only.):
5.2.1 Separators funnels—2-L and 125-mL,
with Teflon stopcock.
5.2.2 Concentrator tube, Kuderna-Dan-
ish— 10-mL, graduated (Kontes K-570050-1025
or equivalent). Calibration must be checked
at the volumes employed in the test. Ground
glass stopper is used to prevent evaporation
of extracts.
5.2.3 Evaporative flask, Kuderna-Danish—
500-mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.4 Snyder column, Kuderna-Danish—
Three-ball macro (Kontes K-503000-0121 or
equivalent).
5.2.5 Snyder column, Kuderna-Danish—
Two-ball micro (Kontes K-569001-0219 or
equivalent).
5,2.6 Vials-—10 to 15-mL, amber glass, with
Teflon-lined screw cap.
5.2.7 Chrornatographic column—300 mm
long x 10 mm ID, with Teflon stopcock and
coarse frit filter disc at bottom.
5.2.8 Chromatographic column—400 mm
long x 11 mm ID, with Teflon stopcock and
coarse frit filter disc at bottom.
5.3 Boiling chips—Approximately 10/40
mesh. Heat to 400 "C for 30 min or Soxhlet ex-
tract with methylene chloride.
5,4 Water bath—Keated, with concentric-
ring cover, capable of temperature control
(±2 °C). The bath should be used in a hood.
5.5 GC/MS system:
5.5.1 Gas chromatograph—An analytical
system complete with a temperature pro-
grammable gas chromatograph and all re-
quired accessories including syringes, ana-
lytical columns, and gases. The injection
port must be designed for capillary columns.
Either split, splitless, or on-column injection
techniques may be employed, as long as the
requirements of Section 7.1.1 are achieved.
5.5.2 Column—60 m long x 0.25 mm ID
glass or fused silica, coated with SP-2330 (or
equivalent) with a film thickness of 0.2 |im.
Any equivalent column must resolve 2, 3, 7,
8-TCDD from the other 21 TCDD isomers."
5.5.3 Mass spectrometer—Either a low res-
olution mass spectrometer (LRMS) or a high
resolution mass spectrometer (HUMS) may
be used. The mass spectrometer must be
equipped with a 70 V (nominal) ion source
and be capable of aquiring m/z abundance
data in real time selected ion monitoring
(SIM) for groups of four or more masses.
5.5.4 GC/MS interface—Any GO to MS
interface can be used tha-t achieves the re-
quirements of Section 7.1.1. GC to MS inter-
faces constructed of all glass or glass-lined
materials are recommended. Glass surfaces
can be deactivated by silanizing* with
dichlorodimethylsilane. To achieve max-
imum sensitivity, the exit end of the cap-
illary column should be placed in the ion
source, A short piece of fused silica capillary
can be used as the interface to overcome
problems associated with straightening" the
exit end of glass capillary columns.
5.5.5 The SIM data acquired during the
Chromatographic program is defined as the
Selected Ion Current Profile (SICP). The
SICP can be acquired under computer con-
trol or as a real time analog output. If com-
puter control is used, there must be software
available to plot the SICP and report peak
height or area data for any m/z in the SICP
between specified time or scan number lim-
its.
5.6 Balance—Analytical, capable of accu-
rately xveighing 0.0001 g.
6. Reagents
6,1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of 2, 3, 7, 8-TCDD,
188
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Environmental Protection Agency
Pt. 136, App. A, Meth. 613
6.2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilute to 100 mL. Wash the solution with
methylene chloride and liexane before use.
6.3 Sodium thiosulfate—(ACS) Granular.
6,4 Sulfuric acid—Concentrated (ACS, sp,
gr. 1.84).
6.5 Acetone, methylene chloride, hexane,
benzene, ortho-xylene, tetradecane—Pes-
ticide quality or equivalent.
6.6 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 °0 for 4 h
in a shallow tray.
6.7 Alumina—Neutral, 80/200 mesh (Fisher
Scientific Co., No. A-54Q or equivalent). Be-
fore use, activate for 24 h at 130 °C in a foil-
covered glass container.
6.8 Silica gel—High purity grade, 100/120
mesh (Fisher Scientific Co., No. S-679 or
equivalent).
6.9 Stock standard solutions (1.00 (ig/uL)—
Stock standard solutimns can be prepared
from pure standard materials or purchased
as certified solutions. Acetone should be
used as the solvent for spiking solutions;
ortho-xylene is recommended for calibration
standards for split injectors; and tetradecane
is recommended for splitless or on-coluin
injectors. Analyze stock internal standards
to verify the absence of native 2,3,7,8-TCDD.
6.9.1 Prepare stock standard solutions of
2,3,7,8-TCDD (mol wt 320) and either -«C14
2,3,7,8-TCDD (mol wt 328) or "Cl,; 2,3,7,8-
TCDD (mol wt 332) in an isolated area by ac-
curately weighing about 0.0100 g of pure ma-
terial. Dissolve the material in pesticide
quality solvent and dilute to volume in a 10-
mL volumetric flask. When compound purity
is assayed to be 96% or greater, the weight
can be used without correction to calculate
the concentration of the stock standard.
Commercially prepared stock standards can
be used at any concentration if they are cer-
tified by the manufacturer or by an inde-
pendent source.
6.9.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store in an isolated refrigerator protected
from light. Stock standard solutions should
be checked frequently for signs of degrada-
tion or evaporation, especially Just prior to
preparing calibration standards or spiking
solutions from them.
6.9.3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with check standards indicates a
problem.
6.10 Internal standard spiking solution (25
ng/mL)—Using" stock standard solution, pre-
pare a spiking solution in acetone of either
'•'Cli.. or '"C)4 2,3,7,8-TCDD at a concentra-
tion of 25 Tig,mL. (See Section 10.2)
6.11 Quality control check sample eon-
cem rate—-See Section 8.2.1.
7. Calibration
7.1 Establish gas chromatograhic oper-
ating conditions equivalent to those given in
Ta.ble 1 and SIM conditions for the mass
spectrometer as described in Section 12.2 The
GC/MS system must be calibrated using the
internal standard technique.
7.1.1 Using stock standards, prepare cali-
bration standards that will allow measure-
ment of relative response factors of at least
three concentration ratios of 2,3,7.8-TCDD to
internal standard. Bach calibration standard
must be prepared to contain the internal
standard at a concentration of 25 ng/mL. If
any interferences are contributed by the in-
ternal standard at m/z 320 and 322, its con-
centration may be reduced in the calibration
standards and in the internal standard spik-
ing solution (Section 6.10). One of the cali-
bration standards should contain 2,3,7,8-
TCDD at a concentration near, but above,
the MDL and the other 2,3,7,8-TCDD con-
centrations should correspond to the ex-
pected range of concentrations found in real
samples or should define the working range
of the GC/MS system.
7.1.2 Using injections of 2 to 5 uL, analyze
each calibration standardaccording to Sec-
tion 12 and tabulate peak height or area re-
sponse against the concentration of 2,3,7,8--
TCDD and internal standard. Calculate re-
sponse factors (RF) for 2,3,7,8-TCDD using
Equation 1.
RF =
(AS)(C1S)
(Ais)(Cs)
Equation 1
where:
A,=SIM response for 2,3,7,8-TCDD m/z 320.
Aiv=SIM response for the internal standard.
m/z 332 for 13C12 2.3,7,8-TCDD m/z 328 for
37 C14 2,3,7,8-TCDD.
Cls=Concentration of the internal standard
(ug/L).
C,=Concentration of 2,3,7,8-TCDD (tig>'L).
If the BP value over the working range is a
constant (<10% relative standard deviation,
RSD), the RF can be assumed to be invariant
and the average RF can be used for calcula-
tions, Alternatively, the results can be used
to plot a calibration curve of response ratios,
A/A;«, vs. RF.
7.1.3 The working calibration curve or RF
must be verified on each working day by the
measurement of one or mare 2,3,7,8-TCDD
calibration standards. If the response for
2.3,7,8-TCDD varies from the predicted re-
sponse by more *:han ±!S% the lest must be
repeated using- a fresh calibration standard.
Alternatively, a new calibration curve must
be prepared.
189
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Pt. 136, App. A, Meth. 613
40 CFR Ch. I (7-1-04 Edition)
7.2 Before using any cleanup procedure,
the analyst must process a series of calibra-
tion standards through the procedure to vali-
date elution patterns and the absence of
interferences from the reagents.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1.2 In recognition of advances that are
occurring in chromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.5, 11.1, and 12.1) to improve the sepa-
rations or lower the cost of measurements.
Each time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8,2
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Bach time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 10%
of all samples with native 2,3,7,8-TCDD to
monitor and evaluate laboratory data qual-
ity. This procedure is described in Section
8.3.
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 10% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure Is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing 2,3,7,8-
TCDD at a concentration of 0.100 (ig/mL in
acetone. The QC check sample concentrate
must be obtained from the U.S. Environ-
mental Protection Agency, Environmental
Monitoring and Support Laboratory in Cin-
cinnati, Ohio, If available. If not available
from that source, the QC check sample con-
centrate must be obtained from another ex-
ternal source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared Independ-
ently from those used for calibration.
8.2.2 Using a pipet, prepare QC check sam-
ples at a concentration of 0.100 ng/L (100 ng/
L) by adding 1.00 mL of QC check sample
concentrate to each of four 1-L aliquots of
reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10.
8.2.4 Calculate the average recovery (X) in
\igfii, and the standard deviation of the re-
covery (s) in |ig/L, for 2,3,7,8-TCDD using the
four results,
8.2.5 Compare s and (X) with the cor-
responding acceptance criteria for precision
and accuracy, respectively, found in Table 2.
If s and X meet the acceptance criteria, the
system performance is acceptable and anal-
ysis of actual samples can begin. If s exceeds
the precision limit or X falls outside the
range for accuracy, the system performance
is unacceptable for 2,3,7,8-TCDD. Locate and
correct the source of the problem and repeat
the test beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing-
basis, spike at least 10% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing one to
ten samples per month, at least one spiked
sample per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of 2,3,7,8-TCDD in the
sample is being checked against a regulatory
concentration limit, the spike should be at
that limit or 1 to 5 times higher than the
background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1.2 If the concentration of 2,3,7,8-TCDD
in the sample is not being checked against a
limit specific to that parameter, the spike
should be at 0.100 (ig/L or 1 to 5 times higher
than the background concentration deter-
mined in Section 8.3.2, whichever concentra-
tion would be larger.
8.3.1.3 If it is Impractical to determine
background levels before spiking (e.g., max-
imum holding times will be exceeded), the
190
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Environmental Protection Agency
Pt. 136, App. A, Meth. 613
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
0.100 ng'L,
8,3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
2,3,7,8-TCDD. If necessary, prepare a new QC
check sample concentrate (Section 8.2.1) ap-
propriate for the background concentration
in the sample. Spike a second sample aliquot
with 1.0 mL of the QC check sample con-
centrate and analyze it to determine the
concentration after spiking (A) of 2.3,7,8-
TCDD. Calculate percent recovery (P) as
100(A-B)%T. where T is the known true value
of the spike.
8.3.3 Compare the percent recovery (P) for
2,3,7,8-TCDD with the corresponding QC ac-
ceptance criteria found in Table 2. These ac-
ceptance criteria were calculated to include
an allowance for error in measurement of
both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1." If spiking was
performed at a concentration lower than
0,100 ng.-ij, the analyst must use either the
QC acceptance criteria in Table 2, or op-
tional QC acceptance criteria calculated for
the specific spike concentration. To cal-
culate optional acceptance criteria for the
recovery of 2,3,7,8-TCDD: (1) Calculate accu-
racy (X') using the equation in Table 3, sub-
stituting the spike concentration (T) for C;
(2) calculate overall precision (S') using the
equation in Table 3, substituting X' for X; (3)
calculate the range for recovery at the spike
concentration as (100 X'/T)±2.44(100 S'/T)%. "
8.3,4 If the recovery of 2,3,7,8-TCDD falls
outside the designated range for recovery, a
check standard must be analyzed as de-
scribed in Section 8.4.
8.4 If the recovery of 2,3,7,8-TCDD fails
the acceptance criteria for recovery in Sec-
tion 8,3, a QC check standard must be pre-
pared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the complexity of the sample matrix and the
performance of the laboratory.
8.4.1 Prepare the QC check 'standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8.2,1 or 8.3.2) to 1 L of rea-
gent water.
8.4,2 Analyze the QC check standard to
determine the concentration measured (A) of
2,3,7,8-TCDD. Calculate the percent recovery
(Ps) as 100 (A/T)%, where T is the true value
of the standard concentration,
8.4.3 Compare the percent recovery (Ps)
with the corresponding QC acceptance cri-
teria found In Table 2. If the recovery of
2,3,7,8-TCDD falls outside the designated
range, the laboratory performance is judged
to be out of control, and the problem must
be immediately identified and corrected. The
analytical result for 2,3,7,8-TCDD in the
unspiked sample Is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the spandard deviation of the percent re-
covery (S|,i. Express the accuracy assessment
as a percent recovery interval from P-2s,, to
P+2s,,. If P=90% and Sp=10%. for example, 'the
accuracy interval is expressed as 70-110%.
Update the accuracy assessment on a regular
basis (e.g. after each five to ten new accu-
racy measurements).
8.6 It is recommended that the laboratory
adopt additional quality assurance pri'.otiees
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. Whenever possible,
the laboratory should analyze standard ref-
erence materials and participate in relevant
performance evaluation studies,
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples must be collected in
glass containers. Conventional sampling
practices12 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
he collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion,
9.2 All samples must be iced or refrig-
erated at 4 CC and protected from light from
the time of collection until extraction. Fill
the sample bottles and, if residual chlorine is
present, add 80 mg of sodium thiosulfate per
liter of sample and mix well. EPA Methods
330.4 and 330.5 may be nsed for measurement
of residual chlorine.13 Field test kits are
available for this purpose.
9,3 Label all samples and containers
"POISON" and ship according- to applicable
U.S. Department of Transportation regula-
tions.
9.4 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.2
70. Sample Extraction
CAUTION: When using this method to ana-
lyze for 2,3,7,8-TCDD, all of the following- op-
erations must be performed in a limited-ac-
cess laboratory with the analyst wearing full
191
-------
Pf. 136, App. A, Meth. 613
40 CFR Ch. I (7-1-04 Edition)
protective covering for all exposed skin sur-
faces. See Section 4,2,
10.1 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-it separator? funnel,
10.2 Add 1.00 mL of internal standard
spiking solution to the sample in the sepa-
ratory funnel. If the final extract will be
concentrated to a fixed volume below 1.00
mL (Section 12.3), only that volume of spik-
ing solution should be added to the sample so
that the final extract will contain 25 ngv'mL
of internal standard at the time of analysis.
10.3 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the vmlume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugatlon, or other physical methods. Col-
lect the methylene chloride extract in a 250-
niL Erlenmeyer flask.
10.4 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining the extracts In the Erlenmeyer
flask. Perform a third extraction in the same
manner.
10.5 Assemble a Kuderna-Danish (K-D)
concentrator by attaching a 10-mL concen-
trator tube to a 500-mL evaporative flask.
Other concentration devices or techniques
may be used In place of the K-D concen-
trator if the requirements of Section 8.2 are
met.
10.6 Pour the combined extract into the
K-D concentrator. Rinse the Erlenmeyer
flask with 20 to 30 mL of methylele chloride
to complete the quantitative transfer.
10.7 Add one or two clean boiling chips to
the evaporative flask and attach a three-ball
Snyder column. Prewet the Snyder column
by adding about 1 rnL of methylene chloride
to the top. Place the K-D apparatus on a hot
water bath (60 to 65 °C) so that the concen-
trator tube is partially immersed in the hot
water, and the entire lower rounded surface
of the flask is bathed with hot vapor, Adjust
the vertical position of the apparatus and
the water temperature as required to com-
plete the concentration in 15 to 20 min. At
the proper rate of distillation the balls of the
column will actively chatter but the cham-
bers will not flood with condensed solvent.
When the apparent volume of liquid reaches
1 rnL, remove the K-D apparatus and allow it
to drain and cool for at least 10 min.
10.8 Momentarily remove the Snyder col-
umn, add 50 mL of hexane and a aew boiling
chip, and reattaeh the Snyder column. Raise
the temperature of the water bath to 85 to
90°C. Concentrate the extract as in Section
10.7, except use hexane to prewet the column.
Remove the Snyder column and rinse the
flask and its lower joint into the concen-
trator tube with 1 to 2 mL of hexane. A 5-rnL
syringe is recommended for this operation.
Set aside the K-D glassware for reuse in Sec-
tion 10.14.
10.9 Pour the hexane extract from the
concentrator tube into a 125-mL separatory
funnel. Rinse the concentrator tube four
times with 10-mL aliquots of hexane. Com-
bine all rinses in the 125-mL separatory fun-
nel.
10.10 Add 50 mL of sodium hydroxide solu-
tion to the funnel and shake for 30 to 60 s.
Discard the aqueous phase.
10.11 Perform a second wash of the or-
ganic layer with 50 mL of reagent water. Dis-
card the aqueous phase.
10,12 Wash the aexane layer with a least
two 50-mL aliquots of concentrated sulfuric
acid. Continue washing the hexane layer
with 50-mL aliquots of concentrated sulfuric
acid until the acid layer remains colorless.
Discard all acid fractions.
10.13 Wash the hexane layer with two 50-
mL aliquots of reagent water. Discard the
aqueous phases.
10.14 Transfer the hexane extract into a
125-mL Erlenmeyer flask containing 1 to 2 g
of anhydrous sodium sulfate. Swirl the flask
for 30 s and decant the hexane extract into
the reassembled K-D apparatus. Complete
the quantitative transfer with two 10-mL
hexane rinses of the Brlenmeyer flask.
10.15 Replace the one or two clean boiling
chips and concentrate the extract to 6 to 10
mL as in Section 10.8.
10.16 Add a clean boiling chip to the con-
centrator tube and attach a two-ball micro-
Snyder column. Prewet the column by add-
ing about 1 mL of hexane to the top. Place
the micro-K-D apparatus on the water bath
so that the concentrator tube is partially
immersed in the hot water. Adjust the
vertical position of the apparatus and the
water temperature as required to complete
the concentration in 5 to 10 min. At the prop-
er rate of distillation the balls of the column
will actively chatter but the chambers will
not flood. When the apparent volume of liq-
uid reaches about 0.5 mL, remove the K-D
apparatus and allow it to drain and cool for
at least 10 rnin. Remove the micro-Snyder
column and rinse its lower joint into the
concentrator tube with 0.2 mL of hexane.
Adjust the extract volume to 1.0 rnL with
hexane. Stopper the concentrator tube and
store refrigerated and protected from light if
further processing will not be performed im-
mediately. If the extract will be stored
192
-------
Environmental Protection Agency
Pt. 136, App, A.Meth. 613
longer than two days, it should be trans-
ferred to a Teflon-sealed screw-cap vial. If
the sample extract requires no further clean-
up, proceed with GC/MS analysis (Section
12), If the sample requires further cleanup,
proceed to Section 11.
10.1" Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
inL graduated cylinder. Record the sample
volume to the nearest 5 niL.
]1, Cleanup and Separation
11.1 Cleanup procedures may not be nec-
essary for a relatively clean sample matrix.
If particular circumstances demand the use
of a cleanup procedure, the analyst may use
either procedure below or any other appro-
priate procedure.'-v-7 However, the analyst
first must demonstrate that the require-
ments of Section 8.2 can be met using the
method as revised to incorporate the cleanup
procedure. Two cleanup column options are
offered to the analyst in this section. The
alumina column should be used first to over-
come interferences. If background problems
are still encountered, the silica gel column
may be helpful.
11.2 Alumina column cleanup for 2.3,7,8-
TCDD:
11.2.1 Fill a 300 mm long x 10 mm ID
chromatographic column with activated alu-
mina to the 150 mm level. Tap the column
gently to settle the alumina and add 10 mm
of anhydrous sodium sulfate to the top.
11.2.2 Preeiute the column with 50 rnL of
hexane. Adjust the elution rate to 1 mL»min.
Discard the eluate and just prior to exposure
of the sodium sulfate layer to the air, quan-
titatively transfer the 1.0-mL sample extract
onto the column using two 2-mL portions of
hexane to complete the transfer.
11-2.3 Just prior to exposure of the sodium
sulfate layer to the air, add 50 mL> of 3%
methylene chloride'95% hexane (V'V) and
continue the elution of the column. Discard
the elxiate,
11.2.4 Next, elui-e the column with 50 mL
of 20% methylene chloride'80% hexane cV/V)
into a 500-mL K-D flask equipped with a 10-
rnL concentrator tube. Concentrate the col-
lected fraction to 1.0 mL as in Section 10.16
and analyze by GC/MS (Section 12).
11.3 Silica gel column cleanup for 2.3,7.8-
TCDD:
11.3.1 Fill a 400 mm long x 11 mm ID
chroma tmgraphic column with silica gel to
the 300 mm level. Tap the column g-ently to
settle the silica gel and add 10 mm of anhy-
drous sodium sulfate to the top.
11.3.2 Preeiute the column with 50 rnL of
20% benzene/80% hexane (V/V). Adjust, the
elution rate to 1 mL/min. Discard the eluate
and just prior to exposure of the sodium sui-
fate layer to the air. quantitatively transfer
the 1.0-mL sample extract onto the column
using two 2-mL portions of 20% benzene/80%
hexane to complete the transfer.
11.3.3 Just prior to exposure of the sodium
sulfate layer to the air, add 40 rnL of 20%
benzene/80% hexane to the column. Collect
the eluate in a clean 500-mL K-D flask
equipped with a 10-mL concentrator tube.
Concentrate the collected fraction to 1.0 mL
as in Section 10.16 and analyze by GC/MS,
12. GC/MS Analysis
12.1 Table 1 summarizes the recommended
operating conditions for the gas cb.ro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. Other capillary col-
umns or chromatographic conditions may be
used if the requirements of Sections 5.5.2 and
8.2 are met.
12.2 Analyze standards and samples with
the mass spectrometer operating in the se-
lected ion monitoring (SIMi mode using a
dwell time to give at least seven points per
peak. For LRMS, use masses at m/z 320, 322,
and 25? for 2.3.7,8-TCDD and either nvz 328
for <7C14 2,3,7,8-TCDD or m/z 332 for "Cu
2.3.7.8-TCDD. For HRMS, use masses at m'z
319.8965 and 321.8936 for 2,3.7,8~TCDD and ei-
ther m/z 327,8847 for -"CU 2,3.7.8-TCDD or m-
z 331.9367 for );C,^ 2,3,7,8-TCDD.
12,3 If lower detection limits are required.
the extract may be carefully evaporated to
dryness under a gentle stream of nitrogen
with the concentrator tube in a water bath
at about 40 0. Conduct this operation imme-
diately before GC/MS analysis. Redissolve
the extract in the desired final volume of
ortho-xylene or tetradecane.
12.4 Calibrate the system daily as de-
scribed in Section 7.
12.5 Inject 2 to 5 uL of the sample extract
into the gas chrematograph. The volume of
calibration standard injected must be meas-
ured, or be the same as all sample Injection
volumes.
12.6 The presence of 2.3.7.8--TCDD is quali-
tatively confirmed if all of the following' cri-
teria are achieved:
12.6.1 The gas ehroniatoiiTaphic column
must resolve 2.3.7.8-TCDD from the other 21
TCDD isomcrs-
12.6.2 ThH masses for native 2.3.7.8-TCDD
i.LRMS-m'z 320. 322. and 2.r>7 and HRMS-m-z
320 and 322> and labeled 2.3,7.8-TCDD (m z 328
or 332) must exhibit a simultaneous max-
imum at, a retention time that matches that
of native 2.3.7,8-TCDD in the calibration
standard, with the performance specifica-
tions of the analytical system.
12.8.3 The chlorine isotope ratio at m-z 320
and m/z 322 must agree to within±10% of that
in the calibration standard.
12.6.4 The signal of all peaks must be
greater than 2.5 times the noise level.
12.7 For quantitation. measure the re-
sponse of the mz 320 peak for 2.3.7.ft-TCDD
193
-------
Pt. 136, App. A, Meth. 613
40 CFR Ch. 1 (7-1-04 Edition)
and the m/z 332 peak for 13C,2 2,3,7,8-TCDD or
the m/z 328 peak for -«CLi 2,3,7,8-TCDD.
12,8 Co-eluting impurities are suspected if
all criteria are achieved except those in Sec-
tion 12,6,3, In this case, another SIM analysis
using masses at m/z 257, 259, 320 and either rn/
a 328 or m/z 322 can be performed. The masses
at m/z 257 and m/z 259 are indicative of the
loss of one chlorine and one carboiiyl group
from 2,3,7,8-TCDD. If masses m/z 257 and m/z
259 give a chlorine isotope ratio that agrees
to within ±10% of the same cluster in the
calibration standards, then the presence of
TCDD can be confirmed. Co-eluting- DDD,
DDE, and PCB residues can be confirmed,
but will require another injection using the
appropriate SIM masses or full repetitive
mass scans. If the response for 37C14 2,3,7,8--
TCDD at m/z 328 is too large, PCB contami-
nation is suspected and can be confirmed by
examining the response at both m/z 326 arid
m/z 328. The ;17C14 2,3,7,8-TCDD internal
standard gives negligible response at m/z 326.
These pesticide residues can be removed
using the alumina column cleanup proce-
dure.
12.9 If broad background interference re-
stricts the sensitivity of the QC/MS analysis,
the analyst should employ additional clean-
up procedures and reanalyze by GC/'MS.
12.10 In those circumstances where these
procedures do not yield a definitive conclu-
sion, the use of high resolution mass spec-
troinetry is suggested.5
13. Calculations
13.1 Calculate the concentration of 2,3,7,8-
TCDD in the sample using the response fac-
tor (BF) determined in Section 7.1.2 and
Equation 2.
(A)(Vt)
Concentration (jig/L) = 7—
Equation 2
where:
A»=SIM response for 2,3,7,8~TCDD at m/z 320.
Ais=SIM response for the internal standard at
m/z 328 or 332.
L.=Amount of internal standard added to
each extract (|ig-).
V,,=Volume of water extracted (L).
13.2 For each sample, calculate the per-
cent recovery of the internal standard by
comparing the area of the m/z peak measured
in the sample to the area of the same peak
in the calibration standard. If the recovery is
below 50%, the analyst should review all as-
pects of his analytical technique.
13,3 Report results in ug/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.' The MDL concentration listed in Table
1 was obtained using reagent water.14 The
MDL actually achieved in a given analysis
will vary depending on instrument sensi-
tivity and matrix effects.
14.2 This method was tested by 11 labora-
tories using reagent water, drinking water,
surface water, and three industrial waste-
waters spiked at six concentrations over the
range 0,02 to 0,20 ng-'L,15 Single operator pre-
cision, overall precision, and method accu-
racy were found to be directly related to the
concentration of the parameter and essen-
tially independent of the sample matrix.
Linear equations to describe these relation-
ships are presented in Table 3.
REFERENCES
1. 40 CPR part 136, appendix B.
2. "Determination of TCDD in Industrial
and Municipal Wastewaters," EPA 600/4-82-
028, National Technical Information Service,
PB82-196882, Springfield, Virginia 22161, April
1982.
3, Buser. H.B., and Bappe, C, "High Resolu-
tion Gas Chromatography of the 22
Tetrachlorodibenzo-p-dioxin Isomers," Ana-
lytical Chemistry, 52, 2257 (1980),
4. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
5, Harless, R. L., Oswald. E. O., and
Wilkinson. M. K. "Sample Preparation and
Gas ChroniatogTaphy/Mass Spectronietry De-
termination of 2,3.7,8-Tetrachlorodibenzo-p-
dioxin," Analytical Chemistry, 52, 1239 (1980),
6. Laniparski, L. L,, and Nestrick, T. J.
"Determination of Tetra-, Hepta-, and
Octachlorodibenzo-p-dioxin Isomers in Par-
ticulate Samples at Parts per Trillion Lev-
els," Analytical Chemistry, 52, 2045 (1980).
7. Longhorst, M. L., and Shadoff, L. A.
"Determination of Parts-per-Trillion Con-
centrations of Tetra-, Hexa-, and Octachloro-
dibenzo-p-dioxins in Human Milk," Analytical
Chemistry, 52, 2037 (1980).
8. "Carcinogens—Working with Carcino-
gens," Department of Health, Education, aad
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
9. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910),
Occuptional Safety and Health Administra-
tion, OSHA 2206 (.Revised, January 1976).
194
-------
Environmental Protection Agency
Pt. 136, App, A, Meth. 624
10, "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
11. Provost, L. P., and Elder, B. S., "In-
terpretation of Percent Recovery Data,"
American Laboratory, 15, 58-63 (1983). (The
value 2.44 used in the equation in Section
8.3.3 is two times the value 1.22 derived in
this report.)
12. ASTM Annual Book of Standards, Part
31, D3370-76, "Standard Practices for Sam-
pling' Water," American Society for Testing'
and Materials, Philadelphia.
13, "Methods, 330.4 (Titrimetrie, DPD-FAS)
and 330.5 (Spectrophotometric DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79--02Q, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory. Cincinnati, Ohio
45268, March 1979.
14. Wong, A.S, et al. "The Determination of
2.3,7,8-TGDD in Industrial and Municipal
Waste-waters, Method 613, Part l^Develop-
ment and Detection Limits," G. Choudhay, L.
Keith, and C. Ruppe, ed., Butterworth Inc.,
(1983).
15. "EPA Method Study 26, Method 613:
2,3,7, 8-Tetraehlorodiben.20-p-dio.xm," EPA
600/4-84-037, National Technical Information
Service, PB84-188879, Spring-field, Virginia
22161, May 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMIT
Parameter
Retention
time (rnin)
2,3,7,8-TCDD ...
13.1
Method
detection
limit (jig/
L)
0.002
Column conditions: SP-2330 coated an a 60 m Song x 0.25
rnm ID glass column with hydrogen carrier gas at 40 cm/sec
linear velocity, splitless injection using tetradecane. Column
temperature heid isothermal at 200-C for 1 rnin, then pro-
grammed at 8cC/min to 250 :'C and heid. Use of helium car-
rier gas will approximately double the retention time.
TABLE 2—QC ACCEPTANCE CRITERIA—METHOD
613
s=Standard deviation of four recovery measurements, in ug/
L (.Section 8.2.4).
X^Average recovery for four recovery measurements, in ug/
L (Section 8.2.4).
P, P,=Peroent recovery measured (Section 8.3.2, Section
8.4.2).
NOTE: These criteria are based directly upon the method
performance data in Table 3. Where necessary, the limits for
recovery have been broadened to assure applicability of the
limits to concentrations below those used to develop Table 3.
TABLE 3—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 613
Overall precision,
S' (uA)/L)
Parameter
Accuracy, as recov-
ery. X 'fog/I)
Single analyst, pre-
cision, $r (U/L)
2,3,7,8-TCDD
0.86C+0.00145
0.13X-0.00129 I
0 19X+0.00028
X'=Expected recovery for one or more measurements, of a sample containing a concentration of C, in ng/L.
s/=Expected single analyst standard deviation of measurements a! an average concentration found of X, in |Kj/L,
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X. in ug/L,
C=True value for the concentration, in ug/L.
X=Average recovery found for measurements of samples containing a concentration of C, in U.Q/L,
METHOD 624—PURGEABLES
1. Scope and Application
1.1 This method covers the determination
of a number of purgeable orgranies. The fol-
lowing parameters may be determined by
this method:
Parameter
Benzene
Bromodichloromethane
Bromoform
Brornomethane
Carbon tetrachloride
Chlorobenzene
Chloroethan©
2-Chloroethylvinyl elher
Chloroform
Chloromethane
Dibromochloromethane
1 ,2-Dichlorobenzene
STORET
No.
34030
32101
32104
34413
32102
34301
34311
34576
32106
34418
32105
34536
CAS No.
71-43-2
75-27-4
75-25-2
74-83-9
56-23-5
108-90-7
75-00-3
110-75-8
67-66-3
74-87^
124-48-1
95-50-1
Parameter
1,3-Dichlorobenzene
1 ,4-Dichlorobenzene
1,1-Dichloroethane
1 ,2-Dichloroethane
1,1-Dichloroethane
trans-1 ,2-Dichloroefhene
1 2-Dichioropropane
cis~1 ,3-Dichloropropene
trans-1 ,3-Dichloropropene
Ethyl benzene
Methylene chloride
1,1.2,2-Tetrachloroethane
Fefrachloroethene
Toluene
1,1,1-Trichloroelhene
1,1,2-Trichioroethene ,
Trichloroethane .,
Triehlorofluoromethane
Vinyl chloride .-
STORET
No.
34566
34S71
34496
34531
34501
34548
34541
34704
34699
34371
34423
34516
34475
34010
34506
34511
39180
34488
39175
CAS No.
541-73-1
106-46-7
75-34-3
107-06-2
75-35-4
156-60-5
78-87-5
10061-01-5
10061-02-6
100-41-4
75-09-2
79-34-5
127~18-»
1 08-88-3
71-55-6
79-00-5
79-01-6
75-63^>
75-01-4
195
-------
Pt. 136, App. A, Meth. 624
40 CFR Ch. I (7-1-04 Edition)
1,2 The method may be extended to screen
samples for acroleln (STORET No. 34210. CAS
No. 107-03-8) and acrylonitrile (STORET No,
34215, CAS No. 107-1J-11. however, the pre-
ferred method for these two compounds in
Method 603.
1.3 This is a purge and trap gas chromato-
graphic/mass spectrometer (GO/MS) method
applicable to the determination of the com-
pounds listed above in municipal and indus-
trial discharges as provided under 40 CFE
136.1.
1.4 The method detection limit CMDL, de-
fined in Section 14.1)1 for each parameter is
listed in Table 1. The MDL for a specific
waste-water may differ from those listed, de-
pending upon the nature of interferences in
the sample matrix.
1.5 Any modification to this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5. De-
pending upon the nature of the modification
and the extent of intended use, the applicant
may be required to demonstrate that the
modifications will produce equivalent results
when applied to relevant wastewaters.
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the operation of a purge and trap
system and a gas chromatograph/mass spec-
trometer and in the interpretation of mass
spectra. Bach analyst must demonstrate the
ability to generate acceptable results with
this method using the procedure described in
Section 8.2.
2. Summary of Method
2.1 An inert gas is bubbled through a 5-mL
water sample contained in a specially-de-
signed purging chamber at ambient tempera-
ture. The purgeables are efficiently trans-
ferred from the aqueous phase to the vapor
phase. The vapor is swept through a sorbent
trap where the purgeables are trapped. After
purging is completed, the trap is heated and
backflushed with the inert gas to desorb the
purgeables onto a gas chromatographic col-
umn. The gas chromatograph is temperature
programmed to separate the purgeables
which are then detected with a mass spec-
trometer.2--
3. Interferences
3.1 Impurities in the purge gas, organic
compounds outgassing from the plumbing
ahead of the trap, and solvent vapors in the
laboratory account for the majority of con-
tamination problems. The analytical system
must be demonstated to be free from con-
tamination under the conditions of the anal-
ysis by running laboratory reagent blanks as
described in Section 8.1.3. The use of non-
Teflon plastic tubing, non-Teflon thread
sealants, or flow controllers with rubber
components in the purge and trap system
should be avoided.
3.2 Samples can be contaminated by diffu-
sion of volatile organics (particularly fluoro-
carbons and methylene chloride) through the
septum seal into the sample during shipment
and storage. A field reagent blank prepared
from reagent water and carried through the
sampling and handling protocol can serve as
a check on such contamination.
3.3 Contamination by carry-over can
occur whenever high level and low level sam-
ples are sequentially analyzed. To reduce
carry-over, the purging device and sample
syringe must be rinsed with reagent water
between sample analyses. Whenever an un-
usually concentrated sample is encountered,
it should be followed by an analysis of rea-
gent water to check for cross contamination.
For samples containing large amounts of
water-soluble materials, suspended solids,
high boiling compounds or high pureeable
levels, it may be necessary to wash the purg-
ing device with a detergent solution, rinse it
with distilled water, and then dry it in a 105
°C oven between analyses. The trap and
other parts of the system are also subject to
contamination; therefore, frequent bakeout
and purging of the entire system may be re-
quired.
4. Safety
4.1 The toxicity or carcinogenicity of
each reagent used in this method has not
been precisely defined; however, each chem-
ical compound should be- treated as a poten-
tial health hazard. From this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this
methmd. A reference file of material data
handling sheets should also be made avail-
able to all personnel involved in the chem-
ical analysis. Additional references to lab-
oratory safety are available and have been
identified4 6 for the information of the ana-
lyst.
4.2. The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens; benzene, carbon tetra-
ehloride, chloroform, 1,4-dlchlorobenzene.
and vinyl chloride. Primary standards of
these toxic compounds should be prepared in
a hood. A NIOSHMESA approved toxic gas
respirator should be worn when the analyst
handles high concentrations of these toxic
compounds,
5. Apparatus and Materials
5.1 Sampling' equipment, for discrete sam-
pling.
196
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Environmental Protection Agency
Pt. 136, App. A, Meth. 624
5,1.1 Vial—25-mL capacity or larger,
equipped with a screw cap with a hole in the
center (Pierce #13075 or equivalent). Deter-
gent wash, rinse with tap and distilled water,
and dry at 105 °C before use.
5,1.2 Septum—Teflon-faced silieane
(Pierce #12722 or equivalent). Detergent
wash, rinse with tap and distilled water, and
dry at 105 °C for 1 h before use.
5,2 Purge and trap system—The purge and
trap system consists of three separate pieces
of equipment: A purging device, trap, and
deserter. Several complete systems are now
commercially available.
5.2.1 The purging device must be designed
to accept 5-mL samples with a water column
at least 3 cm deep. The gaseous head space
between the water column and the trap must
have a total volume of less than 15 mL. The
purge gas must pass though the water col-
umn as finely divided bubbles with a diame-
ter of less than 3 mm at the origin. The
purge gas must be introduced no more than
5 mm from the base of the water column.
The purging device illustrated in Figure 1
meets these design criteria.
5.2.2 The trap must be at least 25 cm long
and have an Inside diameter of at least 0.105
in. The trap must be packed to contain the
following minimum lengths of adsorbents; 1.0
cm of methyl silicone coated packing (Sec-
tion 6.3.2), 15 cm of 2,6-dyphenylene oxide
polymer (Section 8.3.1), and 8 cm of silica gel
(Section 6.3.3). The minimum specifications
for the trap are illustrated in Figure 2.
5.2.3 The desorber should be capable of
rapidly heating the trap to 180 °C. The poly-
mer section of the trap should not be heated
higher than 180 °C and the remaining sec-
tions should not exceed 200 CC. The desorber
illustrated in Figure 2 meets these design
criteria.
5.2.4 The purge and trap system may be
assembled as a separate unit or be coupled to
a gas chromatograph as illustrated in Fig-
ures 3 and 4.
5.3 GC/MS system:
5.3.1 Gas chromatograph—An analytical
system complete with a temperature pro-
g'rammable gas chromatograph suitable for
on-column injection and all required acces-
sories including syringes, analytical col-
umns, and gases.
5.3.2 Column—6 ft long x 0.1 in ID stain-
less steel or glass, packed with 1% SP-1000
on Carbopack B (60/80 mesh) or equivalent.
This column was used to develop the method
performance statements in Section 14.
Guidelines for the use of alternate column
packing's are provided in Section 11.1.
5.3.3 Mass spectrometer—Capable of scan-
ning1 from 20 to 260 amu every 7 ? or less, uti-
lizing 70 V (nominal) eleooron energy in the
electron impact ionization mode, a,nd pro-
ducing" a mass spectrum which meets all the
criteria in Table 2 when Song oi 4-bromofluo-
robenzene (BFB'i is injected through the GC
inlet.
5,3.4 GC/MS interface^Any GC to MS
interface that gives acceptable calibration
points at 50 ng or less per injection for each
of the parameters of interest and achieves all
acceptable performance criteria (Section 10)
may be used. GC to MS interfaces con-
structed of all glass or glass-lined materials
are recommended. Glass can be deactivated
by silanizing with dichlorodlmethylsilane.
5.3.5 Data system—A computer system
must be interfaced to the mass spectrometer
that allows the continuous acquisition and
storage on machine-readable media of all
mass spectra obtained throughout the dura-
tion of the chromatographic program. The
computer must have software that allows
searching any GC/MS data file for specific ml
z (masses) and plotting such m/z abundances
versus time or scan number. This type of
plot is defined as an Extracted Ion Current
Profile (BICP), Software must also be avail-
able that allows integrating the abundance
in any EICP between specified time or scan
number limits.
5.4 Syringes—S-rnL, glass hypodermic
with Luerlok tip (two each), if applicable to
the purging device.
5.5 Micro syringes—25-nL, 0,006 In. ID nee-
dle.
5.6 Syringe valve—2-way, with Luer ends
(three each).
5.7 Syringe—5-mli, gas-tight with shut-off
valve.
5.8 Bottle—15-mL, screw-cap, with Teflon
cap liner.
5.9 Balance—Analytical, capable of accu-
rately weighing 0.0001 g.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.1.1 Reagent water can be generated by
passing tap water through a carbon filter bed
containing about 1 Ib of activated carbon
(Filtrasorb-300, Calgon Corp., or equivalent).
6.1.2 A water purification system
(Millipore Super-Q or equivalent) may be
used to generate reagent water.
6.1.3 Beagent water may also be prepared
by boiling water for 15 min. Subsequently,
while maintaining the temperature at 90 °C,
bubble a contaminant-free inert gas through
the water for 1 h. While still hot, transfer
the water to a narrow mouth screw-cap bot-
tle and seal with a Teflon-lined septum and
cap.
6.2 Sodium thiosnlfate—(ACS) Granular.
6.3 Trap material":
6.3.1 2.6-Dipher.,vlpne oxide polymer--
Tenax. (60/80 mesh), chromatographic, grade
or equivalent
6.3,2 Methyl siliuone packing- 3% OV--1 on
Chromosorb-W (60'80 mesh; or eqaiva'enl.
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40 CFR Ch. I (7-1-04 Edition)
6.3,3 Silica gel—35/60 mesh, Davison,
grade-15 or equivalent.
6,4 Methanol—Pesticide quality or equiv-
alent.
6,5 Stock standard solutions—Stock
standard solutions may be prepared from
pure standard materials or purchased as
certified solutions. Prepare stock standard
solutions in methanol using assayed liquids
or gases as appropriate. Because of the tox-
icity of some of the compounds, primary di-
lutions of these materials should be prepared
in a hood. A NIOSH/MESA approved toxic
gas respirator should toe used when the ana-
lyst handles high concentrations of such ma-
terials.
6.5.1 Place about 9.8 mL of methanol into
a 10-mL ground glass stoppered volumetric
flask. Allow the flask to stand, unstoppered,
for about 10 min or until all alcohol wetted
surfaces have dried. Weigh the flask to the
nearest 0.1 mg.
6.5.2 Add the assayed reference material:
6.5.2.1 Liquids—Using a 10Q-(iL syringe,
immediately add two or more drops of as-
sayed reference material to the flask, then
reweigh. Be sure that the drops fall directly
into the alcohol without contacting the neck
of the flask,
6.5.2.2 Gases—To prepare standards for
any of the four halocarbons that boil below
30 °C (bromomethane, chloroethane,
chloromethane, and vinyl chloride), fill a 5-
mL valved gas-tight syringe with the ref-
erence standard to the 5,0-mL mark. Lower
the needle to 5 mm above the methanol me-
niscus. Slowly introduce the reference stand-
ard above the surface of the liquid (the heavy
gas will rapidly dissolve in the methanol).
6.5.3 Reweigh, dilute to volume, stopper,
then mix by inverting the flask several
times. Calculate the concentration in (ig/^L
from the net gain in weight. When compound
purity is assayed to be 96% or greater, the
weight may be used without correction to
calculate the concentration of the stock
standard. Commercially prepared stock
standards may be used at any concentration
if they are certified toy the manufacturer or
by an independent source.
6.5.4 Transfer the stock standard solution
into a Teflon-sealed screw-cap bottle. Store,
with minimal headspace, at -10 to -20 °C
and protect from light.
6.5.5 Prepare fresh standards weekly for
the four gases and 2-chloroethylvinyl ether.
All other standards must be replaced after
one month, or sooner if comparison with
check standards indicates a problem.
6.6 Secondary dilution standards—Using
stock solutions, prepare secondary dilution
standards in methanol that contain the com-
pounds of interest, either singly or mixed to-
gether. The secondary dilution standards
should "be prepared at concentrations such
that the aqueous calibration standards pre-
pared in Section 7.3 will bracket the working
range of the analytical system. Secondary
dilution standards should be stored with
minimal headspace and should be checked
frequently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7 Surrogate standard spiking solution—
Select a minimum of three surrogate com-
pounds from Table 3. Prepare stock standard
solutions for each surrogate standard in
methanol as described in Section 6.5. Prepare
a surrogate standard spiking solution from
these stock standards at a concentration of
15 jig/mL in water. Store the solutions at t "C
in Teflon-sealed glass containers with a min-
imum of headspace. The solutions should be
checked frequently for stability. The addi-
tion of 10 jiL of this solution of 5 mL of sam-
ple or standard is equivalent to a concentra-
tion of 30 jig/L of each surrogate standard.
6,8 BPB Standard—Prepare a 25 jig/mL so-
lution of BFB in methanol.
6.9 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Assemble a purge and trap system that
meets the specifications in Section 5.2. Con-
dition the trap overnight at 180 °C by
backflushing with an inert gas flow of at
least 20 rnL/min. Condition the trap for 10
min once daily prior to use,
7.2 Connect the purge and trap system to
a gas chromatograph. The gas chro-
matograph must be operated using tempera-
ture and flow rate conditions equivalent to
those given in Table 1.
7.3 Internal standard calibration proce-
dure—To use this approach, the analyst must
select three or more internal standards that
are similar in analytical behavior to the
compounds of interest. The analyst must fur-
ther demonstrate that the measurement of
the internal standard is not affected by
method or matrix interferences. Some rec-
ommended internal standards are listed in
Table 3.
7.3,1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter by carefully adding 20.0 uL of
one or more secondary dilution standards to
50, 250, or 500 mL of reagent water, A 2o-uL
syringe with a 0,006 in. ID needle should be
used for this operation. One of the calibra-
tion standards should be at a concentration
near, but above, the MDL (Table 1) and the
other concentrations should correspond to
the expected range of concentrations found
in real samples or should define the working
range of the GO/MS system. These aqueous
standards can be stored up to 24 h, if held in
sealed vials with zero headspace as described
in Section 9.2. If not so stored, they must be
discarded after 1 h.
7.3,2 Prepare a spiking solution con-
taining each of the internal standards using
the procedures described in Sections 6.5 and
198
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Environmental Protection Agency
Pt, 136, App. A, Meth. 624
6.6. It is recommended that the secondary di-
lution standard be prepared at a concentra-
tion of 15 |ig/mL of each internal standard
compound. The addition of 10 jiL of this
standard to 5.0 niL of sample or calibration
standard would be equivalent to 30 (ig/L.
7.3.3 Analyze each calibration standard
according to Section 11. adding 10 (4.L of in-
ternal standard spiking solution directly to
the syringe (Section 11.4). Tabulate the area
response of the characteristic m/z against
concentration for each compound and inter-
nal standard, and calculate response factors
(RP) for each compound using Equation 1.
RF =
(AS)(C.S)
(A,)(CS)
Equation 1
where:
A ,=Area of the characteristic m/z for the pa-
rameter to be measured,
Als=Area of the characteristic m/z for the
Inernal standard.
els=Concentration of the internal standard.
("^Concentration of the parameter to be
measured.
If the RF value over the working range is a
constant (<35% RSD), the RP can be assumed
to be invariant and the average RF can be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, A JA^, vs. RF.
7.4 The working calibration curve or RF
must be verified on each working day by the
measurement of a QC check sample.
7.4.1 Prepare the QC check sample as de-
scribed in Section 8.2.2.
7.4.2 Analyze the QC check sample accord-
ing to the method beginning in Section 10.
7.4.3 For each parameter, compare the re-
sponse (Q) with the corresponding" calibra-
tion acceptance criteria found in Table 5. If
the responses for all parameters of interest
fall within the designated ranges, analysis of
actual samples can begin. If any individual Q
falls outside the range, proceed according to
Section 7.4.4.
NOTE: The large number of parameters in
Table 5 present a substantial probability
that one or more will not meet the calibra-
tion acceptance criteria when all parameters
are analyzed.
7.4.4 Repeat the test only for those pa-
rameters that failed to meet the calibration
acceptance criteria. If the response for a pa-
rameter does not fall within the range In
this second test, a new calibration curve or
RF must be prepared for that parameter ac-
cording1 to Section 7.3.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes Indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation.
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method, This ability is established
as described in Section 8,2.
8.1.2 In recognition of advances that are
occurring in ehromatography, the analyst is
permitted certain options (detailed in Sec-
tion 11.1) to improve the separations or lower
the cost of measurements. Each time such a
modification is made to the method, the ana-
lyst is required to repeat the procedure in
Section 8.2.
8.1.3 Bach day. the analyst must analyze a
reagent water blank to demonstrate that
interferences from the analytical system are
under control.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 5% of
all samples to monitor and evaluate labora-
tory data quality. This procedure is de-
scribed in Section 8,3.
8.1,5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 5% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8,1.6 The laboratory must spike all sam-
ples with surrogate standards to monitor
continuing laboratory performance. This
procedure is described in Section 8,5.
8.1.7 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.6.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QG) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 10
(ig/mlj in methanol. The QC check sample
concentrate must be obtained from the U.S.
Environmental Protection Agency. Environ-
mental Monitoring and Support Laboratory
in Cincinnati, Ohio, if available. If not avail-
able from that source, the QC check sample
199
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Pt. 136, App. A, Meth. 624
40 CFR Ch. I (7-1-04 Edition)
concentrate must be obtained from another
external source. If not available from either
source above, the QC check sample con-
centrate must be prepared by the laboratory
using stock standards prepared independ-
ently from those used for calibration,
8.2,2 Prepare a QC check sample to con-
tain 20 ug/I_i of each parameter by adding 200
(iL of QC check sample concentrate to 100 mL
of reagent water.
8.2.3 Analyze four 5-rnL aliqnots of the
well-mixed QC check sample according to
the method beginning in Section 10.
8.2.4 Calculate the average recovery (X) in
ug/L, and the standard deviation of the re-
covery (s) in )Lgfii, for each parameter of in-
terest using the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively,
found in Table 5. If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Table 5 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8,2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.3.
8.2.6.2 Beginning with Section 8.2.3, repeat
the test only for those parameters that
failed to meet criteria. Bepeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2,3.
8.3 The laboratory must, on an ongoing
basis, spike at least 5% of the samples from
each sample site being monitored to assess
accuracy. For laboratories analyzing 1 to 20
samples per month, at least one spiked sam-
ple per month is required.
8.3.1 The concentration of the spike in the
sample should be determined as follows:
8.3.1.1 If, as in compliance monitoring,
the concentration of a specific parameter in
the sample is being checked against a regu-
latory concentration limit, the spike should
be at- that limit or 1 to 5 times higher than
the background concentration determined in
Section 8,3,2, wtiiebevw- concentration would
be larger.
83,1,2 If the coi^.en* ration of a specific
parameter in the Cample is not being
checked against a limit specific to that pa-
rameter, the spike should be at 20 (ig/L or 1
to 5 times higher than the background con-
centration determined in Section 8.3.2,
whichever concentration would be larger.
8.3.2 Analyze one 5-mL, sample aliquot to
determine the background concentration (B)
of each parameter. If necessary, prepare a
new QC check sample concentrate (Section
8.2.1) appropriate for the background con-
centrations in the sample. Spike a second 5-
mL sample aliquot with 10 uL of the QC
check sample concentrate and analyze it to
determine the concentration after spiking
(A) of each parameter. Calculate each per-
cent recovery (P) as 100(A-B)%/T, where T is
the known true value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 5. These
acceptance criteria wer calculated to include
an allowance for error in measurement of
both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will be accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1.7 If spiking was
performed at a concentration lower than 20
ug/L, the analyst must use either the QC ac-
ceptance criteria in Table 5, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recoveryof
a parameter: (1) Calculate accuracy (X')
using the equation in Table 6, substituting
the spike concentration (T) for C: (2) cal-
culate overall precision (S') using the equa-
tion in Table 6, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X'/T) (±2.44(100 S'/T)%.7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described In Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed,
NOTE: The frequency for the required
anlaysis of a QC check standard will depend
upon the number of parameters being simul-
taneously tested, the complexity of the sam-
ple matrix, and the performance of the lab-
oratory. If the entire list of parameters in
Table 5 must be measured in the sample in
Section 8.3, the probability that the analysis
of a QC check standard will be required is
high. In this case the QC check standard
should be routinely analyzed with the spiked
sample.
8,4.1 Prepare Hit QC cbfct.k standard by
adding 10 jiL of QO check sample concentrate
iSec-lion 8,2.) or 8.C.21 to 5 ml., of teagent
water. The QC che<;k standard neeue only to
200
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Environmental Protection Agency
Pt. 136, App. A, Meth. 624
contain the parameters that failed criteria
in the test In Section 8,3.
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A.T)%, where T is the true
value of the standard concentration.
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 5. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As a quality control check, the labora-
tory must spike all samples with the surro-
gate standard spiking solutions as described
in Section 11.4, and calculate the percent re-
covery of each surrogate compound.
8.6 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent recovery interval from P—2sp to
P + 2s,,, If P=90% and sp=10%, for example.
the accuracy interval is expressed as 70-
110%. Update the accuracy assessment for
each parameter a regular basis (e.g. after
each five to ten new accuracy measure-
ments).
8,7 It is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. Whenever possible,
the laboratory should analyze standard ref-
erence materials and participate in relevant
performance evaluation studies.
9.1 All samples must be iced or refrig-
erated from the time of collection until anal-
ysis. If the sample contains residual chlo-
rine, add sodium thiosulfate preservative (10
mg'-'4Q mL is sufficient for up to 5 ppm Cl.;) to
the empty sample bottle just prior to ship-
ping- to the sampling site. EPA Methods 330,4
and 330.5 may be used for measurement of re-
sidual chlorine.8 Field test kits are available
for this purpose.
9.2 Grab samples must be collected in
glass containers having a total volume of at
least 25 mL, Pill the sample bottle just to
overflowing in such a manner that no air
bubbles pass through the sample as the bot-
tle is being filled. Seal the bottle so that no
air bubbles are entrapped in It. If preserva-
tive has been added, shake vigorously for 1
min. Maintain the hermetic seal on the sam-
ple bottle until time of analysis.
9.3 Experimental evidence indicates that
some aromatic compounds, notably benzene.
toluene, and ethyl benzene are susceptible to
rapid biological degradation under certain
environmental conditions.3 Refrigeration
alone may not be adequate to preserve these
compounds in wastewaters for more than
seven days. For this reason, a separate sam-
ple should be collected, acidified, and ana-
lyzed when these aromatics are to be deter-
mined, Collect about 500 mL of sample in a
clean container. Adjust the pH of the sample
to about 2 by adding 1+1 HC1 while stirring
vigorously, Check pH with narrow range (1.4
to 2.8) pH paper. Fill a sample container as
described in Section 9.2.
9.4 All samples must be analyzed within
14 days of collection.3
10. Daily GC.'MS Performance Tests
10.1 At the beginning- of each day that
analyses are to be performed, the GC.'MS sys-
tem must be checked to see if acceptable
performance criteria are achieved for BPB.5
The performance test must be passed before
any samples, blanks, or standards are ana-
lyzed, unless the instrument has met the
DPTPP test described in Method 625 earlier
in the day.1"
10.2 These performance tests require the
following instrumental parameters:
Electron Energy: 70 V (nominal)
Mass Range: 20 to 260 amu
Scan Time: To give at least 5 scans pet-
peak but not to exceed 7 s per scan.
10.3 At the beginning- of each day. inject 2
U.L of BFB solution directly on the column.
Alternatively, add 2 nL of BPB solution to
5.0 mL of reagent water or standard solution
and anal3rze the solution according- to sec-
tion 11. Obtain a background-corrected mass
spectrum of BFB and confirm that all the
key m/z criteria in Table 2 are achieved. If
all the criteria are not achieved, the analyst
must retune the mass spectrometer and re-
peat the test until all criteria are achieved.
11. Sample Purging and Gas Chromatography
11.1 Table 1 summarizes the recommended
operating conditions for the g-as chro-
matograph. Included in this table are reten-
tion times and MDL that can be achieved
under these conditions. An example of the
separations achieved by this column is
shown in Figure 5. Other packed columns or
chromatographic conditions may be used if
the requirements of Section 8.2 are met.
201
-------
Pt. 136, App. A, Meth. 624
40 CFR Ch. i (7-1-04 Edition)
11.2 After achieving the key m/z abun-
dance criteria in Section 10, calibrate the
system daiy as described in Section 7,
11.3 Adjust the purge gas (helium) flow
rate to 40 mL/min. Attach the trap inlet to
the purging device, and set the purge and
trap system to purge (Figure 3). Open the sy-
ringe valve located on the purging device
sample introduction needle.
11.4 Allow the sample to come to ambient
temperature prior to introducing it into the
syringe. Remove the plunger from a 5-mL sy-
ringe and attach a closed syringe valve. Open
the sample bottle (or standard) and carefully
pour the sample into the syringe barrel to
just short of overflowing. Replace the sy-
ringe plunger and compress the sample. Open
the syringe valve and vent any residual air
while adjusting the sample volume to S.O mL.
Since this process of taking an aliquot de-
stroys the validity of the sample for future
analysis, the analyst should fill a second sy-
ringe at this time to protect against possible
loss of data. Add 10.0 uL of the surrogate
splicing solution (Section 6.7) and 10.0 uL of
the internal standard spiking solution (Sec-
tion 7.3.2) through the valve bore, then close
the valve. The surrogate and internal stand-
ards may be mixed and added as a single
spiking solution.
11.5 Attach the syringe-syringe valve as-
sembly to the syringe valve on the purging
device. Open the syringe valves and inject
the sample into the purging chamber,
11.6 Close both valves and purge the sam-
ple for ll.Q±0.1 mm at ambient temperature.
11.7 After the 11-min purge time, attach
the trap to the chromatograph, adjust the
purge and trap system to the desorb mode
(Figure 4), and begin to temperature pro-
gram the gas chromatograph, Introduce the
trapped materials to the G-C column by rap-
idly heating the trap to 180 "C while
backflushing the trap with an inert gas be-
tween 20 and 60 mL/min for 4 min. If rapid
heating of the trap cannot be achieved, the
GC cloumn must he used as a secondary trap
by cooling it to 30 °C (subambient tempera-
ture, if problems persist) instead of the ini-
tial program temperature of 45 °C.
11.8 While the trap is being desorbed into
the gas chromatograph, empty the purging
chamber using the sample introduction sy-
ringe. Wash the chamber with two 5-mL
flushes of reagent water.
11.9 After desorbing the sample for 4 min,
recondition the trap by returning the purge
and trap system to the purge mode. Wait 15
s then close the syringe valve on the purging
device to begin gas flow through the trap.
The trap temperature should be maintained
at 180 °C. After approximately 7 min, turn
off the trap heater and open the syringe
valve to stop the gas flow through the trap.
When the trap Is cool, the next sample can
be analyzed.
11.10 If the response for any m/z exceeds
the working range of the system, prepare a
dilution of the sample with reagent water
from the aliquot in the second syringe and
reanalyze.
12. Qualitative Identification
12.1 Obtain EICPs for the primary m/z
(Table 4) and at least two secondary masses
for each parameter of interest. The following
criteria must be met to make a qualitative
identification:
12.1.1 The characteristic masses of each
parameter of interest must maximize in the
same or within one scan of each other.
12.1.2 The retention time must fall within
±30 s of the retention time of the authentic
compound.
12.1.3 The relative peak heights of the
three characteristic masses in the EICPs
must fall within ±20% of the relative inten-
sities of these masses in a reference mass
spectrum. The reference mass spectrum can
be obtained from a standard analyzed in the
GC/MS system or from a reference library.
12,2 Structural isomers that have very
similar mass spectra and less than 30 s dif-
ference in retention time, can be explicitly
identified only if the resolution between au-
thentic isomers in a standard mix is accept-
able. Acceptable resolution is achieved if the
baseline to valley height between the iso-
mers is less than 25% of the sum of the two
peak heights. Otherwise, structural isomers
are identified as isomeric pairs.
13. Calculations
13.1 When a parameter has been identi-
fied, the quantitation of that parameter
should be based on the integrated abundance
from the EICP of the primary characteristic
m/z given in Table 4. If the sample produces
an interference for the primary m/z, use a
secondary characteristic m/z to quantitate.
Calculate the concentration in the sample
using the response factor (RF) determined in
Section 7.3.3 and Equation 2.
Concentration (fig/L) =
(AS)(C.S)
(Ais)(RF)
Equation 2
where:
As=Area of the characteristic m/z for the pa-
rameter or surrogate standard to be meas-
ured.
Ajs=Area of the characteristic m/z for the in-
ternal standard.
C,s=Concentration of the internal standard.
13.2 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
202
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Environmental Protection Agency
14. Method Performance
14.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in
Table 1 were obtained using reagent water.11
Similar results were achieved using rep-
resentative wastewaters. The MDL actually
achieved in a given analysis will vary de-
pending on instrument sensitivity and ma-
trix effects.
14.2 This method was tested by 15 labora-
tories using reagent water, drinking water.
surface water, and industrial wastewaters
spiked at six concentrations over the range
5-600 ug'L,12Single operator precision, overall
precision, and method accuracy were found
to lie directly related to the concentration of
the parameter and essentially independent of
the sample matrix. Linear equations to de-
scribe these relationships are presented in
Table 5.
REFERENCES
1. 40 CPR part 136, appendix B.
2, Bellar, T.A., and Lichtenberg, J.J. "De-
termining Volatile Organics at MicrogTam-
per-Litre Levels by Gas Chromatography."
Journal American Water Works Association, 66,
739 (1974).
3. Bellar, T.A., and Lichtenberg. J.J.
"Semi-Automated Headspace Analysis of
Drinking Waters and Industrial Waters for
Purgeable Volatile Organic Compounds, "
Measurement of Organic Pollutants in Water
and Wastewater, C.E. Van Hall, editor,
American Society for Testing and Materials.
Philadelphia, PA. Special Technical Publica-
tion 686, 1978.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service. Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CPR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety In Academic Chemistry Labora-
tories." American Chemical Society Publica-
tion, Committee on Chemical Safety. 3rd
Edition. 1979,
7. Provost, L.P., and Elder. B..S. "Interpre-
tation of Percent Recovery Data," American
Laboratory. 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.2.3 is two
times the value 1,22 derived in this report.)
8. "Methods 330.4 (Titrimetrie, DPD-FAS)
and 330.5 (Spectrophotornetric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
Pt. 136, App. A, Meth. 624
and Support Laboratory, Cincinnati. Ohio
45268, March 1979.
9. Budde, W.L.. and Eichelberger. J.W.
"Performance Tests for the Evaluation of
Computerized Eas Chromatog'raphy'Mass
Spectrometry Equipment and Laboratories,"
EPA-600/4^80-025, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory. Cincinnati, Ohio
45268, April 1980.
10. Eichelberger. J.W.. Harris. L.E., and
Budde, W.L. "Reference Compound to Cali-
brate Ion Abundance Measurement in Gas
Chromatography—Mass Spectrometry Sys-
tems," Analytical Chemistry, 47, 995-1000 (1975).
11. "Method Detection Limit for Methods
624 and 625," Olynyk, P., Budde, W.L., and
Eichelberger. J.W. Unpublished report, May
14, 1980,
12. "EPA Method Study 29 EPA Method
624^Purgeablea," EPA 600/4-84-054, National
Technical Information Service. PB84-209915,
Springfield, Virginia 22161. June 1984.
13."Method Performance Data for Method
624," Memorandum from R. Slater and T.
Pressley, U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268. Jan-
uary 17, 1984.
TABLE 1—CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMITS
Parameter
Chloromethane
Bromomethane
Vinyl chloride
Chloroelhane
Methylene chloride
Trichloroffuoromethane
1.1-DichlofOethene
1,1-Dichioroethane
trans-1,2-Dichloroethene ...
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Carbon tetrachloride
BrGrtiodichloromethane
1,2-Dichloroproane
cis-1,3-DichIoropropene ....
Trichioroethene
Benzene
Dibromochlorornethane
1.1,2-Trichloroethane
trans-1,3~Dichioropropene .
2-ChloroethylvinSyl ether . .
Bromoform
1,1,2,2-Tetrachloroethane .
Tetrachlorosthene
Toluene
Chlorobenzene
Ethy! benzene
1,3-Dichlorobenzene
1,2-Dichlorobenzene
Retention
!irne (min)
2.3
3-1
38
4,6
6.4
8.3
9.0
10.1
10.8
11-4
12.1
13,4
13.7
14,3
15.7
15-9
16.5
17,0
17.1
172
17.2
18.6
198
22.1
22.2
23.5
24,6
26.4
33,9
35.0
Method
detection
limit (i;g/Li
nd
nd
nd
nd
2.8
nd
2.8
4 7
1.6
1.6
2.8
3.8
2.8
2,2
6.0
5.0
1 9
44
3.1
5,0
nd
nd
4,7
6,9
4.1
6.0
B.O
7.2
nd
rid
203
-------
Pt. 136, App. A, Meth. 624
40 CFR Ch. I (7-1-04 Edition)
TABLE 1 — CHROMATOGRAPHIC CONDITIONS AND
METHOD DETECTION LIMITS — Continued
TABLE 4 — CHARACTERISTIC MASSES FOR
PURGEABLE CflGANIGS
Parameter
1,4-Dichiorobenzene
35.4
nd
Column conditions: Carbopak B (60/80 mesh) coated with
1% SP-10GO packed in a 6 ft by 0.1 in. ID glass column wrth
helium carrier gas at 30 mL/rnin. flow rate, Coiumn tempera-
ture held at 45^C for 3 min,, then programmed at S^C/rmn. !o
220 C and held for 15 mm.
nd=not determined.
TABLE 2—-BFB KEY M/Z ABUNDANCE CRITERIA
Mass
50
75
95
96
174
175
m/z Abundance criteria
15 to 40% of mass 95.
30 to 60% of mass 95.
Base Peak, 100% Relative
Abundance.
5 to 9% of mass 95.
<2% of mass 174.
5 to 9% of mass 174.
>95% but <101% of mass
174.
5 to 9% of mass 1 76.
TABLE 3—SUGGESTED SURROGATE AND
INTERNAL STANDARDS
Compound
Secondary
masses
Parameter
CWoromethane
Bromomethane ,, ,,
Vinyl chloride ....................
Chloroethane
Methylene chloride
Trichlorofluoramethane
1,1-Dichloroethene
1,1 "Dichloroethane
trans-l.2-Dichl0roethene ..
Chloroform
1,2-Dichloroethane ,.
1,1,1-Trichioroethane ........
Carbon tetrachloride .........
Brornodichloro methane
1,2-Dichloropropane
trans-1,3-Dichioropropene
Trichioroethene .,
Benzene ............................
Dibromochloromethane
1.1,2-Trichioroethane
cis-1,3-Dichloropropene ....
2-Chloroethylvinyl ether ....
Brornoform
1.1,2,2-Tetrachloroethane .
Benzene d-6
4-Bromofluoroberizene
1 .2-Dichloraethane d-4
1 ,4-Difiuorobenzene
Ethylbenzene d-5
Ethyibenzene d-10
Fluorobenzene
Pentafluorobenzene
Bromochiorcmethane ,
2-Bromo-1-chloropropane .
1. 4-Dichlorobutane
i " I
.. ' 17,0 '
.. i 28.3 |
.. 1 12.1 I
.. j 19.6
.. ! 26.4 !
.. ! 26.4 1
18.4
; 23-5 i
.. ! 93
.. i 19.2. !
..] 258 j^
84
95 ! 174. 176
102 j
114
63, 88
111 \
98
96
70
168
128
77
49, 130. 51
79, 156
55 90, 92
Tetrachloroethene
Toluene
Chlorobenzene
Ethyl benzene
1 ,3-Dichlorobenzene .
1,2-DichlGFObenzene .
1,4-DichIorobenzene .
Pri-
mary j
50
94
62
64
84
101
96
63
83
98
97
117
127
112
75
130
78
127
75
106
173
168
164
92
112
106
146
146
146
Secondary
64.
66.
49, 51, and 86.
103.
61 and 98.
65, 83, 85, 98,
and 100.
61 and 98.
85.
62, 64, and 100.
99, 117, and 119.
119 and 121.
83, 85, and 129.
63, 65, and 114.
77.
95, 97, and 132.
129, 208, and
206.
83, 85, 99, 132.
and 134.
77.
63 and 65.
171, 175, 250,
252, 254, and
256.
83, 85. 131, 133.
and 166.
129, 131. and
166.
91.
114.
91.
148 and 113.
148 and 113.
148 and 113.
1 For chromatographic conditions, see Tabio 1.
TABLE 5—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 624"
Limit for ' Range for X
Range for P,
P, (%)
Benzene
Bromodichloromethane
Bromoiorm ,
Bromomethane
Carbon telracWoride
Chio^obenzen"
Chloroelhane
2-Chloroeihylvinyl ether , ,
Chloroform
Chlorometnane ,
DibromGcnioromethane
1 ,2-DJehlorobenzene
1 ,3-DicNorobenzene
1,4-Dichlorobenzer.e
1,1 -Dichloroethane
1,2-Dichloroethane
1,1-Dichlorofhsne
trans-1,2-Dichloroelhene
12.8- 27.2
13.1 -26.9 ;
142 -25.8 '
2.8-37.2
14.6- 25.4 i
13.2-26.8 i
7.6-32.4 j
D - 44.8
13.5-26.5 i
D-408
13.5-26.5
12.6-27.4 j
14.6-254
126-27.4
14.5-25.5 I
13.6 -26.4
10.1-299
13.9-26.1
6.9 i 15.2
6.4 10.1
5.4i 11.4
17.9; D
5.2 17.2
6.3 16.4
1 1 .4 | 8.4
25.9 ! D
6.1 '. 13.7
19.8 I D
6.1 : 13.8
7.1 j 11.8
55 ; 170
7.1 . 11.8
5.1 14.2
60 14.3
9 1 j 3.7
5.7 13.6
- 26.0
-28.0
-31.1
-41.2
- 23.5
- 27.4
- 40-4
-50.4
- 24.2
-45.9
-26.6
- 34.7
-28.8
-34.7
- 28.5
-27.4
-42.3
-28.5
37-
35-
45-
D-
70-
37 -
14-
D-
51-
D-
53-
18-
59-
18-
59-
49-
D-
54^
151
155
169
242
140
160
230
305
13B
273
149
190
156
190
155
155
234
156
204
-------
Environmental Protection Agency
Pt. 136, App. A.Mefh. 624
TABLE 5—CALIBRATION AND QC ACCEPTANCE CRITERIA—METHOD 624^—Continued
1,2-Dichioropropane
eis-lsS-Dichioropropene ......
trans~1,3-DicNoropfGpene ...
Ethyl benzene
Methylene chloride .............
1,1,2,2-Teirachiofoethane ...
Tetraohloroethene ... .....
Toluene
1,1,1-Trichtoroethane ,„.,,,.,.
1.1,2-Trichloroethane ..,,
Trichloroethene .,
Trichlorofluoromefhane .......
Vinyl chloride
Range for Q Limit for
Range for X
(HA)/L) s (M/9/Lj | (M/9/L)
r H
6.8-335
4.8-35.2
10.0-30.0
11.8-28,2
12.1-27.9
12,1-27.9
14.7-25.3
14.9-25-1
15.0-25.0
14.2-25.8
13.3-26.7
9.6-30.4
13.8 3.8-36.2
15.8
10.4
7.5
7.4
7.4
5.0
4.8
4.6
5.5
6.6
10.0
1.0-39.0
7.6 - 32.4
17.4-26.7
D-41.0
13.5-27.2
17.0-26.6
16.6-26.7
13.7-30.1
14.3-27.1
18.6-27.6
8.9-31.5
0.8-39.2 | 20,0 | D-43.5
Range for P,
P. (%)
D-210
0-227
17-183
37-162
0-221
46-157
64-148
47-150
52-162
52-150
71-157
17-181
D-251
Q= Concentration measured in QC check sample, in pg/L (Section 7.5,3)
s= Standard deviation of four recovery measurements, in jig/L (Section 8,2.4).
X= Average recovery of four recovery measurements, in ug/L (Section 8.2.4),
p. ps= Percent recovery measured, {Section 8.3,2, Section 8.4.2).
DK Detected; result must be greater than zero.
* Criteria were calculated assuming a QC check sample concentration of 20 ^g/L
NOTE: These criteria are based directly upon the method performance data in Table 6, Where necessary, the limits foe recov-
ery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 6.
TABLE 8—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 624
Parameter
Bromoform ,. ,.,..,. , .,.,.,...,,,.,,. ...... — ....... — ,,.,.,....,.,,,.,
Carbon tetrachloride ,, ,,, - -
Chforobenzene ..,,,...,,..,..,,,...,.»..,,...,..»...,.,.,.,,.,..,,,,.,,,., ,,
2-ChIofoethyMny) ether <* ., ..,
Chloroform ....,...,
Chloromelhane ,., , , ....,.,,,..
t .3~Dicriforobenzene .,.,, ,,.. ,...-,
1.4-~0ichlorobenzeneh
1,1-Dichloroethane .,.,.....,,, ,.„„...,.,., ,........,„.,..
1,2-Dichloroethane , ,.,.
1,1-Dichloroethene .,.,.,.„...,.,.., .....,.,.,.....,,., ,..,..,-.,.,..,..,.„...,
trans-l,2,-Dichlaroethene
"LS-Dichloropropane"-1 ,,,, ,.. , .,, ,., ,
cis-1,3-DtehIorapropene;t
Ethyl benzene , ,.,„-...
Methylene chloride
1,1.2,2-Tetrachloroethane .,.
Tetrachloroethene
1,1,1-Trichloroethane , , ., „
1,1,2-Trichloroethane
Trichloroethene ,.,.,....,....,.......„., ..,...,.,...,.,......,.,.,........,.,
T rich io roll ouromefhane
Vinyl chloride
Accuracy, as
recovery, X'
«U
0.93C+2.00
1 03C - 1 58
1.18C-2.35
1.00C
1.10C-1.68
0.98C+2.28
1 18C+0 81
1.00C
0.93C+0.33
1.03OQ.81
1.01C-0.03
0.94O4.47
1.060-1-1.68
094O4.47
1 .GSO0.36
1. 02O0.45
1.12OQ.61
1.05OQ.Q3
LOCO
1.00C
1 ooc
G.98O2.48
0.87C+1.88
0.93C-I-1.76
1.06C+0.60
0.98C+2.03
1 .06C+0.73
0.95C+1.71
1 .0402.27
0.99O0.39
1.00C
Single analyst
precision, s~'
(M9/L)
0.26X-1.74
0 1 5X+0 59
0.12X-G.36
043X
0.12X^0.25
0.16X-0.09
0 14X+2 78
0.62X
0.16X+0.22
0.37X-2.14
0.17X-0 18
0.22X-1.45
0.14X-0.48
0.22X-1.45
0.13X-0.05
0.17X-0.32
0.17X^1.06
0.14X+0.09
0.33X
0.38X
0 25X
0.14X+1.00
0.1SX+1.07
0.16X+0.69
0.13X-0.18
0.15X-071
0.12X-0.15
0.14X+0.02
0.13X+0.36
033X-1.48
0.48X
Overall preci-
sion, S' (fig/L)
1 - - '
025X-1 33
0 20X-f1 13
0.17X+1.38
0.58X
0.11X+0.37
0.26X-1.92
0 29X+1 75
0.84X
0.18X^0.16
0.58X+0.43
0 17X»049
0.30X-1.20
0.18X-0.82
0.30X-1.20
0.16X+0.47
0.21 X- 0.38
0.43X-0.22
0.19X^0.17
0.45X
O.S2X
0 34X
0.26X-1.72
0.32X+4.00
020X^0.41
0.16X-0.45
0.22X-1 71
0.21X-0.39
0.18X1-0.00
0 12X-rQ.S9
0.34X-0.39
0.65X
X'=Expected recovery for one or more measurements of a sample containing a concentration of C. in f;g/L.
S!=Expected single analyst standard deviation of measurements at an average concentration found ofX. in jjg/L.
S'=Expected inter!aboratory standard deviation of measurements at an average conceniration found ofX, in ug/L
C=sTrue value for the concentration, in ug/L.
X^Average recovery found for measurements of samples containing a concentration of C, in |ig/L.
•L Estimates based upon the performance in a single laboratosy.''
""Due io chromaiographic resolution problems, performance statements for these isorners are based upon Jhe sums of their
concentrations.
205
-------
Pt. 136,App. A,M©th. 624
40 CFR Ch. ! (7-1-04 Edition)
OPTIONAL
FOAM
TRAP
-EXIT % IN.
0. D.
—-14MM 0. D,
INLET W IN.
0. D.
% IN.
0. D. EXIT
1 I
1 I
11
11
11
INLET
2-WAY SYRINGE VALVE
•17CM. 20 GAUGE SYRINGE NEEDLE
,0.0. RUBBER SEPTUM
10MU. 0. D. 1/16 IN. O.D.
W STAINLESS STEEL
-INLET
W IN. 0. D.
13X MOLECULAR
SIEVE PURGE
GAS FILTER
PURGE GAS
FLOW
CONTROL
10MM GLASS FRIT
MEDIUM POROSITY
Figyre 1. Purging device.
206
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 624
PACKING PROCEDURE
GLASS
WOOL 5MN!
GRADE 15
SILICA GEL8CM
TEW AX 15CM
3%OV-1 1CM
GLASS 5MM
WOOL
CONSTRUCTION
COMPRESSION
FITTING NUT
AND FERRULES
14FT. 7n/FOOT
RESISTANCE WIRE
WRAPPED SOLID
THERMOCOUPLE/
„ CONTROLLER
SENSOR
TRAP INLET
TUBING 25CM
0.105 IN. I.D.
0.125 IN. O.D.
STAINLESS STEEL
Figure 2. Trap packings and construction to include
desorb capability.
207
-------
Pt. 136, App. A, Meth. 624
40 CFR Ch. I (7-1-04 Edition)
CARRIER GAS FLOW CONTROL
PRESSURE REGULATOR
\
PURGE GAS
FLOW CONTROL \|
13X MOLECULAR
SIEVE FILTER
LIQUID INJECTION PORTS
COLUMN OVEN
[1 fl fl jT-J->j~- CONFIRMATORY COLUMN
n_L> TO DETECTOR
I "-— ANALYTICAL COLUMN
OPTIONAL 4-PORT COLUMN
SELECTION VALVE
jf i 51 / TRAP WLET
VALVE -//RESISTANCE WIRE
CHEATER CONTROL
TRAP (OFF i
22'C
PURGING
DEVICE
Note:ALL LINES BETWEEN
TRAP AND GC
SHOULD BE HEATED
TO 80*C
Figure 3. Purge and trap system - purge mode.
CARRIER GAS
FLOW CONTROL
PRESSURE
REGULATOR,
LIQUID INJECTION PORTS
PURGE GAS
FLOW CONTROL^ i '
13X MOLECULAR
SIEVE FILTER
,COLUMN OVEN
I n n n i J CONFIRMATORY COLUMN
nr n n rTn_L>TO DETECTOR
fjflJ U U U [ ^-ANALYTICAL COLUMN
OPTIONAL 4-PORT COLUMN
SELECTION VALVE
6-PORT TRAP INLET
VALVE J RESISTANCE WIRE UC,TCD
HcATtn
~7^\^ CONTROL
ONJ
Note:
ALL LINES BETWEEN
TRAP AND GC
SHOULD BE HEATED
TO 95°C.
PURGING
DEVICE
Figure 4, Purge and trap system - desorb mode.
208
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
COLUMN: 1% SP-1000 ON CARBOPACK-B
PROGRAM: 45°C FOR 3 WIN, 8°C/MIN TO 220°C
DETECTOR: MASS SPECTROMETER
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z 9 = ^
ui 3 o 'r
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12 14 IS 18 20
RETENTION TIME, MIN.
Figure 5. Gas chromatogram of volatile organics.
METHOD 625—BASE-NEUTRALS AND ACIDS
1. Scope and Application
1.1 This method covers the determinat-ion
of a number of organic compounds that are
partitioned into an organic solvent and are
amenable to gas chromatography. The pa-
rameters listed in Tables 1 and 2 may be
qualitatively and quantitatively determined
using this method.
1.2 The method may be extended to in-
clude the parameters listed In Table 3. Benzi-
dine can be subject to oxidative losses during-
solvent concentration. Under the alkaline
conditions of the extraction step. a-BHC, •/-
BHC. endosulfan I and II. and endrin are sub-
ject to decomposition.
Hexachlorocyclopentadiene is subject to
thermal decomposition in the inlet of the gas
chromatograph, chemical reaction in ace-
tone solution, and photochemical decomposi-
tion. N-nitrosodimethylamine is difficult to
separate from the solvent under the
chromatographic conditions described. N-
nitrosodiphenylamine decomposes in the gas
chromatographic inlet and cannot be sepa-
rated from diphenylamine. The preferred
method for each of these parameters is listed
in Table 3.
1.3 This is a gas chromatographic/mass
spectrometry (GO-MS) method2-14 applicable
to the determination of the compounds listed
in Tables 1, 2, and 3 in municipal and indus-
trial discharges as provided under 40 CFR
138.1.
209
-------
Pt. 136, App. A, Mefh. 625
40 CFR Ch. I (7-1-04 Edition)
1.4 The method detection limit (MDL, de-
fined in Section 16.1)1 for each parameter is
listed in Tables 4 and 5. The MDL for a spe-
cific wastewater may differ from those list-
ed, depending upon the nature of inter-
ferences in the sample matrix.
1.5 Any modification to this method, be-
yond those expressly permitted, shall be con-
sidered as a major modification subject to
application and approval of alternate test
procedures under 40 CPR 136.4 and 136.5. De-
pending upon the nature of the modification
and the extent of intended use, the applicant
may be required to demonstrate that the
modifications will produce equivalent results
when applied to relevant wastewaters.
1.6 This method is restricted to use by or
under the supervision of analysts experi-
enced in the use of a gas chromatograph/
mass spectrometer and in the interpretation
of mass spectra. Each analyst must dem-
onstrate the ability to generate acceptable
results with this method using the procedure
described in Section 8.2.
2, Summary of Method
2.1 A measured volume of sample, approxi-
mately 1-L, is serially extracted with meth-
ylene chloride at a pH greater than 11 and
again at a pH less than 2 using a separatory
funnel or a continuous extractor.2 The meth-
ylene chloride extract is dried, concentrated
to a volume of 1 mL, and analyzed by Q-C/MS.
Qualitative identification of the parameters
in the extract is performed using the reten-
tion time and the relative abundance of
three characteristic masses (m/z). Quan-
titative analysis is performed using internal
standard techniques with a single char-
acteristic m/z,
3. Interferences
3,1 Method interferences may be caused
by contaminants in solvents, reagents, glass-
ware, and other sample processing hardware
that lead to discrete artifacts and/or ele-
vated baselines in the total ion current pro-
files. All of these materials must be rou-
tinely demonstrated to be free from inter-
ferences under the conditions of the analysis
by running laboratory reagent blanks as de-
scribed in Section 8.1.3,
3.1.1 Glassware must he scrupulously
cleaned.3 Clean all glassware as soon as pos-
sible after use by rinsing with the last sol-
vent used in it. Solvent rinsing should be fol-
lowed by detergent washing with hot water,
and rinses with tap water and distilled
water. The glassware should then be drained
dry, and heated in a muffle furnace at 400 °C
for 15 to 30 min. Some thermally stable ma-
terials, such as PCBs, may not be eliminated
by this treatment- Solvent rinses with ace-
tone and pesticide quality hexane may be
substituted for the muffle furnace heating.
Thmroug'h rinsing with such solvents usually
eliminates PCB interference. Volumetric
ware should not be heated in a muffle fur-
nace. After drying and cooling, glassware
should be sealed and stored in a clean envi-
ronment to prevent any accumulation of
dust or other contaminants. Store inverted
or capped with aluminum foil.
3.1.2 The use of high purity reagents and
solvents helps to minimize interference prob-
lems. Purification of solvents by distillation
in all-glass systems may be required.
3.2 Matrix interferences may be caused by
contaminants that are co-extracted from the
sample. The extent of matrix interferences
will vary considerably from source to source,
depending upon the nature and diversity of
the industrial complex or municipality being
sampled.
3.3 The base-neutral extraction may cause
significantly reduced recovery of phenol, 2-
methylphenol, and 2.4-dinaethylphenol. The
analyst must recognize that results obtained
under these conditions are minimum con-
centrations.
3.4 The packed gas chromatographic col-
umns recommended for the basic fraction
may not exhibit sufficient resolution for cer-
tain isomeric pairs including the following:
anthracene and phenanthrene: chrysene and
benzo(a)anthracene; and
benzo(b)fluoranthene and
benzo(k)fluoranthene. The gas
chromatographic retention time and mass
spectra for these pairs of compounds are not
sufficiently different to make an unambig-
uous identification. Alternative techniques
should be used to identify and quantify these
specific compounds, such as Method 610.
3,5 In samples that contain an inordinate
number of interferences, the use of chemical
ionization (CI) mass spectrometry may make
identification easier. Tables 6 and 7 give
characteristic GI ions for most of the com-
pounds covered by this method. The use of OI
mass spectrometry to support electron ion-
ization (El) mass spectrometry is encouraged
but not required.
4. Safety
4,1 The toxlcity or carcinogenicity of
each reagent used in this method have not
been precisely defined; however, each chem-
ical compound should be treated as a poten-
tial health hazard. Prom this viewpoint, ex-
posure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified-1-6 for
the information of the analyst.
210
-------
Environmental Protection Agency
Pt, 136, App. A, Meth. 625
4.2 The following parameters covered by
this method have been tentatively classified
as known or suspected, human or mamma-
lian carcinogens: benzo(a)anthraeene, benzi-
dine, 3,3'-dichlorobenzidine, benzo(a)pyrene,
ot-BHC, (J-BHC, 5-BHC, y-BHC,
dibenzo(a,h)anthraeene, N-
nitrosodimethylainine, 4,4'-DDT, and poly-
chlorinated biphenyls (PCBs). Primary
standards of these toxic compounds should
be prepared in a hood. A NIOSH/MESA ap-
proved toxic gas respirator should be worn
when the analyst handles high concentra-
tions of these toxic compounds.
5. Apparatus and Materials
5.1 Sampling equipment, for discrete or
composit sampling.
5.1.1 Grab sample bottle—1-L or 1-gt,
amber glass, fitted with a screw cap lined
with Teflon, Foil may be substituted for Tef-
lon if the sample is not corrosive. If amber
bottles are not available, protect samples
from light. The bottle and cap liner must be
washed, rinsed with acetone or methylene
chloride, and dried before use to minimize
contamination.
5.1.2 Automatic sampler (optional')—The
sampler must incorporate glass sample con-
tainers for the collection of a minimum of
250 rnL of sample. Sample containers must be
kept refrigerated at 4 °C and protected from
light during compositing. If the sampler uses
a peristaltic pump, a minimum length of
compressible silicone rubber tubing may be
used, before use, however, the compressible
tubing should be throughly rinsed with
methanol, followed by repeated rinsing's with
distilled water to minimize the potential for
contamination of the sample. An integrating
flow meter is required to collect flow propor-
tional composites.
5.2 Glassware
-------
Pt. 136, App. A, Meth, 625
40 CFR Ch. I (7-1-04 Edition)
allows Integrating the abundance in any
KICP between specified time or scan number
limits.
6. Reagents
6.1 Reagent water—Reagent water is de-
fined as a water in which an interferent is
not observed at the MDL of the parameters
of interest.
6.2 Sodium hydroxide solution (10 N)—
Dissolve 40 g of NaOH (ACS) in reagent water
and dilate to 100 mL.
6.3 Sodium thlosulfate—(ACS) Granular.
6.4 Sulfuric acid (1+1)—Slowly, add 50 mL
of H,SO4 (ACS, sp, gr. 1.84) to 50 mL of rea-
gent water.
6.5 Acetone, methanol, methlylene chlo-
ride—Pesticide quality or equivalent.
6.6 Sodium sulfate—(ACS) Granular, an-
hydrous. Purify by heating at 400 CC for 4 h
In a shallow tray.
6.7 Stock standard solutions (1.00 (ig/nD—
standard solutions can be prepared from pure
standard materials or purchased as certified
solutions.
6.7.1 Prepare stock standard solutions by
accurately weighing about 0.0100 g of pure
material, Dissolve the material in pesticide
quality acetone or other suitable solvent and
dilute to volume in a 10-mL volumetric
flask. Larger volumes can be used at the con-
venience of the analyst. When compound pu-
rity is assayed to be 96% or greater, the
weight may be used without correction to
calculate the concentration of the stock
standard. Commercially prepared stock
standards may be used at any concentration
if they are certified by the manufacturer or
by an independent source.
6.7.2 Transfer the stock standard solu-
tions into Teflon-sealed screw-cap bottles.
Store at 4 °C and protect from light. Stock
standard solutions should be checked fre-
quently for signs of degradation or evapo-
ration, especially just prior to preparing
calibration standards from them.
6.7 3 Stock standard solutions must be re-
placed after six months, or sooner if com-
parison with quality control check samples
indicate a problem.
8.8 Surrogate standard spiking' solution—
Select a minimum of three surrogate com-
pounds from Table 8. Prepare a surrogate
standard spiking- solution containing each
selected surrogate compound at a concentra-
tion of 100 ugv'raL in acetone. Addition of 1.00
mL of this solution to 1000 mL of sample is
equivalent to a concentration of 100 ng.'L of
each surrogate standard. Store the spiking1
solution at 4 "C in Teflon-sealed glass con-
tainer. The solution should be checked fre-
quently for stability. The solution must be
replaced after six months, or sooner if com-
parison with quality control check standards
indicates a problem.
6.9 DFTPP standard—Prepare a 25
solution of DPTPP in acetone.
6.10 Quality control check sample con-
centrate—See Section 8.2.1.
7. Calibration
7.1 Establish gas chromatographic oper-
ating parameters equivalent to those indi-
cated in Table 4 or 5.
7.2 Internal standard calibration proce-
dure—To use this approach, the analyst must
select three or more internal standards that
are similar in analytical behavior to the
compounds of interest, The analyst must fur-
ther demonstrate that the measurement of
the internal standards Is not affected by
method or matrix interferences. Some rec-
ommended internal standards are listed in
Table 8. Use the base peak m/z as the pri-
mary m/z for quantification of the standards.
If interferences are noted, use one of the
next two most intense m/z quantities for
quantification.
7.2.1 Prepare calibration standards at a
minimum of three concentration levels for
each parameter of interest by adding appro-
priate volumes of one or more stock stand-
ards to a volumetric flask. To each calibra-
tion standard or standard mixture, add a
known constant amount of one or more in-
ternal standards, and and dilute to volume
with acetone. One of the calibration stand-
ards should be at a concentration near, but
above, the MDL and the other concentra-
tions should correspond to the expected
range of concentrations found in real sam-
ples or should define the working range of
the GC/MS system.
7.2.2 Using injections of 2 to 5 jiL. analyze
each calibration standard according to Sec-
tion 13 and tabulate the area of the primary
characteristic m/z (Tables 4 and 5) against
concentration for each compound and inter-
nal standard. Calculate response factors iBP)
for each compound using Equation 1.
RF=(AJ(C,)
Equation 1
where:
A.,=Area of the characteristic m,;z for the pa-
rameter to be measured.
A;i=Area of the characteristic m/z for the in-
ternal standard.
Cis=Concentration of the internal standard
t|Jg'L).
Cs=Concentration of the parameter to be
measured (ug/L).
If the BF value over the working range is a
constant (<35% RSD), the RP can be assumed
to be invariant and the average RP ca.n be
used for calculations. Alternatively, the re-
sults can be used to plot a calibration curve
of response ratios, AV/A», vs. RF.
7.3 The working calibration curve or RP
must be verified on each working- day by the
212
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
measurement of one or more calibration
standards. If the response for any parameter
varies from the predicted response by more
than ±20%, the test must be repeated uning
a fresh calibration standard. Alternatively, a
new calibration curve must be prepared for
that compound.
8. Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality con-
trol program. The minimum requirements of
this program consist of an Initial demonstra-
tion of laboratory capability and an ongoing
analysis of spiked samples to evaluate and
document data quality. The laboratory must
maintain records to document the quality of
data that is generated. Ongoing data quality
checks are compared with established per-
formance criteria to determine if the results
of analyses meet the performance character-
istics of the method. When results of sample
spikes indicate atypical method perform-
ance, a quality control check standard must
be analyzed to confirm that the measure-
ments were performed in an in-control mode
of operation,
8.1.1 The analyst must make an initial,
one-time, demonstration of the ability to
generate acceptable accuracy and precision
with this method. This ability is established
as described in Section 8.2.
8.1,2 In recognition of advances that are
occuringr in ehromatography, the analyst is
permitted certain options (detailed in Sec-
tions 10.6 and 13.1) to improve the separa-
tions or lower the cost of measurements.
Bach time such a modification is made to
the method, the analyst is required to repeat
the procedure in Section 8.2.
8.1.3 Before processing any samples, the
analyst must analyze a reagent water blank
to demonstrate that interferences from the
analytical system and glassware are under
control. Each time a set of samples is ex-
tracted or reagents are changed, a reagent
water blank must be processed as a safe-
guard against laboratory contamination.
8.1.4 The laboratory must, on an ongoing
basis, spike and analyze a minimum of 5% of
all samples to monitor and evaluate labora-
tory data quality. This procedure is de-
scribed in Section 8.3,
8.1.5 The laboratory must, on an ongoing
basis, demonstrate through the analyses of
quality control check standards that the op-
eration of the measurement system is in con-
trol. This procedure is described in Section
8.4. The frequency of the check standard
analyses is equivalent to 5% of all samples
analyzed but may be reduced if spike recov-
eries from samples (Section 8.3) meet all
specified quality control criteria.
8.1.6 The laboratory must maintain per-
formance records to document the quality of
data that is generated. This procedure is de-
scribed in Section 8.5.
8.2 To establish the ability to generate
acceptable accuracy and precision, the ana-
lyst must perform the following operations.
8.2.1 A quality control (QC) check sample
concentrate is required containing each pa-
rameter of interest at a concentration of 100
Hg/rnL in acetone. Multiple solutions may be
required, PCBs and multicomponent pes-
ticides may be omitted from this test. The
QC check sample concentrate must be ob-
tained from the U.S. Environmental Protec-
tion Agency, Environmental Monitoring and
Support Laboratory in Cincinnati, Ohio, if
available. If not available from that source,
the QC check sample concentrate must be
obtained from another external source. If not
available from either source above, the QC
check sample concentrate must be prepared
by the laboratory using stock standards pre-
pared independently from those used for cali-
bration.
8.2.2 Using a pipet, prepare QC check sam-
ples at a concentration of 100 ngv'L by adding
1.00 mL of QC check sample concentrate to
each of four 1-L aliquots of reagent water.
8.2.3 Analyze the well-mixed QC check
samples according to the method beginning
in Section 10 or 11.
8.2.4 Calculate the average recovery (X) in
ug/L, and the standard deviation of the re-
covery (s) in jig.'L, for each parameter using
the four results.
8.2.5 For each parameter compare s and X
with the corresponding acceptance criteria
for precision and accuracy, respectively.
found in Table 8, If s and X for all param-
eters of interest meet the acceptance cri-
teria, the system performance is acceptable
and analysis of actual samples can begin. If
any individual s exceeds the precision limit
or any individual X falls outside the range
for accuracy, the system performance is un-
acceptable for that parameter.
NOTE: The large number of parameters in
Table 6 present a substantial probability
that one or more will fail at least one of the
acceptance criteria when all parameters are
analyzed.
8.2.6 When one or more of the parameters
tested fail at least one of the acceptance cri-
teria, the analyst must proceed according to
Section 8.2.6.1 or 8.2.6.2.
8.2.6.1 Locate and correct the source of
the problem and repeat the test for all pa-
rameters of interest beginning with Section
8.2.2.
8.2.6.2 Beginning with Section 8.2.2. repeat
the test only for those parameters that
failed to meet criteria. Repeated failure,
however, will confirm a general problem
with the measurement system. If this occurs,
locate and correct the source of the problem
and repeat the test for all compounds of in-
terest beginning with Section 8.2.2.
8.3 The laboratory must, on an ongoing
basis, spike at least 5% of the samples from
each sample site being monitored to assess
213
-------
Pt. 136, App. A, Mefh. 625
40 CFR Ch. i (7-1-04 Edition)
accuracy. For laboratories analyzing 1 to 20
samples per month, at least one spiked sam-
ple per month is required.
8.3.1. The concentration of the spike in
the sample should be determined as follows;
8.3.1 If, as in compliance monitoring, the
concentration of a specific parameter in the
sample is being- checked against a regulatory
concentration limit, the spike should be at
that limit or 1 to 5 times higher than the
background concentration determined in
Section 8.3.2, whichever concentration would
be larger.
8.3.1,2 If the concentration of a specific
parameter in the sample is not being
checked against a limit specific to that pa-
rameter. the spike should be at 100 iig/L or 1
to 5 times higher than the background con-
centration determined in Section 8,3,2,
whichever concentration would be larger,
8.3,1.3 If it is impractical to determine
background levels before spiking (e.g.. max-
imum holding- times will be exceeded), the
spike concentration should be (1) the regu-
latory concentration limit, if any; or, if none
(2) the larger of either 5 times higher than
the expected background concentration or
8.3.2 Analyze one sample aliquot to deter-
mine the background concentration (B) of
each parameter. If necessary, prepare a new
QC check sample concentrate (Section 8,2.1)
appropriate for the background concentra-
tions in the sample. Spike a second sample
aliquot with 1.0 mL of the QC check sample
concentrate and analyze it to determine the
concentration after spiking (A) of each pa-
rameter. Calculate each percent recovery (P)
as 1QQ(A-B)%/T, where T is the known true
value of the spike.
8.3.3 Compare the percent recovery (P) for
each parameter with the corresponding QC
acceptance criteria found in Table 6. These
acceptance criteria were calculated to in-
clude an allowance for error in measurement
of both the background and spike concentra-
tions, assuming a spike to background ratio
of 5:1. This error will tie accounted for to the
extent that the analyst's spike to back-
ground ratio approaches 5:1. 7 If spiking was
performed at a concentration lower than 100
Hg/L, the analyst must use either the QC ac-
ceptance criteria in Table 6, or optional QC
acceptance criteria calculated for the spe-
cific spike concentration. To calculate op-
tional acceptance criteria for the recovery of
a parameter: (1) Calculate accuracy (X')
using the equation in Table 7, substituting
the spike concentration (T) for C; (2) cal-
culate overall precision (S') using the equa-
tion in Table 7, substituting X' for X; (3) cal-
culate the range for recovery at the spike
concentration as (100 X7T)±2.44(100 S'/T)%7
8.3.4 If any individual P falls outside the
designated range for recovery, that param-
eter has failed the acceptance criteria. A
check standard containing each parameter
that failed the criteria must be analyzed as
described in Section 8.4.
8.4 If any parameter fails the acceptance
criteria for recovery in Section 8.3, a QC
check standard containing each parameter
that failed must be prepared and analyzed.
NOTE: The frequency for the required anal-
ysis of a QC check standard will depend upon
the number of parameters being simulta-
neously tested, the complexity of the sample
matrix, and the performance of the labora-
tory. If the entire list of single-component
parameters in Table 6 must be measured in
the sample in Section 8.3, the probability
that the analysis of a QC check standard will
be required is high. In this case the QC check
standard should be routinely analyzed with
the spike sample.
8.4.1 Prepare the QC check standard by
adding 1.0 mL of QC check sample con-
centrate (Section 8,2.1 or 8.3,2) to 1 L of rea-
gent water. The QC check standard needs
only to contain the parameters that failed
criteria in the test in Section 8,3,
8.4.2 Analyze the QC check standard to
determine the concentration measured (A) of
each parameter. Calculate each percent re-
covery (Ps) as 100 (A/T)%, where T is the true
value of the standard concentration,
8.4.3 Compare the percent recovery (Ps)
for each parameter with the corresponding
QC acceptance criteria found in Table 6. Only
parameters that failed the test in Section 8.3
need to be compared with these criteria. If
the recovery of any such parameter falls out-
side the designated range, the laboratory
performance for that parameter is judged to
be out of control, and the problem must be
immediately identified and corrected. The
analytical result for that parameter in the
unspiked sample is suspect and may not be
reported for regulatory compliance purposes.
8.5 As part of the QC program for the lab-
oratory, method accuracy for wastewater
samples must be assessed and records must
be maintained. After the analysis of five
spiked wastewater samples as in Section 8.3,
calculate the average percent recovery (P)
and the standard deviation of the percent re-
covery (sp). Express the accuracy assessment
as a percent interval from P —2sp to P+2sp. If
P=90% and sp=10%, for example, the accuracy
interval is expressed as 70 — 110%. Update the
accuracy assessment for each parameter on a
regular basis (e.g. after each five to ten new
accuracy measurements).
8.6 As a quality control check, the labora-
tory must spike all samples with the surro-
gate standard spiking solution as described
in Section 10.2, and calculate the percent re-
covery of each surrogate compound.
8.7 It Is recommended that the laboratory
adopt additional quality assurance practices
for use with this method. The specific prac-
tices that are most productive depend upon
the needs of the laboratory and the nature of
214
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Environmental Protection Agency
Pt, 136, App. A, Meth. 625
the samples. Field duplicates may be ana-
lyzed to assess the precision of the environ-
mental measurements. Whenever possible,
the laboratory should analyze standard ref-
erence materials and participate in relevant
performance evaluation studies.
9. Sample Collection, Preservation, and
Handling
9.1 Grab samples mast be collected in
glass containers, Conventional sampling
practices8 should be followed, except that
the bottle must not be prerinsed with sample
before collection. Composite samples should
be collected in refrigerated glass containers
in accordance with the requirements of the
program. Automatic sampling equipment
must be as free as possible of Tygon tubing
and other potential sources of contamina-
tion.
9.2 All sampling must be iced or refrig-
erated at 4 °C from the time of collection
until extraction. Pill the sample bottles and.
if residual chlorine is present, add 80 mg of
sodium thiosulfate per liter of sample and
mix well. EPA Methods 330.4 and 330.5 may
be used for measurement of residual chlo-
rine.' Field test kits are available for this
purpose.
9.3 All samples must be extracted within 7
days of collection and completely analyzed
within 40 days of extraction.
10. Separator^ Funnel Extraction
10.1 Samples are usually extracted using
separatory funnel techniques. If emulsions
will prevent achieving acceptable solvent re-
covery with separatory funnel extractions,
continuous extraction (Section 11) may be
used. The separatory funnel extraction
scheme described below assumes a sample
volume of 1 Ij. When sample volumes of 2 L.
are to be extracted, use 250, 100, and 100-mL
volumes of methylene chloride for the serial
extraction of the base/neutrals and 200, 100,
and 100-mL volumes of methylene chloride
for the acids.
10.2 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Pour the entire sample
into a 2-L separatory funnel. Pipet 1.00 mL
of the surrogate standard spiking solution
into the separatory funnel and mix well.
Check the pH of the sample with wide-range
pH paper and adjust to pH>ll with sodium
hydroxide solution.
10.3 Add 60 mL of methylene chloride to
the sample bottle, seal, and shake for 30 s to
rinse the inner surface. Transfer the solvent
to the separatory funnel and extract the
sample by shaking the funnel for 2 min. with
periodic venting to release excess pressure.
Allow the organic layer to separate from the
water phase for a minimum of 10 min. If the
emulsion interface between layers is more
than one-third the volume of the solvent
layer, the analyst must employ mechanical
techniques to complete the phase separation.
The optimum technique depends upon the
sample, but may include stirring, filtration
of the emulsion through glass wool, cen-
trifugation, or other physical methods. Col-
lect the methylene chloride extract in a 250-
mL Erlenmeyer flask. If the emulsion cannot
be broken (recovery of less than 80% of the
methylene chloride, corrected for the water
solubility of methylene chloride), transfer
the sample, solvent, and emulsion into the
extraction chamber of a continuous extrac-
tor and proceed as described in Section 11.3.
10.4 Add a second 60-mL volume of meth-
ylene chloride to the sample bottle and re-
peat the extraction procedure a second time,
combining' the extracts in the Erlenmeyer
flask. Perform a third extraction in the same
manner. Label the combined extract as the
base/neutral fraction.
10.5 Adjust the pH of the aqueous phase to
less than 2 using snlfuric acid. Serially ex-
tract the acidified aqueous phase three times
with 60-mL aliquots of methylene chloride.
Collect and combine the extracts in a 250-mL
Erlenmeyer flask and label the combined ex-
tracts as the acid fraction.
10.6 For each fraction, assemble a
Kuderna-Danish (K-D) concentrator by at-
taching a 10-mL concentrator tube to a 500-
mL evaporative flask. Other concentration
devices or techniques may be used in place of
the K-D concentrator if the requirements of
Section 8.2 are met.
10.7 For each fraction, pour the combined
extract through a solvent-rinsed drying col-
umn containing about 10 cm of anhydrous so-
dium snlfate, and collect the extract In the
K-D concentrator. Rinse the Erlenmeyer
flask and column with 20 to 30 mL of meth-
ylene chloride to complete the quantitative
transfer.
10.8 Add one or two clean boiling chips
and attach a three-ball Snyder column to the
evaporative flask for each fraction. Prewet
each Snyder column by adding about 1 rnL of
methylene chloride to the top. Place the K-
D apparatus on a hot water bath (60 to 65 °C)
so that the concentrator tube is partially
immersed in the hot water, and the entire
lower rounded surface of the flask is bathed
with hot vapor. Adjust the vertical position
of the apparatus and the water temperature
as required to complete the concentration in
15 to 20 min. At the proper rate of distilla-
tion the balls of the column will actively
chatter but the chambers will not flood with
condensed solvent. When the apparent vol-
ume of liquid reaches 1 mL, remove the K-D
apparatus from the water bath and allow it
to drain and cool for at least 10 min. Remove
the Snyder column and rinse the flask and
its lower joint into the concentrator tube
with 1 to 2 mL of methylene chloride. A 5-
mL syringe Is recommended for this oper-
ation.
215
203-160 D-8
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
10.9 Add another one or two clean boiling
chips to tie concentrator tube for each frac-
tion and attach a two-ball mlcro-Snyder col-
umn. Prewet the Snyder column by adding
about O.S mL of methylene chloride to the
top. Place the K-D apparatus on a hot water
bath (60 to 66 °C) so that the concentrator
tube is partially immersed in hot water. Ad-
just the vertical position of the apparatus
and the water temperature as required to
complete the concentration in 5 to 10 min.
At the proper rate of distillation the balls of
the column will actively chatter but the
chambers will not flood with condensed sol-
vent. When the apparent volume of liquid
reaches about 0.5 mL, remove the K-D appa-
ratus from the water bath and allow it to
drain and cool for at least 10 min. Remove
the Snyder column and rinse the flask and
its lower joint into the concentrator tube
with approximately 0.2 mL of acetone or
methylene chloride. Adjust the final volume
to 1.0 mL with the solvent. Stopper the con-
centrator tube and store refrigerated if fur-
ther processing will not be performed imme-
diately. If the extracts will be stored longer
than two days, they should be transferred to
Teflon-sealed screw-cap vials and labeled
base/neutral or acid fraction as appropriate.
10.10 Determine the original sample vol-
ume by refilling the sample bottle to the
mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample
volume to the nearest 5 niL.
11. Continuous Extraction
11.1 When experience with a sample from
a given source indicates that a serious emul-
sion problem will result or an emulsion is en-
countered using a separatory funnel in Sec-
tion 10.3, a continuous extractor should be
used.
11,2 Mark the water meniscus on the side
of the sample bottle for later determination
of sample volume. Check the pH of the sam-
ple with wide-range pH paper and adjust to
pH >11 with sodium hydroxide solution.
Transfer the sample to the continuous ex-
tractor and using a pipet, add 1.00 mL of sur-
rogate standard spiking solution and mix
well. Add 60 mL of methylene chloride to the
sample bottle, seal, and shake for 30 s to
rinse the inner surface. Transfer the solvent
to the extractor.
11.3 Repeat the sample bottle rinse with
an additional 50 to 100-mL portion of meth-
ylene chloride and add the rinse to the ex-
tractor.
11.4 Add 200 to 500 mL of methylene chlo-
ride to the distilling flask, add sufficient re-
agent water to ensure proper operation, and
extract for 24 h. Allow to cool, then detach
the distilling flask. Dry, concentrate, and
seal the extract as in Sections 10.6 through
10.9.
11.5 Charge a clean distilling flask with
500 mL of methylene chloride and attach it
to the continuous extractor. Carefully, while
stirring, adjust the pH of the aqueous phase
to less than 2 using sulfurie acid. Extract for
24 h. Dry, concentrate, and seal the extract
as in Sections 10.6 through 10.9.
12. Daily GC/MS Performance Tests
12.1 At the beginning of each day that
analyses are to be performed, the GC/MS sys-
tem must be checked to see if acceptable
performance criteria are achieved for
DFTPP.10 Each day that benzidine is to be
determined, the tailing factor criterion de-
scribed in Section 12.4 must be achieved.
Each day that the acids are to be deter-
mined, the tailing factor criterion in Section
12.5 must be achieved.
12.2 These performance tests require the
following instrumental parameters:
Electron Energy: 70 V (nominal)
Mass Eange: 35 to 450 amu
Scan Time: To give at least 5 scans per peak
but not to exceed 1 s per scan.
12.3 DFTPP performance test—At the be-
ginning of each day, inject 2 nL (50 ng) of
DFTPP standard solution. Obtain a back-
ground-corrected mass spectra of DFTPP
and confirm that all the key m/z criteria in
Table 9 are achieved. If all the criteria are
not achieved, the analyst must retune the
mass spectrometer and repeat the test until
all criteria are achieved. The performance
criteria must be achieved before any sam-
ples, blanks, or standards are analyzed. The
taililg factor tests in Sections 12,4 and 12.5
may be performed simultaneously with the
DFTPP test.
12.4 Column performance test for base/
neutrals—At the beginning of each day that
the base/neutral fraction is to be analyzed
for benzidine, the benzidine tailing factor
must be calculated. Inject 100 ng of benzidine
either separately or as a part of a standard
mixture that may contain DFTPP and cal-
culate the tailing factor. The benzidine tail-
ing factor must be less than 3.0. Calculation
of the tailing factor is illustrated in Figure
13.n Replace the column packing if the tail-
ing factor criterion cannot be achieved.
12.5 Column performance test for acids—
At the beginning of each day that the acids
are to be determined, inject 50 ng of
pentachlorophenol either separately or as a
part of a standard mix that may contain
DPTPP. The tailing factor for
pentachlorophenol must be less than 5. Cal-
culation of the tailing factor is illustrated in
Figure 13.u Replace the column packing if
the tailing factor criterion cannot be
achieved.
13. Gas Chromatagraphy/Mass Spectrometry
13.1 Table 4 summarizes the recommended
gas chromatographic operating conditions
for the base/neutral fraction. Table 5 summa-
rizes the recommended gas chromatographic
216
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
operating conditions for the acid fraction.
Included in these tables are retention times
and MDL that can be achieved under these
conditions. Examples of the separations
achieved by these columns are shown in Fig-
ures 1 through 12, Other packed or capillary
(open-tubular) columns or chrornatographic
conditions may be used if the requirements
of Section 8.2 are met.
13.2 After conducting the GO/MS perform-
ance tests in Section 12, calibrate the system
daily as described in Section 7.
13.3 The internal standard must be added
to sample extract and mixed thoroughly im-
mediately before it is injected into the in-
strument. This procedure minimizes losses
due to adsorption, chemical reaction or
evaporation.
13.4 Inject 2 to 5 nL of the sample extract
or standard into the GC/MS system using the
solvent-flush technique,12 Smaller (1.0 nL)
volumes may be injected if automatic de-
vices are employed. Record the volume in-
jected to the nearest 0.05 nL.
13.5 If the response for any m/z exceeds
the working range of the GC/MS system, di-
lute the extract and reanalyze.
13.6 Perform all qualitative and quan-
titative measurements as described in Sec-
tions 14 and 15. When the extracts are not
being used for analyses, store them refrig-
erated at 4°C, protected from light in screw-
cap vials equipped with unpierced Teflon-
lined septa.
14, Qualitative Identification
14.1 Obtain EICPs for the primary m/z and
the two other masses listed in Tables 4 and
5. See Section 7.3 for masses to be used with
internal and surrogate standards. The fol-
lowing criteria must be met to make a quali-
tative identification:
14.1.1 The characteristic masses of each
parameter of interest must maximize in the
same or within one scan of each other.
14.1.2 The retention time must fall within
±30 s of the retention time of the authentic
compound.
14.1.3 The relative peak heights of the
three characteristic masses in the EIOPs
must fall within ±20% of the relative inten-
sities of these masses in a reference mass
spectrum. The reference mass spectrum can
be obtained from a standard analyzed in the
GC/MS system or from a reference library.
14.2 Structural isomers that have very
similar mass spectra and less than 30 s dif-
ference in retention time, can be explicitly
identified only if the resolution between au-
thentic isomers in a standard mix is accept-
able. Acceptable resolution is achieved if the
baseline to valley height between the iso-
mers is less than 25% of the sum of the two
peak heights. Otherwise, structural isomers
are identified as isomeric pairs.
15. Calculations
15.1 When a parameter has been identi-
fied, the quantitation of that parameter will
be based on the integrated abundance from
the EICP of the primary characteristic m/z
in Tables 4 and 5. Use the base peak m/z for
internal and surrogate standards. If the sam-
ple produces an interference for the primary
m/z, use a secondary characteristic m/z to
quantitate.
Calculate the concentration in the sample
using the response factor (RF) determined in
Section 7.2.2 and Equation 3.
(A.XI.)
Concentration
Equation 3
where:
AN=Area of the characteristic m/z for the pa-
rameter or surrogate standard to be meas-
ured,
Ai»=Area of the characteristic m/z for the in-
ternal standard.
I«=Arnount of internal standard added to
each extract (ng).
V0=Volume of water extracted (L).
15.2 Report results in ng/L without correc-
tion for recovery data. All QC data obtained
should be reported with the sample results.
16. Method Performance
16.1 The method detection limit (MDL) is
defined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the value is above
zero.1 The MDL concentrations listed in Ta-
bles 4 and 5 were obtained using reagent
water.13 The MDL actually achieved in a
given analysis will vary depending on instru-
ment sensitivity and matrix effects.
16.2 This method was tested by 15 labora-
tories using reagent water, drinking water.
surface water, and industrial wastewaters
spiked at six concentrations over the range 5
to 1300 ug/L.14 Single operator precision,
overall precision, and method accuracy were
found to be directly related to the concentra-
tion of the parameter and essentially inde-
pendent of the sample matrix. Linear equa-
tions to describe these relationships are pre-
sented in Table 7.
17. Screening Procedure for 2,3,7,8-
TetmchloroAibenzo-p-dioxin (2,3,7,3-TCDD)
17.1 If the sample must be screened for
the presence of 2,3,7,8-TCDD, it is rec-
ommended that the reference material not
be handled in the laboratory unless extensive
safety precautions are employed. It is suffi-
cient to analyze the base/neutral extract by
selected ion monitoring (SIM) GC/MS tech-
niques, as follows;
17.1.1 Concentrate the base/neutral ex-
tract to a final volume of 0.2 ml.
217
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
17,1.2 Adjust the temperature of the base/
neutral column (Section 5.6,2) to 220 °C.
17.1.3 Operate the mass spectrometer to
acquire data In the SIM mode using the Ions
at m/z 257, 320 and 322 and a dwell time no
greater than 333 milliseconds per mass.
17.1.4 Inject 5 to 7 nL of the base/neutral
extract. Collect SIM data for a total of 10
mln.
17,1.5 The possible presence of 2,3,7,8-
TCDD is indicated if all three masses exhibit
simultaneous peaks at any point in the se-
lected ion current profiles.
17.1.6 For each occurrence where the pos-
sible presence of 2,3,7,8-TCDD is indicated,
calculate and retain the relative abundances
of each of the three masses.
17.2 False positives to this test may be
caused by the presence of single or coelutlngr
combinations of compounds whose mass
spectra contain all of these masses.
17.3 Conclusive results of the presence and
concentration level of 2,3,7,8-TCDD can be
obtained only from a properly equipped lab-
oratory through the use of EPA Method 613
or other approved alternate test procedures.
REFERENCES
1. 40 CPE part 136, appendix B.
2. "Sampling and Analysis Procedures for
Screening of Industrial Effluents for Priority
Pollutants," U.S. Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268,
March 1977, Revised April 1977. Available
from Effluent Guidelines Division, Wash-
ington, DC 20460.
3. ASTM Annual Book of Standards, Part
31, D3694-78. "Standard Practices for Prepara-
tion of Sample Containers and for Preserva-
tion of Organic Constituents," American So-
ciety for Testing and Materials, Philadel-
phia.
4. "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
5. "OSHA Safety and Health Standards,
General Industry," (29 CFR part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206 (Revised, January 1976).
6. "Safety in Academic Chemistry Labora-
tories,"American Chemical Society Publica-
tion, Committee on Chemical Safety, 3rd
Edition, 1979.
7. Provost, L.P., and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15, 58-63 (1983). (The value 2.44
used in the equation in Section 8.3.3 is two
times the value 1.22 derived in this report.)
8, ASTM Annual Book of Standards, Part
31, D3370-76, "Standard Practices for Sam-
pling Water," American Society for Testing
and Materials, Philadelphia.
9. "Methods 330.4 (Titrimetric, DPD-PAS)
and 330.5 (Spectrophotometric, DPD) for
Chlorine, Total Residual," Methods for
Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, U.S. Environmental Pro-
tection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
45268, March 1979.
10. Eichelberger, J.W., Harris, L.E., and
Budde, W.L. "Reference Compound to Cali-
brate Ion Abundance Measurement in Gas
Chromatography-Mass Spectometry," Analyt-
ical Chemistry, 47, 995 (1975).
11. McNair, N.M. and Bonelli, E.J. "Basic
Chromatography," Consolidated Printing,
Berkeley, California, p. 52,1969.
12. Burke, J.A. "Gas Chromatography for
Pesticide Residue Analysis; Some Practical
Aspects," Journal of the Association of Official
Analytical Chemists, 48,1037 (1965).
13. Olynyk, P., Budde, W.L., and
Eichelberger, J.W. "Method Detection Limit
for Methods 624 and 625," Unpublished report,
May 14, 1980.
14. "EPA Method Study 30, Method 625,
Base/Neutrals, Acids, and Pesticides," EPA
600/4-84-053, National Technical Information
Service, PB84-206572, Springfield, Virginia
22161, June 1984.
TABLE 1— BASE/NEUTRAL EXTRACTABLES
Parameter
Acenaphthene ,
AWrin
Benzo(b)ftuoranthene .
Benzyl butyl phthalate
p-BHC
S-BMC
Bis(2-chloroethoxy)methane
Bis(2-ethylhexyl) phthalate
B(s(2-chlorolsopropyl) ether"
4-Bromophenyi phenyl ether"
4-Chlorophenyl phenyl ether
44'-DDD
4 4*-DDE
4 4'-DDT
Dibenzo(a,hSanthracene
1 ,3-Diehlorobenzene
1 ,2-Dichlorobenzene
3,3'-Dfch!orobenzidine
Diethyt phthalate .. ..
Dimethyl phttialate ..,...„,.
Di-n-octylphthaiate
Endosutfan sulfate
STORE!
No.
34205
34200
34220
39330
34526
34230
34242
34247
34521
34292
39338
34259
34273
34278
39100
34283
34636
39350
34581
34641
34320
39310
39320
39300
34556
39110
34566
34536
34571
34631
39380
34336
34341
34611
34626
34596
343S1
CAS No.
83-32-9
208-96-8
120-12-7
309-00-2
56-55-3
205-99-2
207-08-9
50-32-8
191-24-2
86-68-7
319_85-7
319-86-8
111-44-4
m-ai-i
117-81-7
108-60-1
101-55-3
57-74-9
91-58-7
7005-72-3
218-01-9
72-54-8
72-55-9
50-29-3
53-70-3
84-74-2
541-73-1
95-50-1
106-46-7
91-94-1
60-57-1
84-66-2
131-11-3
121-14-2
606-20-2
117-84-0
1031-07-8
218
-------
Environmental Protection Agency
Pt. 136, App, A, Metti. 625
TABLE 1—BASE/NEUTRAL EXTRACTABLES—
Continued
TABLE 2—ACID EXTRACTABLES
Parameter
Hexachloroeihane ,
Indeno{li2,3-cd)pyrene
Nitrobenzene
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254
PCB-1260
Toxaphene
1 ,2,4-TricNorobenzene
STORET
No.
34366
34378
34381
39410
39420
39700
34391
34396
34403
34408
34696
34447
34428
34671
39488
39492
39496
39500
39504
39508
34461
34469
39400
34551
CAS No.
7421-93—4
206-44-0
86-73-7
76-44-8
1024-57-3
1 1 8-74-1
87-68-3
67-72-1
193-39-5
78-59-1
91-20-3
98-95-3
621-64-7
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
1 1 097-69-1
11096-82-5
85-01-8
129-00-0
8001-35-2
120-82-1
Parameter
4-Ch!orc~3-methylphenoi
2-ChIorophenot
2,4-Dich!oropheno1
2,4-Dlmethylphenol
2,4-DiniJrophenol
2-Methyl-4,6-dinitrophenol
2-Nitropheno!
Penlachloropheno! ...
2.4,6-TrichlorODhenol
STORET
No.
34452
34586
34601
34606
34616
34657
34591
34646
38032
34694
34621
CAS No.
59-50-7
95-57-8
120-83-2
105-67-9
51-28-5
534-52-1
88-75-5
100-02-7
87-86-5
108-95-2
88-06-2
TABLE 3—ADDITIONAL EXTRACTABLE
PARAMETERS"
Parameter
Benzldine
P-BHC
8-BHC
Endosulfan I
Endosulfan (I
Endrin
Hexachlorocylopentadiene
N-Nltrosodimethylsmine ....
N-Nilrosodiphenyiamine ....
STORET
No.
39120
39337
39340
34361
34356
39390
34386
34438
34433
CAS No.
92-87-5
319-84-6
58-89-8
959-98-8
33213-65-9
72-20-8
17-6,1-6,
62-75-9
86-30-6
Meth-
od
605
608
608
608
608
608
612
607
607
»The proper chemical name is 2,2'-oxybis(1-ebloropropane).
•"See Section 1.2.
TABLE 4—CHROMATOGRAPHIC CONDITIONS, METHOD DETECTION LIMITS, AND CHARACTERISTIC
MASSES FOR BASE/NEUTRAL EXTRACTABLES
Parameter
1 ,3-Dich!orobenzene ,„..,„„...,..,.„„.....,,
1,2-DichIorobenzene ..,...,.,,. ,.,
Nitrobenzene ,.,„„., ,,„, ,.,., „,
Dimethyl phihalate .,,..,... ,.
2,6-Din!tfOto!uens .«..,,,,., >.,.., ,,
4~Chk>rophenyl phenyl ether ...,,.,..<....,„
2,4-Djratrololuene .............................
Diethyl phthalate
N-Nitrosodiphenylamine15 ......................
|}-BHCi>
4-Bromophenyl phenyl ether
i-BHC"
Phenanthrene
B-BHC
Reten-
tion time
(min)
7.4
7.8
8.4
8.4
8.4
9.3
11.1
11.4
11.8
11.9
12.1
12.2
13.9
15.9
17.4
17.8
18.3
18.7
19.5
19.5
19.8
20.1
20.5
21.0
21.1
21.2
22.4
22.8
22.8
23.4
Method
detec-
tion limit
0»*L)
1.9
4.4
1.6
5.7
1.9
5.7
1.9
0.9
1.9
2.2
1.6
5.3
1.9
3.5
1.9
1.6
1.9
1.9
4.2
5.7
1.9
1.9
1.9
1.9
5.4
1.9
4.2
Characteristic masses
Electron impact
Primary
146
146
117
93
146
45
130
77
225
180
82
128
93
237
162
152
154
163
165
186
204
165
149
169
284
183
248
183
178
178
181
Sec-
ondary
148
148
201
63
148
77
42
123
223
182
95
129
95
235
164
151
153
194
89
165
206
63
177
168
142
181
250
181
179
179
183
Sec-
ondary
113
113
199
95
113
79
101
65
227
145
138
127
123
272
127
153
152
164
121
167
141
182
150
167
249
109
141
109
176
176
109
Chemical ionization
Methane
146
146
199
63
146
"
124
223
181
139
129
65
235
163
152
154
151
183
166
183
177
169
284
249
178
178
Methane I Methane
I ^
148
201
107
148
135
152
225
183
167
157
107
237
191
153
155
163
211
167
211
223
170
286
251
179
179
150
150
203
109
150
137
164
227
209
178
169
137
239
203
181
183
164
223
195
223
251
198
288
277
207
207
219
-------
Pt 136, App. A, Mefh. 625
40 CFR Ch. I (7-1-04 Edition)
TABLE 4—CHROMATOGRAPHIC CONDITIONS, METHOD DETECTION LIMITS, AND CHARACTERISTIC
MASSES FOR BASE/NEUTRAL EXTRACTABLES—Continued
Parameter
Heptachlor ...... ........... . ........
S-BHC
Aldnn
OibutyJ phthalate
Heptachlor epoxide ...... ....
Dieldrki ...„...,..,.,..,.„, ...
44'-DDE ...... ... . .... .. .....
Endrin h
Endosulfan Hh ..,..»„,...„„.„,.„„..„„.„«.,.,
4 4'-DDD ......... ........ .
4 4'-DDT
Endosuttan sutfats ,.,. ,.,.... «„.,
Endrin aldehyde
Butyl benzyf phthalate
Bis(2-ethy1hexyl) phthalate
Chrysene ....... .,,„.,,„.-.. ......
Benzo(a)anthracen©
Benzo(b)fiuoranttiene
Benzo(k)fluQranth@r!0 ,..,..,.,.,.„.,...,..,„„..
lndeno{1 2,3-cd) pyrene <,.
Ghtordane*
PCB 1016C ,
PCS 1221C
PCB 1232«
PCB 1242« ,
PCB 1248"
PCB 1254=
PCB 1260«
Reten-
tion time
(min)
23.4
Z3.7
24,0
24.7
25.6
26.4
26.5
27.2
27.2
27.3
27.9
28.6
28.6
28.3
29,3
29.8
29.9
30,6
31.5
31.5
32.2
32,5
34.9
34.9
36.4
42.7
43.2
45,1
19-30
25-34
18-30
15-30
15-32
15-32
12-34
22-34
23-32
Method
detec-
tion limit
(H9/L)
1.9
3.1
1.9
2.5
2.2
2,2
2.5
5.6
1,9
2.6
44
4.7
5.6
2,5
2.5
2.5
7.8
18.5
2.5
4.8
2.5
2.5
3.7
2,5
4.1
30
36
Characteristic masses
Electron impact
Primary
100
183
66
149
353
237
202
79
248
202
81
237
235
184
235
272
67
149
149
228
228
252
149
252
252
252
276
278
276
42
373
159
224
190
190
224
294
294
330
Sec-
ondary
272
109
263
150
355
339
101
263
248
101
263
339
237
92
237
387
345
91
167
22S
229
254
253
253
253
138
139
138
74
375
231
260
224
224
280
330
330
362
Sec-
ondary
274
181
220
104
351
341
100
279
176
100
82
341
188
185
185
422
250
208
279
229
226
126
125
125
125
277
279
277
44
377
233
294
260
260
294
262
362
394
Chemical ionization
Methane
149
203
203
185
149
149
223
228
252
252
252
276
278
276
Methane
205
231
231
213
299
229
229
253
253
253
277
279
277
Methane
279
243
243
225
327
257
257
281
281
281
305
307
305
sThe proper chemical name is 2,2'-bisoxy(1-chloroprapane).
'See Section 1.2.
«These compounds are mixtures of various tamers (See Figures 2 through 12), Column conditions: Supeleoport (100/120
mesh) coated with 3% SP-2250 packed In a 1.8 m long x 2 mm ID glass column with helium canter gas at 30 mlAnin. flow rate.
Column temperature held isothermal at 50*C for 4 min., then programmed at 8°C/min. to 270°C and held for 30 min.
TABLE 5—CHROMATOGRAPHIC CONDITIONS, METHOD DETECTION LIMITS, AND CHARACTERISTIC
MASSES FOR ACID EXTRACTABLES
Parameter
2-Ch!orophenol
2 4-Dimethylphenol . .
2 4-Dinitrophenol
2-Methyl-4 6-dinltrophenol
Pentachlorooheno!
Reten-
tion time
(mini
5,9
6.5
8.0
9.4
9.8
11.8
13.2
15.9
16.2
17.5
Method
detec-
tion limit
(HS/D
3.3
3.6
1.5
2.7
2.7
2.7
3.0
42
24
3.8
Characteristic masses
Electron Impact
Primary
128
139
94
122
162
196
142
184
198
286
Sec-
ondary
64
65
65
107
164
198
107
63
182
264
Sec-
ondary
130
109
66
121
98
200
144
154
77
268
Chemical ionization
Methane
129
140
95
123
163
197
143
185
199
267
Methane
131
168
123
151
185
199
171
213
227
265
Methane
157
122
135
163
167
201
183
225
239
269
220
-------
Environmental Protection Agency
Pt. 136, App. A, Meth, 625
TABLE 5—CHROMATOGRAPHIC CONDITIONS, METHOD DETECTION LIMITS, AND CHARACTERISTIC
MASSES FOR ACID EXTRACTABLES—Continued
Reten-
tion time
(minj
Method
detec-
tion limit
(Mi/I-)
Characteristic masses
Electron Impact
Primary
Sec-
ondary
Sec-
ondary
Chemical ionization
Methane Methane Methane
4-Nitrophenol.
20.3
139
109
Column conditions: Sypelcoport (100/120 mesh) coated with 1% SP-124GDA packed in a 1-8 m long x 2mm ID glass column
with helium carrier gas at 30 mUmin. flow rate. Column temperature held isothermal at 70 °C for 2 min. then programmed at 8
°C/min. to 200 °C.
TABLE 6—QC ACCEPTANCE CRITERIA—METHOD 625
Parameter
Test conclu-
sion (jig/L)
Limits for s
Range for
Range for
P, Pt (Per-
cent)
Acenaphthene
Acenaphthylene
Aldrin
Anthracene
Benzo(a)anthracene
Benzo^b)fluoranthene
Benzo(k)fluoranttiene
Benzofajpyrene
Benzo(gni)perylene
Benzyl butyl phtfialate
(J-BHC
S-BHC
Bis(2-chloroethyl) ether
Bls(2-chloroethoxy)methane
Bis(2-chloroisopropyl) ether*
Bis(2-ethylhexyl) phthalate
4-Brornophenyl phenyi ether
2-Chloronaphthalene
4-Chlorophenyl phenyi ether
Chrysene
4,4'-DDD
4,4'-DDE
4,4'-DOT
Dibenzo(a,h)anthfacane
Di-n-butyl phthalate
1,2-Dichlorobenzene
1,3-Dichforobenzene
1,4,-Dichlorobenzene
3,3'-Dhlorobenzidine
Diefdrin
Diethyl phthalate
Dimethyl phthalate
2,4-Dlnitrotoluene
2,6-Dinitrotoluene
Di-n-octyl phthalate
Endosuffan suffate
Endrin aldehyde
Fluoranthene .
Fiuorene
Heptachlor
Heptachlor epoxide
Hexachlorobenzene
Hexachlorobutadiene
Hexachioroethane
lndeno(1,2,3-cd)pyrene
Isophorone
Naphthalene
Nitrobenzene
N-Nitrosodi-n-propylamine
PCB-1260
Phenanthrene
Pyrene
1,2,4-Triehlorobenzene
4-Chloro-3-methytphenoi
2-Chlorophenol
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100 |
100 I
27.6
40.2
39.0
32.0
27.6
38.8
32.3
39.0
58.9
23.4
31.5
21.8
55.0
34.5
46.3
41.1
23.0
13.0
33.4
48.3
31.0
32.0
61.6
70.0
16.7
30.9
41.7
32.1
71.4
30.7
26,5
23.2
21.8
29.6
31.4
16.7
32.5
32.8
20.7
37.2
54.7
24.9
26.3
24.5
44.6
63.3
30.1
39.3
55.4
54.2
20.6
25.2
28.1
37.2
28.7
60.1-132.3
53.5-126.0
7.2-152.2
43.4-118.0
41.8-133.0
42.0-140.4
25.2-145.7
31.7-148.0
D-195,0
D-139.9
41.5-130.6
D-100.0
42.9-126.0
49.2-164.7
62.8-138.6
28.9-136.8
64.9-114.4
64.5-113.5
38.4-144.7
44.1-139.9
D-134.5
19.2-119,7
D-170.6
D-199.7
8.4-111.0
48,6-112.0
16.7-153.9
37.3-105.7
8.2-212.5
44.3-119.3
D-100.0
D-100.0
47.5-126.9
68.1-136.7
18-6-131.8
D-103.5
D-188.8
42.9-121.3
71.6-108.4
D-172.2
70.9-109.4
7.8-141.5
37.8-102.2
55.2-100.0
D-150.9
46.6-180-2
35.6-119.6
54.3-157.6
13.6-197.9
19.3-121.0
65.2-108.7
69.6-100.0
57.3-129.2
40.8-127.9
36.2-120.4
47-145
33-145
D-166
27-133
33-143
24-159
11-162
17-163
D-219
D-152
24-149
D-110
12-158
33-184
36-166
8-158
53-127
60-118
25-158
17-168
D-145
4-136
D-203
D-227
1-118
32-129
D-172
20-124
D-262
29-136
D-114
D-112
39-139
50-158
4-146
D-107
D-209
26-137
59-121
D-192
26-155
D-152
24-116
40-113
D-171
21-196
21-133
35-180
D-230
D-164
54-120
52-115
44-142
22-147
23-134
221
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
TABLE &—QC ACCEPTANCE CRITERIA—METHOD 625—Continued
Parameter
2,4-Dirnelhylphenol
2-Methyf-4,6-dinttrophenQl
4-NftrophsneJ ,
2,4.6-TrichloroDhenol
Test conclu-
sion (ng/Lj
100
100
100
100
100
100
100
100
100
Limits for s
0*L)
264
26.1
498
93.2
352
47.2
489
226
31.7
Range for
Xlngfl.)
525-121.7
41.8-109.0
D-172,9
53.0-100.0
45 0-166,7
13.0-106.5
38 1-151 8
166-100.0
52.4-129.2
Range for
P, P, (Per-
cent)
39-135
32-119
D-191
D-181
29-1 82
D-132
14-176
5-112
37-144
S=Standard deviation for four recovery measurements, in ^g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in nd/L (section 8.2.4).
P, P,=Percent recovery measured (Section 8.3.2, Section 8.4.2).
D=Detected; result must be greater than zero.
NOTC: These criteria are based directly upon the method performance data in Table 7. Where necessary, the limits for recov*
ery have been broadened to assure applicability of the lirnts to concentrations below those used to develop Table 7.
"The proper chemical name is 2,2'oxybis(1-chloroprapane).
TABLE 7—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 625
Parameter
Aldrin
Benzo(k)fluoranthene
Benzyl butyl phthalate
(S-BHC ,.
8-BHC
Bis(2-chloroethyl) ether
44'-DDD .. ...
4,4'-DDE
44'-DDT . ..
Diethyl phthalate
2,4-DirtitrotQluene
Naohthalene
Accuracy, as
recovery, X'
(|ig/U
0,96C=0.19
0.890=0.74
0 78C-1 66
0800=068
0,880-060
0.9X-1.80
0.87C-1.56
0900-0 13
0.98C-0.86
0.660-1.68
087C-094
0.29C-1.09
0.86C-1.54
1.12C-5.04
1.03C-231
O.B4C-1.18
0910-1 34
0.89C=0.01
0.91C-0.53
0.93C-1.00
0.56C-0.40
0.70C-0.54
0.79C-328
0.88C-4.72
0.59C=0 71
0.80C=0.28
086C-070
073C-1 47
1.23C- 12.65
0.82C-0.16
0.43C=1.00
0.200=1.03
0.920-4.81
1.060-360
0.76C-0.79
0.39C=0.41
0760-386
0810=1 10
0.90C-0.00
0.87C-2.97
0.92C-1.87
0 74C=0.66
0.71C-1.01
0.73C-0.83
078C-3 10
1.12C-1.41
0.76C=1.58
Single analyst
precision, sr'
(W/L)
0.15X-0.12
0 24X - 1 06
027X-1 28
021X-032
0.15X=093
0.22X=0.43
0.19X=1.03
0,22X=Q 48
0.29X=2.40
0,18X=0.94
0.20X-058
0.34X=0.86
0.35X-0.99
0.16X=1.34
0.24X=0 28
0.26X=0.73
013X-0.66
0.07X-0.52
0.20X-0.94
0.28X=0.13
0.29X-0.32
0.26X-1.17
0.42X=0.19
0.30X=8.51
0 13X=1 16
0.20X=0.47
0 25X=0 68
0 24X=0.23
0.28X=7.33
0.20X-0.16
0.28X=1.44
0.54X=0.19
0.12X-1.06
014X=1 26
0.21X=1.19
0.12X=2.47
0 18X=391
022X-0.73
0.12X=0.26
0.24X-0.56
0.33X-0.46
0.18X-0.10
0.19X=0.92
0.17X=0.67
029X=1.46
0.27X=0.77
0.21X-0.41
Overall preci-
sion, S' (ng/L)
0.21 X- 0.67
026X-0.54
043X=1 13
027X-064
026X-028
0.29X=0.96
0.35X=0.40
0.32X=1 .35
0.51 X- 0.44
0,53X=0,92
0 SOX- 1.94
0.93X-0.17
0.35X=0.10
0.26X=2.01
0 25X=1 04
0.36X=0.67
0.16X=0,66
0.13X=0.34
0.30X-0.46
0.33X-0.09
0.66X-0.96
0.39X-1.04
0.65X-0.58
0.59X=0.25
0.39X=0.60
0.24X=0.39
041X=0 11
0.29X=0.36
0.47X=3.45
0.26X-0.07
0.52X=0.22
1.05X-0.92
0.21X=1.50
0.19X=0.35
0.37X-1.19
0.63X-1.03
073X-0.62
0.28X-0.60
0.13X=0.61
0.50X-0.23
0.28X=0.64
0.43X-0.52
0.26X-0.49
0.17X=0.80
0.50X=0.44
0.33X=0.26
0.30X-0.68
222
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
TABLE 7—METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATION—METHOD 625-
Continued
Parameter
N-Nitrosodi-n-propylamine
PCB-1260
2-Chforophenol
2-Methyl-4,6-Dinitrophenol
2-Nitrophenol ,
4-Nitrophenol ,
Phenol
2,4.6-TrichlorophenoI ,
Accuracy, as
recovery, X'
(M9"-)
1.09C-3.05
1.12C-6.22
0.810-10,86
0.87C - 0.06
0.84C-0.16
0.94C-0.79
0 84C-0 35
0.78C=0.29
0.87C=0.13
071C=441
081C-1804
1.04C-2B.04
1.07C-1.15
0.61C-1.22
0.93C-1 .99
0.43C=1,26
0.91C-0.18
Single analyst
precision, s,'
(M9/U
0.19X-0.92
0.27X=Q,68
0.35X=3.61
0.12X=0.57
0.16X=0.06
0.15X-0.85
0 23X-0 75
0.18X=1.46
0.15X=1.25
0 16X=1 21
0.38X=2 36
0.05X-42.29
0.16X=1.94
0.38X=2.57
0.24X-3.03
Q.26X=0.73
0.16X=2.22
Overall preci-
sion, S' (fig/L}
0.27X-0.21
0.44X=0.47
0.43X=1.82
0.15X-0.25
0.15X=0.31
0.21X-039
029X=1 31
0.28X=0,97
0.21X^1.28
0 22X-1 31
0.42X=26 29
0.26X-2310
0.27X=2.60
0.44X=3.24
0 30X-4 33
0.35X-0.58
0.22X=1.81
X'=Expected recovery for one or more measurements of a sample containing a concentration of C, in ug/U.
s/=Expecfed single analyst standard deviation of measurements at an average concentration found of Xt in n
S'= Expected interiaboratory standard deviatton of measurements at an average concentration found of X, in
C- True value for the concentration, in jig/L,
X= Average recovery found for measurements of samples containing a concentration of C, in ^ig/L
!iThe proper chemical name is 2,2)oxybis(l-chioropropane),
TABLE 8—SUGGESTED INTERNAL AND
SURROGATE STANDARDS
Base/neutral fraction
Anilsne-ds ..,.,.,„,.........,,....,...,.
Anthracene-djo ..,..„.,.„
Benzo(a)anthracene-d,2
4,4'-Dibromobiphenyl
4,4'-
Dibromooctafiuorobiphenyl,
CtecafSuorobiphenyl ..,.,.,,,..
S^^Difiuorobiphenyi
4-Fluoroaniline ,
1-Fiuoronaphthalene ..,,,,..,
2-Fiuoronaphthalene ,.,.,..,.,.,.
Naphthalene-dw -
Nitrobenzene-ds , .,.,. .,
2,3,4,5,8-Pentafiuorobiphenyi
Phenanthrene-dm
Pyridine-ds ,.........,,...
Acid fraction
2-Fiuorophenol.
Pentafluorophenol.
Phenol-ds
2-Perfluoromethyl phenol-
TABLE 9—DFTPP KEY MASSES AND
ABUNDANCE CRITEFHA
, j m/2 Abundance criteria
70
127
197
198
199
275
365
441
442
443
30-60 percent oi mass 198.
Less than 2 percent of mass 69,
Less than 2 percent of mass 69.
40-60 percent of mass 198.
Less than 1 percent of mass 198.
Base peak, 100 percent relative abundance.
6-9 percent of mass 198.
10-30 percent of mass 198.
Greater than 1 percent of mass 198.
Present but less than mass 443,
Greater than 40 percent of mass 198,
17-23 percent of mass 442.
223
-------
•n
5'
3
6>
1
I
tt
e
3)
O
£
2;CHLOROPHENOL §
24IITROPHENQL
PHENOL
S"1
0*1
—j
m
s
2,4-DICHLOROPHENOL
2,4,6-TMCHLOTOPHENOl
4-CHLORO-3-METHYLPHENOL
4-M1TROPHENOL
i-
r- 2,4-DINITROPHENOL
2-METHVL-4,6-DINITROPHENOL
PENTACHLOBOPHENOL
.U-DICHLOROBINZINE
'. 1,4-WCMLOBOBgNZiNI
• 1.2-DICHLOBOBENZENt -V HtXACHLOBOETHANE
BISB-CMLOBOISOPROPrUETHEB + «ISI2-CMLOROETM1fUEtMER
, HEX ACHUWOBUTAOIEME
ACENAPHTHENE
DIMETHYL PHTHALATE
4-CHLOBOPMENYL PHENYL ETWER
f OfETHYlFHTHALATE
_ - HEXACHLOROBENZENE \ 4- LI-DIPHENYLHYORAZtME
^BBOMOPHiNYl PHENVL ETMUR
PHENANTHHENE t ANTHRACENE
3
i
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
COLUMN: 3% SP-2250 ON SUPaCOPORT
PROGRAM: 50°C FOR 4 WIN, 8»C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
a
a
a
i
o
a
a
a
a
o
Q
Q
s
w
10 15 20
RETENTION TIME, MIN.
25
30
Figure 3. Gas chromatogram of pesticide fraction.
225
-------
Pt. 136, App. A, Meth. 625
COLUMN: 3% SP-2250 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN, 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
40 CFR Ch.! (7-1-04 Edition)
20
32
34
22 24 26 28 30
RETENTION TIME, MIN.
Figure 4. Gas chromatogram of chlordane.
36
226
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
COLUMN; 3% SP-2210 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN. 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
34
36 38
RETENTION TIME, MIN.
Figure 5. Gas chromatogram of toxaphene.
227
-------
Pt. 136, App. A, Melil. 625
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 3% SP-22BO ON SUPELCOPORT
PROGRAM: 50°C FOR 4 WIN, 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
18 20 22 24 26 28 30 32
RETENTION TIME, M1N.
Figure 6. Gas chromatogram of PCB-1016.
228
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
COLUMN: 3% SP-22SO ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN, 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
18 20 22 24 26 28 30
RETENTION TIME, MIN.
Figure 7. Gas chromatogram of PCB-1221.
229
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Idiflon)
COLUMN: 3% SP-2250 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN, 8°C/M1N TO 270°C
DETECTOR: MASS SPECTROMETER
m/z-3S TO 4SO
18 20 22 24 26 28 30 32
RETENTION TIME, MIN.
Figure 8. Gas chromatogram of PCB-1232.
230
-------
Environmental Protection Agency
COLUMN: 3% SP-2250 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 WIN. 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
Pt. 136, App. A, Meth. 625
m/z-35 TO 450
18 30 22 24 26 28 30 32
RETENTION TIME, MIN.
Figure 9. Gas chromatogram of PCB-1242.
231
-------
ft. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 3% SP-2210 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN. 8°C/MIN TO 270°C
DETECTOR: MASS SPECTROMETER
20 22 24 26 28 30
RETENTION TIME, MIN.
32
Figure 10. Gas chromatogram of PCB-1248.
232
-------
Environmental Protection Agency
Ft. 136, App. A, Metti. 625
COLUMN: 3% SP-22SQ ON SUPELCOPORT
PROGRAM: 50°C FOR 4 MIN. 8°C/M!N TO 270°C
DETECTOR: MASS SPECTROMETER
^m/z-3ST0450 _ ^ jJW
m/z-362
m/z-330
m/z-294
IB 20 22 24 26 28 30 32
RETENTION TIME, MIN,
34
36
38
Figure 11. Gas chromatogram of PCB-1254.
233
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
COLUMN: 3% SP-2250 ON SUPELCOPORT
PROGRAM: 50°C FOR 4 WIN, 8°C/M1N TO 270°C
DETECTOR: MASS SPECTROMETER
is
22
24 26 28 30 32
RETENTION TIME, MIN.
Figure 12. Gas chromatogram of PCB-1260.
36
38
234
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 625
TAILING FACTOR= —
AB
Example calculation: Peak Heights DE = 100mm
10% Peak Height = BD = 10 mm
Peak Width at 10% Peak Height = AC = 23mm
AB = 11 mm
BC = 12mm
Therefore: Tailing Factors— =1.1
11
Figure 13. Tailing factor calculation.
235
-------
Pt. 136, App. A, Meth. 625
40 CFR Ch. I (7-1-04 Edition)
ATTACHMENT 1 TO METHOD 625
INTRODUCTION
To support measurement of several
semivolatile pollutants, EPA has developed
this attachment to EPA Method 625.1 The
modifications listed in this attachment are
approved only for monitoring wastestreams
from the Centralized Waste Treatment Point
Source Category (40 CFR Part 437) and the
Landfills Point Source Category (40 CPR
Part 445). EPA Method 625 (the Method) in-
volves sample extraction with methylene
chloride followed by analysis of the extract
using either packed or capillary column gras
ehromatography/mass speotrometry (G-C/
MS), This attachment addresses the addition
of the semivolatile pollutants listed in Ta-
bles 1 and 2, to all applicable standard,
stock, and spiking solutions utilized for the
determination of semivolatile organic com-
pounds by EPA Method 625.
1,0
EPA METHOD 625 MODIFICATION
SUMMARY
The additional semivolatile organic com-
pounds listed in Tables 1 and 2 are added to
all applicable calibration, spiking, and other
solutions utilized in the determination of
base/neutral and acid compounds by EPA
Method 625. The instrument is to be cali-
brated with these compounds, using a cap-
illary column, and all procedures and quality
control tests stated in the Method must be
performed.
2.0 SECTION MODIFICATIONS
NOTE: All section and figure numbers in
this Attachment reference section and figure
numbers in EPA Method 625 unless noted
otherwise. Sections not listed here remain
unchanged.
Section 6,7 The stock standard solutions de-
scribed in this section are modified such
that the analytes in Tables 1 and 2 of this
attachment are required in addition to
those specified in the Method.
Section 7.2 The calibration standards de-
scribed in this section are modified to in-
clude the analytes in Tables 1 and 2 of
this attachment.
Section 8.2 The precision and accuracy re-
quirements are modified to include the
analytes listed in Tables 1 and 2 of this
attachment. Additional performance cri-
teria are supplied in Table 5 of this at-
tachment.
Section 8.3 The matrix spike is modified to
include the analytes listed in Tables 1
and 2 of this attachment.
Section 8.4 The QG check standard is modi-
fied to include the analytes listed in Ta-
bles 1 and 2 of this attachment. Addi-
tional performance criteria are supplied
in Table 5 of this attachment.
Section 16.0 Additional method perform-
ance information is supplied with this at-
tachment.
TABLE 1—BASE/NEUTRAL EXTRACTABLES
Parameter
acetophenone ' ....,..,,
carbazole * -
2,3-dichioroaniIine * ...,„.,„.,......,, ...,...,,
Dvridine- ,.,....,....„,....,..,
CAS No.
98~-8&-2
98-55-5
§2-53-3
86-74-8
35_48_7
124-18-5
608-27-5
593-45-3
110-86-1
CAS « Chemical Abstracts Registry.
1 Analysis of this pollutant is approved only for the Central-
ized Waste Treatment industry-
2 Analysis of this pollutant is approved only for the Central-
ized Waste Treatment and Landfills industries.
3 Analysis of this pollutant is approved only for the Landfills
industry.
TABLE 2—ACID EXTRACTABLES
Parameter
CAS No.
p-cresol1 106-44-5
CAS = Chemical Abstracts Registry,
1 Analysis of this pollutant is approved only for the Central-
ized Waste Treatment and Landfills industries.
TABLE 3—CHROMATOGRAPHIC CONDITIONS,1 METHOD DETECTION LIMITS (MDLs)p AND
CHARACTERISTIC M/Z'S FOR BASE/NEUTRAL EXTRACTABLES
Anaiyte
Bis{2-chioroethyl)ether .
1 ,4-Dichlorobenzene
1 .2-Dichlorobenzene
Retention
time
(min)2
4.93
4.95
10.82
10.94
11.11
11.47
11.62
12.17
MDL
(WU
4.6
3.3
5.0
Characteristic m/z's
Electron impact
Primary
79
42
93
93
57
146
146
146
Secondary
52
74
66
148
148
148
Secondary
51
44
65
113
113
113
1 EPA Method 625: Base/Neutrals and Acids,
40 CFR Part 136, Appendix A.
236
-------
Environmental Protection Agency
R. 136, App. A, Meth. 625
TABLE 3—CHROMATOGRAPHIC CONDITIONS, 1 METHOD DETECTION LIMITS (MDLs), AND
CHARACTERISTIC M/Z'S FOR BASE/NEUTRAL EXTRACTABLES—Continued
Aralyte
3,3'-Dichlorobenzidine
Bis(2-ethvl hexyl)phthalate
Benzo(b)fluoranthene .,
Dibenzo(a.h) anthracene
BsnzoCahitoervlene
Retention
time
(minp
12.48
12.51
12.88
12.97
13.08
13.40
14.11
14.82
15.37
15.55
1S.56
16.12
18,47
18.82
18.35
20.48
20.69
20.73
21.30
22.00
22.74
22.90
22.92
23.35
24.44
24.93
25.39
25.98
26.12
26.66
27.84
29.82
30.26
30.56
32.63
34.28
34.33
34.36
34,44
36.17
37.90
37.97
39.17
44.91
45.01
46.56
MDL
(H9/L)
4.7
3A
5.0
2.5
2.0
4.0
Characteristic m/z's
Electron impact
Primary
108
45
105
130
117
77
82
93
180
59
128
225
237
161
162
163
152
165
154
165
149
204
166
169
248
284
57
178
178
167
149
202
184
202
149
252
228
149
228
149
252
252
252
278
276
276
Secondary
107
77
77
42
201
123
95
95
182
129
223
235
163
164
194
151
89
153
63
177
206
165
168
250
142
179
179
150
101
92
101
91
254
229
167
226
253
253
253
139
138
138
Secondary
79
79
51
101
199
65
138
123
145
127
227
272
90
127
164
153
121
152
182
150
141
167
167
141
249
176
176
104
100
185
100
206
126
226
279
229
125
125
125
279
277
277
1 The data presented in this table were obtained under the following conditions:
Column—30 ±5 meters x 0.25 ±.02 mm i.d., 94% msihyl, 5% phenyl, 1% vinyl, bonded phase fused silica capillary column
(DB-5).
Temperature program—Five minutes at 30 °C; 30-280 °C at 8 °C per minute; isothermal at 280 ">C until benzo(ghi)perylene
elutes.
Gas velocity—3Q±5 cm/sec at 30 °C.
2Retention times are from Method 1625, Revision C, using a capillary column, and are intended to be consistent for all
analyles in Tables 4 and 5 of this attachment.
3 Analysis of this pollutant Is approved only for the Centralized Waste Treatment and Landfills industries.
4 Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
TABLE 4—CHROMATOQRAPHIC CONDITIONS,1 METHOD DETECTION LIMITS (MDLs), AND
CHARACTERISTIC M/Z'S FOR ACID EXTRACTABLES
Analyte
2-Chlorophenol
Retention
time2
(min)
10.76
11.08
MDL
WU
Characteristic m/z's
Electron impact
Primary
94
128
Secondary
65
64
Secondary
66
130
237
-------
Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
TABLE 4—CHROMATOGRAPHIC CONDITIONS, 1 METHOD DETECTION LIMITS (MDLs), AND
CHARACTERISTIC M/Z'S FOR ACID EXTRACTABLES—Continued
Anafyte
2-Nitrophenol ,
2,4-DimethylphenoI ,.,,...,..>„.,.. ,,,..„., ,,..,„,...„,..
PentachloroDheno! ...,...,...,...,...„....,.>.„,.,........,.,.,.,...,...
Retention
time2
(min)
12.92
14.38
14,54
15.12
1683
18,80
21.51
21 77
2283
25,52
MDL
(M-9/L)
Characteristic m/z's
Electron impact
Primary I Secondary
108
139
122
107
65
107
162 ' 164
142 i 107
196
184
65
198
198
63
139
182
Secondary
77
109
121
98
144
200
154
109
77
266 264 | 268
1 The data presented in this table were obtained under the following conditions:
Column—30 ±5 meters x 0,25 +.02 mm i,d., 94% methyl, 5% phenyl, 1% vinyl silicone bonded phase fused silica capillary col-
umn (DB-5).
Temperature program—Five minutes at 30 °C; 30-280 "C at 8 °C per minute; isothermal at 280 f!C until b@nzo(ghi)peryiene
elutes.
Gas velocity—30 ±5 cm/sec at 30 °C
2 Retention times are from EPA Method 1625, Revision C, using a capillary column, and are intended to be consistent for ail
analyfes in Tables 3 and 4 of this attachment,
3Anaiysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries,
TABLE 5—QC ACCEPTANCE CRITERIA
Analyte
Test conclu-
sion
(ng/L)
100
100
100
100
100
100
100
100
100
100
Limits for s
(ngfl-)
51
4?
71
17
23
22
70
13
10
ns
Range for X
ftig/L)
23-254
46-163
1S-278
79-1 1 1
30-146
11-617
D-651
40-160
52-147
7-392
Range for
P, P,(%)
61-144
58-156
46-134
73-131
55-126
76-107
D-ns
68-134
65-123
33-158
s = Standard deviation for four recovery measurements, in jiq/L (Section 8.2)
X - Average recovery for four recovery measurements in ^g/L (Section 8.2)
P.Ps = Percent recovery measured (Section 8,3, Section 8.4)
D - Detected; result must be greater than zero,
ns = no specification; limit is outside the range that can be measured reliably,
1 Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
2 Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries
METHOD 1613. REVISION B
Tetra- Through Octa-Chlorinated Dioxins and
Furam by Isotope Dilution HRGC/HRMS
1.0 Scope and Application
1.1 This method Is for determination of
tetra- through octa-chlorinated dibenzo-p-
dioxins (CDDs) and dibenzofnrans (CDFs) In
water, soil, sediment, sludge, tissue, and
other sample matrices by high resolution gas
ehromatogTaphy/high resolution mass spee-
trometry (HRGC/HRMS). The method is for
use in EPA's data gathering and monitoring'
programs associated with the Clean Water
Act, the Resource Conservation and Recov-
ery Act, the Comprehensive Environmental
Response, Compensation and Liability Act,
and the Safe Drinking Water Act. The meth-
od Is based on a compilation of EPA, indus-
try, commercial laboratory, and academic
methods (References 1-6).
1,2 The seventeen 2,3,7,8-snbstltuted
CDDs/CDFs listed In Table 1 may be deter-
mined by this method. Specifications are
also provided for separate determination of
2,3,7,8-tetrachloro-dibenzo-p-dioxin (2,3,7,8-
TCDD) and 2,3,7,8-tetrachloro-dibenzofuran
(2,3,7,8-TCDP).
1.3 The detection limits and quantitation
levels in this method are usually dependent
on the level of Interferences rather than in-
strumental limitations. The minimum levels
(MLs) in Table 2 are the levels at which the
CDDs/CDFs can be determined with no Inter-
ferences present. The Method Detection
238
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
Limit (MDL) for 2,3,7,8-TCDD has been deter-
mined as 4.4 pgfLi (parts-per-quadrlllion)
using this method,
1.4 The GC/MS portions of this method
are for use only by analysts experienced with
HBGC/HRMS or under the close supervision
of such qualified persons. Each laboratory
that uses this method must demonstrate the
ability to generate acceptable results using
the procedure in Section 9.2.
1.5 This method is "performance-based".
The analyst is permitted to modify the
method to overcome interferences or lower
the cost of measurements, provided that all
performance criteria in this method are met.
The requirements for establishing method
equivalency are given in Section 9.1.2.
1.6 Any modification of this method, be-
yond those expressly permitted, shall be con-
sidered a major modification subject to ap-
plication and approval of alternate test pro-
cedures under 40 CPB 136.4 and 136.5.
2,0 Summary of Method
Plow charts that summarize procedures for
sample preparation, extraction, and analysis
are given in Figure 1 for aqueous and solid
samples, Figure 2 for multi-phase samples,
aad Figure 3 for tissue samples.
2.1 Extraction.
2.1.1 Aqueous samples (samples con-
taining less than 1% solids)—Stable
isotopically labeled analogs of 15 of the
2,3,7,8-substituted CDDs/CDFs are spiked
into a 1 L sample, and the sample is ex-
tracted by one of three procedures:
2.1.1.1 Samples containing no visible par-
ticles are extracted with methylene chloride
in a separatory funnel or by the solid-phase
extraction technique summarized in Section
2.1.1.3. The extract is concentrated for clean-
up.
2.1.1.2 Samples containing visible par-
ticles are vacuum filtered through a glass-
fiber filter. The filter is extracted in a Soxh-
let/Dean-Stark (SDS) extractor (Reference
7), and the filtrate is extracted with meth-
ylene chloride in a separatory funnel. The
methylene chloride extract is concentrated
and combined with the SDS extract prior to
cleanup.
2.1.1.3 The sample is vacuum filtered
through a glass-fiber filter on top of a solid-
phase extraction (SPE) disk. The filter and
disk are extracted in an SDS extractor, and
the extract is concentrated for cleanup.
2.1.2 Solid, semi-solid, and multi-phase
samples (but not tissue)—The labeled com-
pounds are spiked into a sample containing
10 g (dry weight) of solids. Samples con-
taining multiple phases are pressure filtered
and any aqueous liquid is discarded. Coarse
solids are ground or homogenized. Any non-
aqueous liquid from multi-phase samples is
combined with the solids and extracted in an
SDS extractor. The extract is concentrated
for cleanup.
2.1.3 Fish and other tissue—The sample is
extracted by one of two procedures:
2.1.3.1 Soxhlet or SDS extraction—A 20 g
aliquot of sample is homogenized, and a 10 g
aliquot is spiked with the labeled com-
pounds. The sample is mixed with sodium
sulfate, allowed to dry for 12-24 hours, and
extracted for 18-24 hours using methylene
chloride:hexane (1:1) in a Soxhlet extractor.
The extract is evaporated to dryness, and the
lipid content is determined.
2.1.3.2 HC1 digestion—A 20 g aliquot is ho-
mogenized, and a 10 g aliquot is placed in a
bottle and spiked with the labeled com-
pounds. After equilibration, 200 mL of hydro-
chloric acid and 200 mL of methylene chlo-
rideihexane (1:1) are added, and the bottle is
agitated for 12-24 hours. The extract is evap-
orated to dryness, and the lipid content is
determined.
2.2 After extraction, }7Cl4-labeled 2,3,7,8-
TCDD is added to each extract to measure
the efficiency of the cleanup process. Sample
cleanups may include back-extraction with
acid and/or base, and gel permeation, alu-
mina, silica gel, Florisil and activated car-
bon chromatography. High-performance liq-
uid chromatography (HPLC) can be used for
further isolation of the 2,3,7,8-isomers or
other specific isomers or congeners. Prior to
the cleanup procedures cited above, tissue
extracts are cleaned up using an anthropo-
genic isolation column, a batch silica gel ad-
sorption, or sulfurie acid and base back-ex-
traction, depending on the tissue extraction
procedure used.
2.3 After cleanup, the extract is con-
centrated to near dryness. Immediately prior
to injection, internal standards are added to
each extract, and an aliquot of the extract is
injected into the gas chromatograph. The
analytes are separated by the GC and de-
tected by a high-resolution (210,000) mass
spectrometer. Two exact m/z's are monitored
for each analyte.
2.4 An individual CDD/CDF is identified
by comparing the GC retention time and ion-
abundance ratio of two exact m/z's with the
corresponding retention time of an authentic
standard and the theoretical or acquired ion-
abundance ratio of the two exact m/z's. The
non-2,3,7,8 substituted isomers and congeners
are identified when retention times and ion-
abundance ratios agree within predefined
limits. Isomer specificity for 2,3,7,8-TCDD
and 2,3,7,8-TCDF is achieved using GG col-
umns that resolve these isomers from the
other tetra-isomers.
2.5 Quantitative analysis is performed
using selected ion current profile (SICP)
areas, in one of three ways:
2.5.1 For the 15 2,3,7,8-substituted CDDs/
CDFs with labeled analogs (see Table 1), the
GC/MS system is calibrated, and the con-
centration of each compound is determined
using the isotope dilution technique.
239
-------
Pf. 136, App, A, Mem. 1613
40 CFR Ch. I (7-1-04 Edition)
2.5,2 For 1,2,3,7,8,9-HxCDD, OCDF, and the
labeled compounds, the GC/MS system Is
calibrated and the concentration of each
compound is determined using the internal
standard technique.
2.5.3 For non-2,3,7,8-substituted isomers
and for all isomers at a given level of
ehlorination (i.e., total TODD), concentra-
tions are determined using response factors
from calibration of the CDDs/CDFs at the
same level of cMorination.
2.6 The quality of the analysis is assured
through reproducible calibration and testing
of the extraction, cleanup, and GC/MS sys-
tems.
3.0 Definitions
Definitions are given in the glossary at the
end of this method.
4,0 Contamination and Interferences
4.1 Solvents, reagents, glassware, and
other sample processing hardware may yield
artifacts and/or elevated baselines causing
misinterpretation of chromatograms (Ref-
erences 8-9). Specific selection of reagents
and purification of solvents by distillation in
all-glass systems may be required. Where
possible, reagents are cleaned by extraction
or solvent rinse.
4.2 Proper cleaning of glassware is ex-
tremely important, because glassware may
not only contaminate the samples but may
also remove the analytes of interest by ad-
sorption on the glass surface.
4.2.J Glassware should be rinsed with sol-
vent and washed with a detergent solution as
soon after use as is practical. Sonioation of
glassware containing a detergent solution
for approximately 30 seconds may aid in
cleaning. Glassware with removable parts,
particularly separatory funnels with
fluoropolymer stopcocks, must be disassem-
bled prior to detergent washing.
4.2.2 After detergent washing, glassware
should be rinsed immediately, first with
methanol, then with hot tap water. The tap
water rinse is followed by another methanol
rinse, then acetone, and then methylene
chloride.
4.2.3 Do not bake reusable glassware in an
oven as a routine part of cleaning. Baking
may be warranted after particularly dirty
samples are encountered but should be mini-
mized, as repeated baking of glassware may
cause active sites on the glass surface that
will irreversibly adsorb CDDs/CDFs.
4.2.4 Immediately prior to use, the Soxh-
let apparatus should be pre-extracted with
toluene for approximately three hours (see
Sections 12.3.1 through 12.3,3). Separatory
funnels should be shaken with methylene
chloride/toluene (80/20 mixture) for two min-
utes, drained, and then shaken with pure
methylene chloride for two minutes.
4.3 All materials used in the analysis
shall be demonstrated to be free from inter-
ferences by running reference matrix method
blanks initially and with each sample batch
(samples started through the extraction
process on a given 12-hour shift, to a max-
imum of 20 samples).
4.3,1 The reference matrix must simulate,
as closely as possible, the sample matrix
under test. Ideally, the reference matrix
should not contain the CDDs/CDFs in detect-
able amounts, but should contain potential
interferents in the concentrations expected
to be found in the samples to be analyzed.
For example, a reference sample of human
adipose tissue containing
pentachloronaphthalene can be used to exer-
cise the cleanup systems when samples con-
taining pentachloronaphthaleae are ex-
pected.
4.3.2 When a reference matrix that simu-
lates the sample matrix under test is not
available, reagent water (Section 7.6.1) can
be used to simulate water samples; play-
ground sand (Section 7.6.2) or white quartz
sand (Section 7.3.2) can be used to simulate
soils; filter paper (Section 7.6.3) can be used
to simulate papers and similar materials;
and corn oil (Section 7.6,4) can be used to
simulate tissues.
4.4 Interferences coextracted from sam-
ples will vary considerably from source to
source, depending on the diversity of the site
being sampled. Interfering compounds may
be present at concentrations several orders
of magnitude higher than the CDDs/CDFs.
The most frequently encountered inter-
ferences are chlorinated biphenyls, methoxy
biphenyls, hydroxydiphenyl ethers,
benzylphenyl ethers, polynuclear aromatics,
and pesticides. Because very low levels of
CDDs/CDFs are measured by this method,
the elimination of interferences is essential.
The cleanup steps given in Section 13 can be
used to reduce or eliminate these inter-
ferences and thereby permit reliable deter-
mination of the CDDs/CDFs at the levels
shown in Table 2.
4.5 Each piece of reusable glassware
should be numbered to associate that glass-
ware with the processing of a particular sam-
ple. This will assist the laboratory in track-
ing possible sources of contamination for in-
dividual samples, identifying glassware asso-
ciated with highly contaminated samples
that may require extra cleaning, and deter-
mining when glassware should be discarded.
4.6 Cleanup of tissue—The natural lipid
content of tissue can interfere in the anal-
ysis of tissue samples for the CDDs/CDFs.
The lipid contents of different species and
portions of tissue can vary widely. Ldpids are
soluble to varying degrees in various organic
solvents and may be present in sufficient
quantity to overwhelm the column
chromatographic cleanup procedures used
for cleanup of sample extracts. Lipids must
240
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
be removed by the lipid removal procedures
In Section 13.7, followed by alumina (Section
13.4) or Florisil (Section 13.8), and carbon
(Section 13.5) as minimum additional clean-
up steps. If chlorodiphenyl ethers are de-
tected, as Indicated by the presence of peaks
at the exact m/z's monitored for these
interferents, alumina and/or Florisil cleanup
must be employed to eliminate these inter-
ferences.
5.0 Safety
5.1 The toxicity or carcinogenicity of
each compound or reagent used in this meth-
od has not been precisely determined; how-
ever, each chemical compound should be
treated as a potential health hazard. Expo-
sure to these compounds should be reduced
to the lowest possible level.
5.1.1 The 2,3,7,8-TCDD isomer has been
found to be acnegenic, carcinogenic, and
teratogenic in laboratory animal studies. It
Is soluble in water to approximately 200 ppt
and in organic solvents to 0.14%. On tie basis
of the available toxicological and physical
properties of 2,3,7,8-TCDD, all of the CDDs/
CDFs should be handled only by highly
trained personnel thoroughly familiar with
handling and cautionary procedures and the
associated risks.
5.1.2 It is recommended that the labora-
tory purchase dilute standard solutions of
the analytes in this method. However, If pri-
mary solutions are prepared, they shall be
prepared in a hood, and a NIOSH/MESA ap-
proved toxic gas respirator shall be worn
when high concentrations are handled.
5.2 The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material safety data
sheets (MSDSs) should also be made avail-
able to all personnel involved in these anal-
yses. It is also suggested that the laboratory
perform personal hygiene monitoring of each
analyst who uses this method and that the
results of this monitoring be made available
to the analyst. Additional information on
laboratory safety can be found in References
10-13. The references and bibliography at the
end of Reference 13 are particularly com-
prehensive in dealing with the general sub-
ject of laboratory safety.
5.3 The CDDs/CDFs and samples suspected
to contain these compounds are handled
using essentially the same techniques em-
ployed in handling radioactive or infectious
materials. Well-ventilated, controlled access
laboratories are required. Assistance in eval-
uating the health hazards of particular lab-
oratory conditions may be obtained from
certain consulting laboratories and from
State Departments of Health or Labor, many
of which have an industrial health service.
The CDDs/CDFs are extremely toxic to lab-
oratory animals. Each laboratory must de-
velop a strict safety program for handling
these compounds. The practices in Ref-
erences 2 and 14 are highly recommended.
5.3.1 Facility—When finely divided sam-
ples (dusts, soils, dry chemicals) are handled,
all operations (including removal of samples
from sample containers, weighing, transfer-
ring, and mixing) should be performed in a
glove box demonstrated to be leak tight or in
a fume hood demonstrated to have adequate
air flow. Gross losses to the laboratory ven-
tilation system must not be allowed. Han-
dling of the dilute solutions normally used in
analytical and animal work presents no in-
halation hazards except In the case of an ac-
cident.
5.3.2 Protective equipment—Disposable
plastic gloves, apron or lab coat, safety
glasses or mask, and a glove box or fume
hood adequate for radioactive work should
be used. During analytical operations that
may give rise to aerosols or dusts, personnel
should wear respirators equipped with acti-
vated carbon filters. Bye protection equip-
ment (preferably full face shields) must be
worn while working with exposed samples or
pure analytical standards. Latex gloves are
commonly used to reduce exposure of the
hands. When handling samples suspected or
known to contain high concentrations of the
CDDs/CDFs, an additional set of gloves can
also be worn beneath the latex gloves.
5.3.3 Training—Workers must be trained
in the proper method of removing contami-
nated gloves and clothing without con-
tacting the exterior surfaces.
5.3,4 Personal hygiene—Hands and fore-
arms should be washed thoroughly after each
manipulation and before breaks (coffee.
lunch, and shift).
5.3.5 Confinement—Isolated work areas
posted with signs, segregated glassware and
tools, and plastic absorbent paper on bench
tops will aid in confining contamination.
5.3.6 Effluent vapors—The effluents of
sample splitters from the gas chromatograph
(GC) and from roughing pumps on the mass
spectrometer (MS) should pass through ei-
ther a column of activated charcoal or be
bubbled through a trap containing oil or
high-boiling alcohols to condense CDD/CDF
vapors.
5.3.7 Waste Handling—Good technique in-
cludes minimizing contaminated waste.
Plastic bag liners should be used in waste
cans. Janitors and other personnel must be
trained in the safe handling of waste.
5.3.8 Decontamination
5.3.8.1 Decontamination of personnel—Use
any mild soap with plenty of scrubbing ac-
tion.
5.3.8.2 Glassware, tools, and surfaces—
Chlorothene NU Solvent is the least toxic
solvent shown to be effective. Satisfactory
cleaning may be accomplished by rinsing
with Chlorothene, then washing with any de-
tergent and water. If glassware is first rinsed
241
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Pt. 136, App. A, Meth. 1613
40 CFi Ch. I (7-1-04 Edition)
with solvent, then the dish water may be dis-
posed of in the sewer. Given the cost of dis-
posal, it is prudent to minimize solvent
wastes.
5.3.9 Laundry—Clothing- known to be con-
taminated should be collected in plastic
bagrs. Persons who convey the bags and laun-
der the clothing should be advised of the haz-
ard and trained in proper handling-, The
clothing- may be put into a washer without
contact if the launderer knows of the poten-
tial problem. The washer should be run
through a cycle before being used again for
otter clothing.
5.3.10 Wipe tests—A useful method of de-
termining: cleanliness of work surfaces and
tools is to wipe the surface with a piece of
filter paper. Extraction and analysis by GO
with an electron capture detector (BCD) can
achieve a limit of detection of 0.1 jig per
wipe; analysis using this method can achieve
an even lower detection limit. Less than 0,1
(ig per wipe indicates acceptable cleanliness;
anything higher warrants further cleaning.
More than 10 |ig on a wipe constitutes an
acute hazard and requires prompt cleaning
before further use of the equipment or work
space, and indicates that unacceptable work
practices have been employed,
5.3.11 Table or wrist-action shaker—The
use of a table or wrist-action shaker for ex-
traction of tissues presents the possibility of
breakage of the extraction bottle and spill-
age of acid and flammable organic solvent. A
secondary containment system around the
shaker is suggested to prevent the spread of
acid and solvents in the event of such a
breakage. The speed and intensity of shaking
action should also be adjusted to minimize
the possibility of breakage.
6.0 Apparatus and Materials
NOTE: Brand names, suppliers, and part
numbers are for illustration purposes only
and no endorsement is implied. Equivalent
performance may be achieved using appa-
ratus and materials other than those speci-
fied here. Meeting the performance require-
ments of this method is the responsibility of
the laboratory.
6.1 Sampling Equipment for Discrete or
Composite Sampling
6.1.1 Sample bottles and caps
6.1.1.1 Liquid samples (waters, sludges and
similar materials containing 5% solids or
less)—Sample bottle, amber glass, 1,1 L min-
imum, with screw cap.
6.1.1.2 Solid samples (soils, sediments,
sludges, paper pulps, filter cake, compost,
and similar materials that contain more
than 5% solids)—Sample bottle, wide mouth,
amber glass, 500 mL minimum.
6,1.1.3 If amber bottles are not available,
samples shall be protected from light.
6.1.1,4 Bottle caps—Threaded to fit sample
bottles. Caps shall be lined with
fluoropolymer.
6.1,1,5 Cleaning
6.1.1.5.1 Bottles are detergent water
washed, then solvent rinsed before use.
6.1.1,5.2 Liners are detergent water
washed, rinsed with reagent water (Section
7.6.1) followed by solvent, and baked at ap-
proximately 200 "C for a minimum of 1 hour
prior to use.
6.1.2 Compositing equipment—Automatic
or manual compositing system incorporating
glass containers cleaned per bottle cleaning
procedure above. Only glass or fluoropolymer
tubing shall be used. If the sampler uses a
peristaltic pump, a minimum length of com-
pressible silicone rubber tubing may be used
ia the pump only. Before use, the tubing
shall be thoroughly rinsed with methanol,
followed by repeated rinsing with reagent
water to minimize sample contamination.
An integrating flow meter is used to collect
proportional composite samples.
6.2 Equipment for Glassware Cleaning-
Laboratory sink with overhead fume hood.
6.3 Equipment for Sample Preparation
6.3.1 Laboratory fume hood of sufficient
size to contain the sample preparation equip-
ment listed below.
6.3.2 Glove box (optional).
6.3.3 Tissue homogenizer—VirTis Model 45
Macro homogenizer (American Scientific
Products H-3515, or equivalent) with stain-
less steel Macro-shaft and Turbo-shear blade.
6.3.4 Meat grinder—Hobart, or equivalent,
with 3-5 mm holes in inner plate.
6.3.5 Equipment for determining percent
moisture
6.3.5.1 Oven—Capable of maintaining a
temperature of 110 ±5 °C.
6.3.5.2 Dessicator.
6.3.6 Balances
6.3.6.1 Analytical—Capable of weighing 0.1
mg-.
6.3.6.2 Top loading—Capable of weighing
10 mg.
6,4 Extraction Apparatus
6.4.1 Water samples
6,4.1.1 pH meter, with combination glass
electrode.
6.4.1.2 pH paper, wide range (Hydrion Pa-
pers, or equivalent).
6.4.1.3 Graduated cylinder, 1 L capacity.
6.4.1.4 Liquid/liquid extraction—Sepa-
ratory funnels, 250 mL, 500 inL, and 2000 mL,
with fluoropolymer stopcocks.
6.4.1.5 Solid-phase extraction
6.4.1.5.1 One liter filtration apparatus, in-
cluding glass funnel, glass frit support,
clamp, adapter, stopper, filtration flask, and
vacuum tubing (Figure 4). For wastewater
samples, the apparatus should accept 90 or
144 mm disks. For drinking water or other
samples containing low solids, smaller disks
may be used.
242
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Environmental Protection Agency
Pt, 136, App. A, Mettl. 1613
6,4.1.5.2 Vacuum source capable of main-
taining 25 in. Hg, equipped with shutoff valve
and vacuum gauge,
6.4.1.5.3 Glass-fiber filter—Whatman GMF
150 (or equivalent), 1 micron pore size, to fit
filtration apparatus In Section 6.4.1.5.1.
6,4.1.5.4 Solid-phase extraction disk con-
taining1 octadeeyl (C18) bonded silica uni-
formly enmeshed in an inert matrix—Fisher
Scientific 14-378F (or equivalent), to fit fil-
tration apparatus in Section 8,4.1,5.1.
6.4.2 Soxhlet/Dean-Stark (SDS) extractor
(Figure 5)—For filters and solid/sludge sam-
ples.
6.4.2.1 Soxhlet—50 mm ID, 200 mL capac-
ity with 600 mL flask (Gal-Glass LG-6900, or
equivalent, except substitute 500 mL round-
bottom flask for 300 mL flat-bottom flask).
6.4.2.2 Thimble—43 x 123 to fit Soxhlet
(Cal-Glass LG-6901-122, or equivalent).
6.4.2,3 Moisture trap—Dean Stark or Bar-
ret with fluoropolymer stopcock, to fit Soxh-
let.
6,4.2.4 Heating mantle—Hemispherical, to
fit 500 mL round-bottom flask (Cal-Glass LG-
8801-112, or equivalent).
6.4.2.5 Variable transformer—Fowerstat
(or equivalent), 110 volt, 10 amp.
6,4.3 Apparatus for extraction of tissue.
6.4.3.1 Bottle for extraction (if digestion/
extraction using HC1 is used)" 500-600 mL
wide-mouth clear glass, with fluoropolymer-
lined cap.
6.4.3.2 Bottle for back-extraction—100-200
mL narrow-mouth clear glass with
flnoropolymer-lined cap.
6.4.3.3 Mechanical shaker—Wrist-action
or platform-type rotary shaker that pro-
duces vigorous agitation (Sybron
Thermolyne Model LE "Big Bill" rotator/
shaker, or equivalent).
6.4.3.4 Back attached to shaker table to
permit agitation of four to nine samples si-
multaneously.
6.4.4 Beakers—400-500 mL.
6.4.5 Spatulas—Stainless steel.
6.5 Filtration Apparatus.
6.5.1 Pyrex glass wool—Solvent-extracted
by SDS for three hours minimum.
NOTE: Baking glass wool may cause active
sites that will irreversibly adsorb CDDs/
CDFs.
6.5.2 Glass funnel—125-250 mL.
6.5.3 Glass-fiber filter paper—Whatman
GF/D (or equivalent), to fit glass funnel in
Section 6,5.2.
6.5.4 Drying column—15-20 mm ID Pyrex
chromatographic column equipped with
coarse-glass frit or glass-wool plug,
6.5.5 Buchner funnel—15 cm.
6,5.6 Glass-fiber filter paper—to fit
Buchner funnel in Section 6.5.5.
6.5.7 Filtration flasks—1.5-2,0 L, with side
arm.
6.5.8 Pressure filtration apparatus—
Millipore YT30 142 HW, or equivalent.
6,6 Centrifuge Apparatus.
6.6.1 Centrifuge—Capable of rotating 500
mL centrifuge bottles or 15 mL centrifuge
tubes at 5,000 rpm minimum,
6,6.2 Centrifuge bottles—500 mL, with
screw-caps, to fit centrifuge.
6.6.3 Centrifuge tubes—12-15 mL, with
screw-caps, to fit centrifuge,
6.7 Cleanup Apparatus.
6.7.1 Automated gel permeation chro-
matograph (Analytical Biochemical Labs,
Inc, Columbia, MO, Model GPC Autoprep
1002, or equivalent).
6.7.1.1 Column—600-700 mm long x 25 mm
ID, packed with 70 g of
SX-3 Bio-beads (Bio-Bad Laboratories, Rich-
mond, CA, or equivalent).
6.7.1.2 Syringe—10 mL, with Luer fitting.
6.7.1.3 Syringe filter holder—stainless
steel, and glass-fiber or fluoropolymer filters
(Gelman 4310, or equivalent).
6.7.1.4 UV detectors—254 nm, preparative
or semi-preparative flow cell (Isco, Inc.,
Type 6; Schmadzu, 5 mm path length; Beck-
man-Altex 152W, 8 |iL micro-prep flow cell, 2
mm path; Pharmacia UV-1, 3 mm flow cell;
LDC Milton-Boy UV-3, monitor #1303; or
equivalent).
6.7,2 Be verse-phase high-performance liq-
uid ohromatograph.
6,7.2.1 Column oven and detector—Perkin-
Blmer Model LC-65T (or equivalent) operated
at 0,02 AUFS at 235 nm.
6.7.2.2 Injector—Eheodyne 7120 (or equiva-
lent) with 50 |iL sample loop.
6.7.2.3 Column—Two 6.2 mm x 250 mm
Zorbax-ODS columns in series (DuPont In-
struments Division, Wilmington, DE, or
equivalent), operated at 50 °C with 2.0 mL/
min methanol isocratic effluent.
6,7.2.4 Pump—Altex 110A (or equivalent).
6.7.3 Pipets.
6.7.3.1 Disposable, pasteur—150 mm long x
5-mm ID (Fisher Scientific 13-678-6A, or
equivalent).
6.7,3.2 Disposable, serologioal—10 mL (6
mm ID).
6.7.4 Glass chromatographic columns.
6.7.4.1 150 mm long x 8-mm ID, (Kontes K-
420155, or equivalent) with coarse-glass frit
or glass-wool plug and 250 mL reservoir.
6.7,4.2 200 mm long x 15 mm ID, with
coarse-glass frit or glass-wool plug and 250
mL reservoir.
6.7,4.3 300 mm long x 25 mm ID, with 300
mL reservoir and glass or fluoropolymer
stopcock,
6.7.5 Stirring apparatus for batch silica
cleanup of tissue extracts.
6.7,5.1 Mechanical stirrer—Corning Model
320, or equivalent.
6.7.5.2 Bottle—500-600 mL wide-mouth
clear glass,
6.7.6 Oven—For baking and storage of ad-
sorbents, capable of maintaining a constant
temperature (±5 °C) in the range of 105-250 "C.
6.8 Concentration Apparatus.
243
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Pt, 136, App. A, Meth. 1613
40 CFR Ch. J (7-1-04 Edition)
6.8.1 Rotary evaporator—Buchi/
Brinkman-Ameriean Scientific No. B5045-10
or equivalent, equipped with a variable tem-
perature water bath.
6.8,1,1 Vacuum source for rotary evapo-
rator equipped with shutoff valve at the
evaporator and vacuum gauge.
6.8,1,2 A reeirealating water pump and
chiller are recommended, as use of tap water
for cooling the evaporator wastes large vol-
umes of water and can lead to Inconsistent
performance as water temperatures and pres-
sures vary.
6.8,1,3 Bound-bottom flask—100 mL and
500 mL or larger, with ground-glass fitting
compatible witli the rotary evaporator.
6.8.2 Kuderna-Danish (K-D) Concentrator.
6.8.2.1 Concentrator tube—10 mL, grad-
uated (Kontes K-570050-1025, or equivalent)
with calibration verified. Ground-glass stop-
per (size 19/22 joint) Is used to prevent evapo-
ration of extracts.
6.8.2.2 Evaporation flask—500 mL (Kontes
K-570001-0500, or equivalent), attached to
concentrator tube with springs (Kontes K-
662750-0012 or equivalent).
6.8.2,3 Snyder column—Three-ball macro
(Kontes K-5Q3000-Q232, or equivalent).
6.8.2,4 Boiling chips.
6.8.2.4.1 Glass or silicon carbide—Approxi-
mately 10/40 mesh, extracted with methylene
chloride and baked at 450 "C for one hour
minimum.
6.8.2.4.2 Fluoropolymer (optional)—Ex-
tracted with methylene chloride.
6.8.2.5 Water bath—Heated, with concen-
tric ring cover, capable of maintaining a
temperature within ±2 °C, installed in a fume
hood.
6.8.3 Nitrogen blowdown apparatus—
Equipped with water bath controlled in. the
range of 30-60 "C (N-Evap, Organomation As-
sociates, Inc., South Berlin, MA, or equiva-
lent), installed in a fume hood.
6.8.4 Sample vials,
6.8.4,1 Amber glass—2-5 mL with
fluoropolymer-lined screw-cap.
6.8.4.2 Glass—0.3 mL, conical, with
fluoropolymer-lined screw or crimp cap.
6,9 Gas Chromatograph—Shall have
splitless or on-column injection port for cap-
illary column, temperature program with
isothermal hold, and shall meet all of the
performance specifications in Section 10.
6.9.1 GC column for CDDs/CDFs and for
Isomer specificity for 2,3,7,8-TCDD—6045 m
long x 0.32±0,02 mm ID; 0.26 (im 5% phenyl,
94% methyl, 1% vinyl silicone bonded-phase
fused-silica capillary column (J&W DB-5, or
equivalent),
6.9.2 GC column for isomer specificity for
2,3,7,8-TCDF~-30±5 m long x 0.32±0.02 mm ID;
0.25 |im bonded-phase fused-silica capillary
column (J&W DB-225, or equivalent).
6.10 Mass Spectrometer—28-40 eV electron
impact ionizatlon, shall tie capable of repet-
itively selectively monitoring 12 exact m/z's
minimum at high resolution (£10,000) during
a period of approximately one second, and
shall meet all of the performance specifica-
tions in Section 10,
6.11 GC/MS Interface—The mass spec-
trometer (MS) shall be interfaced to the GC
such that the end of the capillary column
terminates within 1 cm of the ion source but
does not intercept the electron or ion beams,
6.12 Data System—Capable of collecting,
recording, and storing MS data,
7,0 Reagents and Standards
7.1 pH Adjustment and Back-Extraction.
7.1.1 Potassium hydroxide—Dissolve 20 g
reagent grade KOH in 100 mL reagent water.
7.1.2 Sulfuric acid—Eeagent grade (spe-
cific gravity 1.84).
7.1.3 Hydrochloric acid—Reagent grade,
6N.
7.1.4 Sodium chloride—Reagent grade,
prepare at 5% (w/v) solution in reagent
water.
7.2 Solution Drying and Evaporation.
7.2.1 Solution drying—Sodium sulfate, re-
agent grade, granular, anhydrous (Baker
3375, or equivalent), rinsed with methylene
chloride (20 mL/g), baked at 400 "C for one
hour minimum, cooled in a dessicator, and
stored in a pre-cleaned glass bottle with
screw-cap that prevents moisture from en-
tering. If, after heating, the sodium sulfate
develops a noticeable grayish cast (due to
the presence of carbon in the crystal ma-
trix), that batch of reagent is not suitable
for use and should be discarded. Extraction
with methylene chloride (as opposed to sim-
ple rinsing) and baking at a lower tempera-
ture may produce sodium sulfate that is
suitable for use,
7.2.2 Tissue drying—Sodium sulfate, rea-
gent grade, powdered, treated and stored as
above.
7.2.3 Prepurified nitrogen,
7.3 Extraction.
7.3.1 Solvents—Acetone, toluene,
cyclohexane, hexane, methanol, methylene
chloride, and nonane; distilled in glass, pes-
ticide quality, lot-certified to be free of
interferences,
7.3.2 White quartz sand, 60/70 mesh—For
Soxhlet/Dean-Stark extraction (Aldrieh
Chemical, Cat. No. 27-437-9, or equivalent).
Bake at 450 "C for four hours minimum.
7.4 GPC Calibration Solution—Prepare a
solution containing 300 mg/mL corn oil, 15
mg/mL bis(2-ethylhexyl) phthalate, 1.4 mg/
mL pentachlorophenol, 0.1 mg/mL perylene,
and 0.5 mg/mL sulfur,
7.5 Adsorbents for Sample Cleanup.
7.5.1 Silica gel.
7.5.1.1 Activated silica gel—100-200 mesh,
Supelco 1-3651 (or equivalent), rinsed with
methylene chloride, baked at 180 °C for a
minimum of one hour, cooled in a dessicator,
and stored in a precleaned glass bottle with
244
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
screw-cap that prevents moisture from en-
tering,
7.5.1.2 Acid silica gel (30% w/w)—Thor-
oughly mix 44.0 g of concentrated sulfnric
acid with 100.0 g of activated silica gel in a
clean container. Break up aggregates with a
stirring rod until a uniform mixture is ob-
tained. Store in a bottle with a
fluoropolymer-lined screw-cap.
7.5.1.3 Basic silica gel—Thoroughly mix 30
g of IN sodium hydroxide with 100 g of acti-
vated silica gel in a clean container. Break
up aggregates with a stirring rod until a uni-
form mixture is obtained. Store in a bottle
with a fluoropolymer-lined screw-cap.
7.5.1.4 Potassium silicate.
7.5.1.4.1 Dissolve 56 g of high purity potas-
sium hydroxide (Aldrich, or equivalent) in
300 mL of methanol in a 750-1000 mL flat-bot-
tom flask.
7.5.1.4.2 Add 100 g of silica gel and a stir-
ring bar, and stir on a hot plate at 60-70 °C
for one to two hours.
7.5.1.4.3 Decant the liquid and rinse the
potassium silicate twice with 100 mL por-
tions of methanol, followed by a single rinse
with 100 mL of methylene chloride.
7.5.1.4.4 Spread the potassium silicate on
solvent-rinsed aluminum foil and dry for two
to four hours in a hood.
7.5.1.4.5 Activate overnight at 200-250 °C.
7.5.2 Alumina—Either one of two types of
alumina, acid or basic, may be used in the
cleanup of sample extracts, provided that the
laboratory can meet the performance speci-
fications for the recovery of labeled com-
pounds described in Section 9.3. The same
type of alumina must be used for all samples,
including those used to demonstrate initial
precision and recovery (Section 9.2) and on-
going precision and recovery (Section 15.5).
7.5.2.1 Acid alumina—Supelco 19996-6C (or
equivalent). Activate by heating to 130 °C for
a minimum of 12 hours.
7.5.2.2 Basic alumina—Supelco 19944-6C
(or equivalent). Activate by heating to 600 °C
for a minimum of 24 hours. Alternatively, ac-
tivate by heating in a tube furnace at 650-700
°C under an air flow rate of approximately
400 cc/minnte. Do not heat over 700 °C, as this
can lead to reduced capacity for retaining
the analytes. Store at 130 °C in a covered
flask. Use within five days of baking.
7.5.3 Carbon.
7.5.3.1 Carbopak C—(Supelco 1-0258, or
equivalent).
7.5.3.2 Cellte 545—(Supelco 2-0199, or
equivalent).
7.5.3.3 Thoroughly mix 9.0 g Carbopak C
and 41.0 g Celite 545 to produce an 18% w/w
mixture. Activate the mixture at 130 °C for a
minimnm of six hours. Store in a dessicator.
7.5.4 Anthropogenic isolation column—
Pack the column in Section 6.7.4.3 from bot-
tom to top with the following:
7.5.4.1 2 g silica gel (Section 7.5.1.1).
7.5.4.2 2 g potassium silicate (Section
7.5.1.4).
7.5.4.3 2 g granular anhydrous sodium sul-
fate (Section 7.2.1).
7.5.4.4 10 g acid silica gel (Section 7.5.1.2).
7.5.4.5 2 g granular anhydrous sodium sul-
fate.
7.5.5 Florisil column.
7.5.5.1 Florisil—60-100 mesh, Floridin Corp
(or equivalent). Soxhlet extract in 500 g por-
tions for 24 hours.
7.5.5.2 Insert a glass wool plug into the ta-
pered end of a graduated serological pipet
(Section 6.7.3.2). Pack with 1.5 g (approx 2
mL) of Florisil topped with approx 1 mL of
sodium sulfate (Section 7.2.1) and a glass
wool plug.
7.5.5.3 Activate in an oven at 130-150 °C for
a minimum of 24 hours and cool for 30 min-
utes. Use withia 90 minutes of cooling.
7.6 Reference Matrices—Matrices in
which the CDDs/CDFs and interfering com-
pounds are not detected by this method.
7.6.1 Reagent water—Bottled water pur-
chased locally, or prepared by passage
through activated carbon.
7.6.2 High-solids reference matrix—Play-
ground sand or similar material. Prepared by
extraction with methylene chloride and/or
baking at 450 °C for a minimum of four
hours.
7.6.3 Paper reference matrix—Glass-fiber
filter, Gelman Type A, or equivalent. Cut
paper to simulate the surface area of the
paper sample being tested.
7.6.4 Tissue reference matrix—Corn or
other vegetable oil. May be prepared by ex-
traction with methylene chloride.
7.6.6 Other matrices—This method may be
verified on any reference matrix by per-
forming the teats given in Section 9.2. Ideal-
ly, the matrix should be free of the CDDs/
CDFs, but in no case shall the background
level of the CDDs/CDFs in the reference ma-
trix exceed three times the minimum levels
in Table 2. If low background levels of the
CDDs/CDFs are present in the reference ma-
trix, the spike level of the analytes used in
Section 9.2 should be increased to provide a
spike-to-background ratio in the range of 1:1
to 5:1 (Reference 15).
7.7 Standard Solutions—Purchased as so-
lutions or mixtures with certification to
their purity, concentration, and authen-
ticity, or prepared from materials of known
purity and composition. If the chemical pu-
rity is 98% or greater, the weight may be
used without correction to compute the con-
centration of the standard. When not being
used, standards are stored in the dark at
room temperature in screw-capped vials with
fluoropolymer-lined caps. A mark is placed
on the vial at the level of the solution so
that solvent loss by evaporation can be de-
tected. If solvent loss has occurred, the solu-
tion should be replaced.
7.8 Stock Solutions.
245
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40 CFR Ch. I (7-1-04 Edition)
7.8.1 Preparation—Prepare in nonane per
the steps below or purchase as dilute solu-
tions (Cambridge Isotope Laboratories (OIL),
Woburn, MA, or equivalent). Observe the
safety precautions in Section 5, and the rec-
ommendation in Section 5.1.2.
7.8.2 Dissolve an appropriate amount of
assayed reference material in solvent. For
example, weigh 1-2 mg of 2,3,7,8-TCDD to
three significant figures in a 10 mL ground-
glass-stoppered volumetric flask and fill to
the mark with nonane. After the TCDD is
completely dissolved, transfer the solution
to a clean 15 mL vial with flnoropolymer-
lined cap.
7,8.3 Stock standard solutions should be
checked for signs of degradation prior to the
preparation of calibration or performance
test standards. Reference standards that can
be used to determine the accuracy of calibra-
tion standards are available from OIL and
may be available from other vendors.
7.9 PAR Stock Solution
7.9.1 All CDDs/CDPs—Using the solutions
In Section 7.8, prepare the PAR stock solu-
tion to contain the CDDs/CDPs at the con-
centrations shown in Table 3. When diluted,
the solution will become the PAE (Section
7,14).
7.9.2 If only 2,3,7,8-TCDD and 2,3,7,8-TCDF
are to be determined, prepare the PAR stock
solution to contain these compounds only.
7.10 Labeled-Compound Spiking Solution.
7.10.1 All CDDs/CDPs—Prom stock solu-
tions, or from purchased mixtures, prepare
this solution to contain the labeled com-
pounds in nonane at the concentrations
shown in Table 3, This solution is diluted
with acetone prior to use (Section 7.10.3).
7.10.2 If only 2,3,7,8-TCDD and 2,3,7,8-
TCDF are to be determined, prepare the la-
beled-compound solution to contain these
compounds only. This solution is diluted
with acetone prior to use (Section 7.10.3).
7.10.3 Dilute a sufficient volume of the la-
beled compound solution (Section 7.10.1 or
7.10.2) by a factor of 50 with acetone to pre-
pare a diluted spiking solution. Each sample
requires 1.0 mL of the diluted solution, but
no more solution should be prepared than
can be used in one day.
7.11 Cleanup Standard—Prepare "Cr5-
2,3,7,8-TCDD in nonane at the concentration
shown in Table 3. The cleanup standard Is
added to all extracts prior to cleanup to
measure the efficiency of the cleanup proc-
ess.
7.12 Internal Standard(s).
7.12.1 All CDDs/CDPs—Prepare the inter-
nal standard solution to contain 13C12-1,2,3,4-
TCDD and »C2-l,2,3,7,8,9-HxCDD in nonane at
the concentration shown in Table 3.
7,12.2 If only 2,3,7,8-TCDD and 2,3,7,8-
TCDF are to be determined, prepare the in-
ternal standard solution to contain >^Cn-
1,2,3,4-TCDD only.
7,13 Calibration Standards (CS1 through
CSS)—Combine the solutions in Sections 7.9
through 7,12 to produce the five calibration
solutions shown in Table 4 in nonane. These
solutions permit the relative response (la-
beled to native) and response factor to be
measured as a function of concentration, The
CSS standard is used for calibration
verification (VER). If only 2,3,7,8-TCDD and
2,3,7,8-TCDF are to be determined, combine
the solutions appropriate to these com-
pounds,
7.14 Precision and Recovery (PAR) Stand-
ard—Used for determination of initial (Sec-
tion 9.2) and ongoing (Section 15.5) precision
and recovery, Dilute 10 fiL of the precision
and recovery standard (Section 7.9.1 or 7.9.2)
to 2,0 mL with acetone for each sample ma-
trix for each sample batch. One mL each are
required for the blank and OPB with each
matrix in each batch.
7.15 GC Retention Time Window Defining
Solution and Isomer Specificity Test Stand-
ard—Used to define the beginning and ending
retention times for the dioxin and furan iso-
mers and to demonstrate isomer specificity
of the GC columns employed for determina-
tion of 2,3,7,8-TCDD and 2,3,7,8-TCDF. The
standard must contain the compounds listed
in Table 5 (OIL EDF—4006, or equivalent), at
a minimum. It is not necessary to monitor
the window-defining compounds if only
2,3,7,8-TCDD and 2,3,7,8-TODF are to be de-
termined. In this case, an isomer-specificity
test standard containing the most closely
eluted isomers listed in Table a (CIL EDF-
4033. or equivalent) may he used.
7.16 QC Check Sample—A QC Check Sam-
ple should be obtained from a source inde-
pendent of the calibration standards. Ideally,
this check sample would be a certified ref-
erence material containing the CDDs/CDFs
in known concentrations in a sample matrix
similar to the matrix under test,
7.17 Stability of Solutions—Standard so-
lutions used for quantitative purposes (Sec-
tions 7.9 through 7.15) should be analyzed pe-
riodically, and should be assayed against ref-
erence standards (Section 7.8.3) before fur-
ther use.
8.0 Sample Collection, Preservation, Storage,
and Holding Times
8.1 Collect samples in amber glass con-
tainers following conventional sampling
practices (Reference 16). Aqueous samples
that flow freely are collected in refrigerated
bottles using automatic sampling equip-
ment. Solid samples are collected as grab
samples using wide-mouth jars.
8.2 Maintain aqueous samples in the dark
at 0-4 °C from the time of collection until re-
ceipt at the laboratory. If residual chlorine
is present in aqueous samples, add 80 mg so-
dium thiosulfate per liter of water. EPA
246
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M. 136, App. A, Meth. 1613
Methods 330.4 and 330.5 may be used to meas-
ure residual chlorine (Reference 17). If sam-
ple pH is greater than 9, adjust to pH 7-9
with sulfurie acid.
Maintain solid, semi-solid, oily, and mixed-
phase samples in the dark at <4 "C from the
time of collection until receipt at the labora-
tory.
Store aqueous samples in the dark at 0-4
°C. Store solid, semi-solid, oily, mixed-phase,
and tissue samples in the dark at < —10 °C.
8.3 Fish and Tissue Samples.
8.3.1 Fish may be cleaned, filleted, or
processed In other ways in the field, such
that the laboratory may expect to receive
whole fish, fish fillets, or other tissues for
analysis.
8.3.2 Fish collected in the field should be
wrapped in aluminum foil, and must be
maintained at a temperature less than 4 8C
from the time of collection until receipt at
the laboratory.
8.3.3 Samples must be frozen upon receipt
at the laboratory and maintained in the dark
at < —10 "C until prepared. Maintain unused
sample in the dark at < -10 °C.
8.4 Holding Times.
8.4.1 There are no demonstrated max-
imum holding times associated with CDDs/
CDPs in aqueous, solid, semi-solid, tissues,
or other sample matrices. If stored in the
dark at 0-4 "C and preserved as given above
(if required), aqueous samples may be stored
for up to one year. Similarly, if stored in the
dark at <-10 °C, solid, semi-solid, multi-
phase, and tissue samples may be stored for
up to one year,
8.4.2 Store sample extracts in the dark at
<-10 °C until analyzed. If stored in the dark
at < —10 °C, sample extracts may be stored
for up to one year.
9.0 Quality Assurance/Quality Control
9.1 Each laboratory that uses this method
is required to operate a formal quality assur-
ance program (Reference 18), The minimum
requirements of this program consist of an
initial demonstration of laboratory capa-
bility, analysis of samples spiked with la-
beled compounds to evaluate and document
data quality, and analysis of standards and
blanks as tests of continued performance.
Laboratory performance is compared to es-
tablished performance criteria to determine
if the results of analyses meet the perform-
ance characteristics of the method.
If the method is to be applied to sample
matrix other than water (e.g., soils, filter
cake, compost, tissue) the most appropriate
alternate matrix (Sections 7.6.2 through
7.6.5) is substituted for the reagent water
matrix (Section 7.6.1) in all performance
tests.
9.1,1 The analyst shall make an initial
demonstration of the ability to generate ac-
ceptable accuracy and precision with this
method. This ability is established as de-
scribed in Section 9.2,
9.1.2 In recognition of advances that are
occurring in analytical technology, and to
allow the analyst to overcome sample ma-
trix interferences, the analyst is permitted
certain options to improve separations or
lower the costs of measurements. These op-
tions include alternate extraction, con-
centration, cleanup procedures, and changes
in columns and detectors. Alternate deter-
minative techniques, such as the substi-
tution of spectroscopic or immuno-assay
techniques, and changes that degrade meth-
od performance, are not allowed. If an ana-
lytical technique other than the techniques
specified in this method is used, that tech-
nique must have a specificity equal to or bet-
ter than the specificity of the techniques in
this method for the analytes of interest.
9.1.2.1 Each time a modification is made
to this method, the analyst is required to re-
peat the procedure in Section 9.2. If the de-
tection limit of the method will be affected
by the change, the laboratory is required to
demonstrate that the MDL (40 CFB Part 136,
Appendix B) is lower than one-third the reg-
ulatory compliance level or one-third the
ML in this method, whichever is higher. If
calibration will be affected by the change,
the analyst must recalibrate the Instrument
per Section 10.
9.1.2.2 The laboratory is required to main-
tain records of modifications made to this
method. These records include the following,
at a minimum:
9.1.2.2,1 The names, titles, addresses, and
telephone numbers of the analyst(s) who per-
formed the analyses and modification, and of
the quality control officer who witnessed and
will verify the analyses and modifications.
9.1.2.2.2 A listing of pollutant(s) meas-
ured, by name and CAS Registry number.
9.1.2.2.3 A narrative stating reason(s) for
the modifications.
9.1.2.2.4 Results from all quality control
(QO) tests comparing the modified method to
this method, including:
(a) Calibration (Section 10.5 through 10.7).
(b) Calibration verification (Section 15.3).
(c) Initial precision, and recovery (Section
9.2).
(d) Labeled compound recovery (Section
9.3).
(e) Analysis of blanks (Section 9.5).
(f) Accuracy assessment (Section 9.4).
9.1.2.2.5 Data that will allow- an inde-
pendent reviewer to validate each deter-
mination by tracing the instrument output
(peak height, area, or other signal) to the
final result. These data are to include:
(a) Sample numbers and other identifiers,
(b) Extraction dates.
(c) Analysis dates and times.
(d) Analysis sequence/run chronology.
(e) Sample weight or volume (Section 11).
247
203-160 D-9
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Pt. 136, App. A, Mem. 1613
40 CFR Ch.! (7-1-04 Edition)
(f) Extract volume prior to each, cleanup
step (Section 13).
(g) Extract volume after each cleanup step
(Section 13).
(h) Final extract volume prior to injection
(Section 14).
(i) Injection volume (Section 14.3).
(j) Dilution data, differentiating between
dilution of a sample or extract (Section 17.5).
(k) Instrument and operating conditions.
(1) Column (dimensions, liquid phase, solid
support, film thickness, etc).
(m) Operating conditions (temperatures,
temperature program, flow rates).
(n) Detector (type, operating conditions,
etc).
(o) Chromatograms, printer tapes, and
other recordings of raw data.
(p) Quantitation reports, data system out-
puts, and other data to link the raw data to
the results reported.
9.1.3 Analyses of method blanks are re-
quired to demonstrate freedom from con-
tamination (Section 4.3). The procedures and
criteria for analysis of a method blank are
described in Sections 9.5 and 15.6.
9.1.4 The laboratory shall spike all sam-
ples with labeled compounds to monitor
method performance. This test is described
in Section 9.3. When results of these spikes
indicate atypical method performance for
samples, the samples are diluted to bring
method performance within acceptable lim-
its. Procedures for dilution are given in Sec-
tion 17.5.
9.1.5 The laboratory shall, on an ongoing
basis, demonstrate through calibration
verification and the analysis of the ongoing
precision and recovery aliquot that the ana-
lytical system is in control. These proce-
dures are described in Sections 15.1 through
15.5.
9.1.6 The laboratory shall maintain
records to define the quality of data that is
generated. Development of accuracy state-
ments is described in Section 9.4.
9.2 Initial Precision and Recovery (IPB)—
To establish the ability to generate accept-
able precision and recovery, the analyst
shall perform the following operations.
9.2,1 For low solida (aqueous) samples, ex-
tract, concentrate, and analyze four 1 L
aliquots of reagent water spiked with the di-
luted labeled compound spiking solution
(Section 7.10.3) and the precision and recov-
ery standard (Section 7.14) according to the
procedures in Sections 11 through 18. For an
alternative sample matrix, four aliquots of
the alternative reference matrix (Section 7.6)
are used. All sample processing steps that
are to be used for processing samples, includ-
ing preparation (Section 11), extraction (Sec-
tion 12), and cleanup (Section 13), shall be in-
cluded in this test.
9.2.2 Using results of the set of four anal-
yses, compute the average concentration (X)
of the extracts in ng/mL and the standard de-
viation of the concentration (s) in ng/mL for
each compound, by isotope dilution for
CDDs/CDFs with a labeled analog, and by in-
ternal standard for 1,2,3,7,8,9-HxCDD, OCDF,
and the labeled compounds.
9.2.3 For each CDD/CDF and labeled com-
pound, compare s and X with the cor-
responding limits for initial precision and re-
covery in Table 6. If only 2,3,7,8-TCDD and
2,3,7,8-TCDF are to be determined, compare s
and X with the corresponding limits for ini-
tial precision and recovery in Table 6a. If s
and X for all compounds meet the acceptance
criteria, system performance is acceptable
and analysis of blanks and samples may
begin. If, however, any individual s exceeds
the precision limit or any individual X falls
outside the range for accuracy, system per-
formance is unacceptable for that compound.
Correct the problem and repeat the test (Sec-
tion 9.2).
9.3 The laboratory shall spike all samples
with the diluted labeled compound spiking
solution (Section 7.10.3) to assess method
performance on the sample matrix.
9.3.1 Analyze each sample according to
the procedures in Sections 11 through 18.
9.3.2 Compute the percent recovery of the
labeled compounds and the cleanup standard
using the internal standard method (Section
17,2).
9.3.3 The recovery of each labeled com-
pound must be within the limits in Table 7
when all 2,3,7,8-substituted CDDs/CDFs are
determined, and within the limits in Table
7a when only 2,3,7,8-TCDD and 2,3,7,8-TCDF
are determined. If the recovery of any com-
pound falls outside of these limits, method
performance is unacceptable for that com-
pound in that sample. To overcome such dif-
ficulties, water samples are diluted and
smaller amounts of soils, sludges, sediments,
and other matrices are reanalyzed per Sec-
tion 18.4.
9.4 Recovery of labeled compounds from
samples should be assessed and records
should be maintained.
9.4.1 After the analysis of five samples of
a given matrix type (water, soil, sludge,
pulp, etc.) for which the labeled compounds
pass the tests in Section 9.3, compute the av-
erage percent recovery (R) and tne standard
deviation of the percent recovery (SR) for
the labeled compounds only. Express the as-
sessment as a percent recovery interval from
R-2SR to B=2SR for each matrix. For exam-
ple, if R = 90% and SR = 10% for five analyses
of pulp, the recovery interval is expressed as
7(H10%.
9.4.2 Update the accuracy assessment for
each labeled compound in each matrix on a
regular basis (e.g., after each 5-10 new meas-
urements).
9.5 Method Blanks—Reference matrix
method blanks are analyzed to demonstrate
freedom from contamination (Section 4.3).
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Pt. 136, App, A, Meth. 1613
9.5.1 Prepare, extract, clean up, and con-
centrate a method blank with each sample
batch (samples of tlie same matrix started
through the extraction process on the same
12-hour shift, to a maximum of 20 samples).
The matrix for the method blank shall be
similar to sample matrix for the batch, e.g.,
a 1 L reagent water blank (Section 7.6.1),
high-solids reference matrix blank (Section
7.6.2), paper matrix blank (Section 7.6.3); tis-
sue blank (Section 7.6.4) or alternative ref-
erence matrix blank (Section 7.6.5). Analyze
the blank immediately after analysis of the
OPB (Section 15.5) to demonstrate freedom
from contamination.
9.5.2 If any 2,3,7,8-substituted CDD/CDF
(Table 1) is found in the blank at greater
than the minimum level (Table 2) or one-
tMrd the regulatory compliance level,
whichever is greater; or if any potentially
interfering compound is found in tie blank
at the minimum level for each level of
chlorination given in Table 2 (assuming a re-
sponse factor of 1 relative to the 13Ci2-l,2,3,4-
TODD internal standard for compounds not
listed in Table 1), analysis of samples is halt-
ed until the blank associated with the sam-
ple batch shows no evidence of contamina-
tion at this level. All samples must be asso-
ciated with an uncontaminated method
blank before the results for those samples
may be reported for regulatory compliance
purposes.
9.6 QC Check Sample—Analyze the QC
Check Sample (Section 7.16) periodically to
assure the accuracy of calibration standards
and the overall reliability of. the analytical
process. It is suggested that the QC Check
Sample be analyzed at least quarterly.
9.7 The specifications contained in this
method can be met if the apparatus used is
calibrated properly and then maintained in a
calibrated state. The standards used for cali-
bration (Section 10), calibration verification
(Section 15.3), and for initial (Section 9.2)
and ongoing (Section 15.5) precision and re-
covery should be identical, so that the most
precise results will be obtained. A GC/MS in-
strument will provide the most reproducible
results if dedicated to the settings and condi-
tions required for the analyses of CDDs/CDFs
by this method.
8,8 Depending on specific program re-
quirements, field replicates may be collected
to determine the precision of the sampling
technique, and spiked samples may be re-
quired to determine the accuracy of the
analysis when the internal standard method
is used.
10.0 Calibration
10.1 Establish the operating conditions
necessary to meet the minimum retention
times for the internal standards in Section
10.2.4 and the relative retention times for the
CDDs/CDFs in Table 2.
10.1.1 Suggested QC operating conditions;
Injector temperature: 270 °C
Interface temperature: 290 °C
Initial temperature: 200 °C
Initial time: Two minutes
Temperature program:
200-220 °C, at 5 °C/minute
220 "C for 16 minutes
220-235 °C, at 5 "C/minute
235 °C for seven minutes
235-830 °C, at 5 "C/minute
NOTE: All portions of the column that con-
nect the GC to the ion source shall remain at
or above the interface temperature specified
above during analysis to preclude condensa-
tion of less volatile compounds.
Optimize GC conditions for compound sep-
aration and sensitivity. Once optimized, the
same GC conditions must be used for the
analysis of all standards, blanks, IPR and
OPE aliquots, and samples.
10.1,2 Mass spectrometer (MS) resolu-
tion—Obtain a selected ion current profile
(SICP) of each analyte in Table 3 at the two
exact m/z's specified in Table 8 and at >10,000
resolving power by injecting an authentic
standard of the CDDs/CDFs either singly or
as part of a mixture in which there is no in-
terference between closely eluted compo-
nents.
10.1.2.1 The analysis time for CDDs/CDFs
may exceed the long-term mass stability of
the mass spectrometer. Because the instru-
ment is operated in the high-resolution
mode, mass drifts of a few ppm (e.g., 5 ppm
in mass) can have serious adverse effects on
instrument performance. Therefore, a mass-
drift correction is mandatory and a lock-
mass m/z from PFK is used for drift correc-
tion. The lock-mass m/z is dependent on the
exact m/z*s monitored within each
descriptor, as shown in Table 8. The level of
PFK metered into the HRMS during analyses
should be adjusted so that the amplitude of
the most intense selected look-mass m/z sig-
nal (regardless of the descriptor number)
does not exceed 10% of the full-scale deflec-
tion for a given set of detector parameters.
Under those conditions, sensitivity changes
that might occur during the analysis can be
more effectively monitored.
NOTE: Excessive PFK (or any other ref-
erence substance) may cause noise problems
and contamination of the ion source necessi-
tating increased frequency of source clean-
ing.
10.1.2,2 If the HEMS has the capability to
monitor resolution during the analysis, it is
acceptable to terminate the analysis when
the resolution falls below 10,000 to save rea-
nalysis time.
10.1.2.3 Using a PFK molecular leak, tune
the instrument to meet the minimum re-
quired resolving power of 10,000 (10% valley)
at m/z 304.9824 (PFK) or any other reference
signal close to m/z 304 (from TCDF). For each
249
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40 CFR Ch. I (7-1-04 Edition)
descriptor (Table 8), monitor and record the
resolution and exact m/z's of three to five
reference peaks covering the mass range of
the descriptor. The resolution must be great-
er than or equal to 10,000, and the deviation
between the exact m/z and the theoretical m/
z (Table 8) for each exact m/z monitored
mast be less than 5 ppm.
10.2 Ion Abundance Ratios, Minimum Lev-
els, Signal-to-Noise Ratios, and Absolute Re-
tention Times—Choose an injection volume
of either 1 \iL or 2 (iL, consistent with the ca-
pability of the HRGC/HRMS instrument. In-
ject a 1 pXi or 2 p,L aliquot of the CS1 calibra-
tion solution (Table 4) using the QC condi-
tions from Section 10.1.1. If only 2,3,7,8-TCDD
and 2,3,7,8-TCDF are to be determined, the
operating conditions and specifications
below apply to analysis of those compounds
only.
10.2.1 Measure the SIGP areas for each
analyte, and compute the ion abundance ra-
tios at the exact m/z's specified In Table 8.
Compare the computed ratio to the theo-
retical ratio given in Table 9.
10.2.1.1 The exact m/z's to be monitored in
each descriptor are shown in Table 8. Each
group or descriptor shall be monitored in
succession as a function of QC retention
time to ensure that all CDDs/CDPs are de-
tected. Additional m/z's may be monitored in
each descriptor, and the m/z's may be divided
among more than the five descriptors listed
in Table 8, provided that the laboratory is
able to monitor the m/z's of all the CDDs/
CDPs that may elate from the QC in a given
retention-time window. If only 2,3,7,8-TCDD
and 2,3,7,8-TCDF are to be determined, the
descriptors may be modified to include only
the exact m/z's for the tetra-and penta-iso-
mers, the diphenyl ethers, and the lock ml
z s.
10.2.1.2 The mass spectrometer shall be
operated in a mass-drift correction mode,
using perfluorokerosene (PPK) to provide
look m/z's. The lock-mass for each group of
m/z's is shown in Table 8. Bach lock mass
shall be monitored and shall not vary by
more than ±20% throughout its respective re-
tention time window. Variations of the lock
mass by more than 20% indicate the presence
of coeluting interferences that may signifi-
cantly reduce the sensitivity of the mass
spectrometer. Beinjection of another aliquot
of the sample extract will not resolve the
problem. Additional cleanup of the extract
may be required to remove the interferences.
10.2.2 All CDDs/CDFs and labeled com-
pounds in the CS1 standard shall be within
the QC limits in Table 9 for their respective
ion abundance ratios; otherwise, the mass
spectrometer shall be adjusted and this test
repeated until the m/z ratios fall within the
limits specified. If the adjustment alters the
resolution of the mass spectrometer, resolu-
tion shall be verified (Section 10.1.2) prior to
repeat of the test.
10.2.3 Verify that the HBOC/HEMS instru-
ment meets the minimum levels in Table 2.
The peaks representing the CDDs/CDPs and
labeled compounds in the CS1 calibration
standard must have signal-to-noise ratios (S/
N) greater than or equal to 10.0. Otherwise,
the mass spectrometer shall be adjusted and
this test repeated until the minimum levels
in Table 2 are met.
10.2.4 The absolute retention time of I3d2-
1,2,3,4-TCDD (Section 7.12) shall exceed 25.0
minutes on the DB-5 column, and the reten-
tion time of 13C12-1,2,3,4-TCDD shall exceed
15.0 minutes on the DB-225 column; other-
wise, the QC temperature program shall be
adjusted and this test repeated until the
above-stated minimum retention time cri-
teria are met.
2010.3 Retention-Time Windows—Analyze
the window defining mixtures (Section 7.15)
using the optimized temperature program in
Section 10.1. Table 5 gives the elution order
(first/last) of the window-defining com-
pounds. If 2,3,7,8-TCDD and 2,3,7,8-TCDP only
are to be analyzed, this test is not required.
10.4 Isomer Specificity,
10,4.1 Analyze the isomer specificity test
standards (Section 7.15) using the procedure
in Section 14 and the optimized conditions
for sample analysis (Section 10.1.1).
10,4.2 Compute the percent valley between
the GC peaks that elute most closely to the
2,3,7,8-TCDD and TCDP isomers, on their re-
spective columns, per Figures 6 and 7.
10.4.3 Verify that the height of the valley
between the most closely elated isomers and
the 2,3,7,8-substituted isomers is less than
25% (computed as 100 x/y in Figures 6 and 7).
If the valley exceeds 25%, adjust the analyt-
ical conditions and repeat the test or replace
the GC column and recalibrate (Sections
10.1.2 through 10.7).
10.5 Calibration by Isotope Dilution—Iso-
tope dilution calibration is used for the 15
2,3,7,8-substituted CDDs/CDFs for which la-
beled compounds are added to samples prior
to extraction. The reference compound for
each CDD/CDF compound is shown in Table
2.
10,5.1 A calibration curve encompassing
the concentration range is prepared for each
compound to be determined. The relative re-
sponse (RR) (labeled to native) vs. concentra-
tion in standard solutions is plotted or com-
puted using a linear regression. Relative re-
sponse is determined according to the proce-
dures described below. Five calibration
points are employed.
10.5.2 The response of each CDD/CDF rel-
ative to its labeled analog is determined
using the area responses of both the primary
and secondary exact m/z's specified in Table
8, for each calibration standard, as follows:
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Environmental Protection Agency
Pt, 136, App. A, Meth. 1613
RR =
(Aln+A2n)C,
(All+A2l}Cn
where:
Aln and A2, = Tlie areas of the primary and
secondary m/z's for the CDD/CDF.
Ali and A2i = The areas of the primary and
secondary m/z's for the labeled compound.
Oi = The concentration of the labeled com-
pound in the calibration standard (Table
4).
C,i = The concentration of the native com-
pound in the calibration standard (Table
4),
10.5.3 To calibrate the analytical system
by isotope dilution, inject a volume of cali-
bration standards CS1 through CSS (Section
7.13 and Table 4) identical to the volume cho-
sen in Section 10,2, using the procedure in
Section 14 and the conditions In Section
10.1.1 and Table 2. Compute the relative re-
sponse (BB) at each concentration.
10.5.4 Linearity—If the relative response
for any compound is constant (less than 20%
coefficient of variation) over the five-point
calibration range, an averaged relative re-
sponse may be used for that compound; oth-
erwise, the complete calibration curve for
that compound shall be used over the five-
point calibration range.
10,6 Calibration by Internal Standard—
The internal standard method is applied to
determination of 1,2,3,7,8,9-HxCDD (Section
17.1,2), OCDP (Section 17.1.1), the non 2,3,7,8-
substituted compounds, and to the deter-
mination of labeled compounds for
intralaboratory statistics (Sections 9.4 and
15.5,4),
10.6.1 Response factors—Calibration re-
quires the determination of response factors
(BP) defined by the following equation:
(Als+A2s)Cis
(Aljs + A2is)Cs
where:
A1B and A2S = The areas of the primary and
secondary m/z's for the CDD/CDP.
Ali, and A2|S = The areas of the primary and
secondary m/z's for the internal standard.
Cls = The concentration of the internal stand-
ard (Table 4),
C5 = The concentration of the compound in
the calibration standard (Table 4).
NOTE: There Is only one m/z for "014-2,3,7,8-
TCDD. See Table 8,
10.6.2 To calibrate the analytical system
by internal standard, inject 1.0 (iL or 2.0 p.L
of calibration standards CS1 through CSS
(Section 7.13 and Table 4) using the proce-
dure in Section 14 and the conditions in Sec-
tion 10.1.1 and Table 2. Compute the response
factor (RF) at each concentration.
10.6.3 Linearity—If the response factor
(RP) for any compound is constant (less than
35% coefficient of variation) over the five-
point calibration range, an averaged re-
sponse factor may be used for that com-
pound; otherwise, the complete calibration
curve for that compound shall be used over
the five-point range.
10.7 Combined Calibration—By using cali-
bration solutions (Section 7.13 and Table 4)
containing the CDDs/CDFs and labeled com-
pounds and the internal standards, a single
set of analyses can be used to produce cali-
bration curves for the isotope dilution and
internal standard methods. These curves are
verified each shift (Section 15.3) by analyzing
the calibration verification standard (VEB,
Table 4). Becalibration is required if any of
the calibration verification criteria (Section
15.3) cannot be met,
10.8 Data Storage—MS data shall be col-
lected, recorded, and stored.
10.8.1 Data acquisition—The signal at
each exact m/z shall be collected repetitively
throughout the monitoring period and stored
on a mass storage device.
10.8.2 Response factors and multipoint
calibrations—The data system shall be used
to record and maintain lists of response fac-
tors (response ratios for isotope dilution) and
multipoint calibration curves. Computations
of relative standard deviation (coefficient of
variation) shall be used to test calibration
linearity. Statistics on initial performance
(Section 9.2) and ongoing performance (Sec-
tion 15.5) should be computed and main-
tained, either on the instrument data sys-
tem, or on a separate computer system.
11.0 Sample Preparation
11.1 Sample preparation involves modi-
fying the physical form of the sample so that
the CDDs/CDFs can be extracted efficiently.
In general, the samples must be in a liquid
form or in the form of finely divided solids in
order for efficient extraction to take place.
Table 10 lists the phases and suggested quan-
tities for extraction of various sample mat-
rices.
For samples known or expected to contain
high levels of the CDDs/CDFs, the smallest
sample size representative of the entire sam-
ple should be used (see Section 17.5).
For all samples, the blank and IPR/QPR
aliquots must be processed through the same
steps as the sample to check for contamina-
tion and losses in the preparation processes.
11.1.1 For samples that contain particles,
percent solids and particle size are deter-
mined using the procedures in Sections 11.2
and 11.3, respectively.
11.1.2 Aqueous samples—Because CDDs/
CDFs may be bound to suspended particles,
the preparation of aqueous samples is de-
pendent on the solids content of the sample.
251
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40 CFR Ch. I (7-1-04 Edition)
11.1.2.1 Aqueous samples visibly absent
particles are prepared per Section 11.4 and
extracted directly using the separatory fun-
nel or SPE techniques in Sections 12.1 or
12.2, respectively.
11.1.2.2 Aqueous samples containing visi-
ble particles and containing one percent sus-
pended solids or less are prepared using the
procedure in Section 11.4. After preparation,
the sample is extracted directly using the
SPE technique in 12.2 or filtered per Section
11.4.3. After filtration, the particles and fil-
ter are extracted using the SDS procedure in
Section 12.3 and the filtrate is extracted
using the separatory funnel procedure in
Section 12.1.
11.1.2.3 Por aqueous samples containing
greater than one percent solids, a sample ali-
quot sufficient to provide 10 g of dry solids is
used, as described in Section 11.5.
11.1,3 Solid samples are prepared using
the procedure described in Section 11.5 fol-
lowed by extraction via the SDS procedure
in Section 12.3.
11.1.4 Multiphase samples—The phase(s)
containing the CDDs/CDFs is separated from
the non-CDD/CDF phase using pressure fil-
tration and centrifugation, as described in
Section 11.6. The CDDs/CDFs will be in the
organic phase in a multiphase sample in
which an organic phase exists.
11.1.5 Procedures for grinding, homogeni-
zation, and blending of various sample
phases are given in Section 11.7.
11.1.6 Tissue samples—Preparation proce-
dures for fish and other tissues are given in
Section 11.8.
11.2 Determination of Percent Suspended
Solids.
NOTE: This aliquot is used for determining
the solids content of the sample, not for de-
termination of CDDs/CDFs.
11.2.1 Aqueous liquids and multi-phase
samples consisting of mainly an aqueous
phase.
11.2.1.1 Dessicate and weigh a GF/D filter
(Section 6.5.3) to three significant figures.
11.2.1.2 Filter 10.0±0.02 mL of well-mixed
sample through the filter.
11.2.1.3 Dry the filter a minimum of 12
hours at 110±5 °C and cool in a dessicator.
11.2.1.4 Calculate percent solids as fol-
lows:
_ weight of sample aliquot after drying (g)-weight of filter (g)
/C SOlJ.ClS ™* '""" '"'" ' mi I in I I ^ iVAJ
10 g
11.2.2 Non-aqueous liquids, solids, semi-
solid samples, and multi-phase samples In
which the main phase is not aqueous; but not
tissues.
11.2.2.1 Weigh 5-10 g of sample to three
significant figures in a tared beaker.
11.2.2.2 Dry a minimum of 12 hours at
110±5 °C, and cool in a dessicator.
11,2.2.3 Calculate percent solids as fol-
lows:
% solids =
weight of sample aliquot after drying
weight of sample aliquot before drying
xlOO
11.3 Determination of Particle Size.
11.3.1 Spread the dried sample from Sec-
tion 11.2.2.2 on a piece of filter paper or alu-
minum foil in a fume hood or glove box.
11.3.2 Estimate the size of the particles in
the sample. If the size of the largest particles
is greater than 1 mm, the particle size must
be reduced to 1 mm or less prior to extrac-
tion using the procedures in Section 11.7.
11.4 Preparation of Aqueous Samples Con-
taining 1% Suspended Solids or Less.
11.4.1 Aqueous samples visibly absent par-
ticles are prepared per the procedure below
and extracted directly using the separatory
funnel or SPE techniques in Sections 12.1 or
12.2, respectively. Aqueous samples con-
taining visible particles and one percent sus-
pended solids or less are prepared using the
procedure below and extracted using either
the SPE technique in Section 12.2 or further
prepared using the filtration procedure in
Section 11.4.3. The filtration procedure is fol-
lowed by SDS extraction of the filter and
particles (Section 12.3) and separatory funnel
extraction of the filtrate (Section 12.1). The
SPE procedure is followed by SDS extraction
of the filter and disk.
11.4.2 Preparation of sample and QC
aliquots.
11.4.2.1 Mark the original level of the
sample on the sample bottle for reference.
Weigh the sample plus bottle to ± 1.
252
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Environmental Protection Agency
Pt. 136,App. A, Meth. 1613
11.4,2.2 Spike 1.0 mL of the diluted la-
beled-compound spiking solution (Section
7.10.3) into the sample bottle. Cap the bottle
and mix the sample by careful shaking.
Allow the sample to equilibrate for one to
two hours, with occasional shaking.
11.4.2.3 For each sample or sample batch
{to a maximum of 20 samples) to be extracted
during- the same 12-hour shift, place two 1.0 L
aliquots of reagent water in clean sample
bottles or flasks.
11.4.2.4 Spike 1.0 mL of the diluted la-
beled-compound spiking solution (Section
7.10.3) Into both, reagent water aliquots. One
of these aliquots will serve as the method
blank.
11.4.2,5 Spike 1.0 mL of the PAR standard
(Section 7.14) into the remaining reagent
water aliquot. This aliquot will serve as the
OPR (Section 15.5).
11.4.2.6 If SPE is to be used, add 5 mL of
methanol to the sample, cap and shake the
sample to mix thoroughly, and proceed to
Section 12.2 for extraction. If SPE is not to
be used, and the sample is visibly absent par-
ticles, proceed to Section 12.1 for extraction.
If SPE is not to be used and the sample con-
tains visible particles, proceed to the fol-
lowing section for filtration of particles.
11.4.3 Filtration of particles.
11.4.3.1 Assemble a Buchner funnel (Sec-
tion 6.5.5) on top of a clean filtration flask.
Apply vacuum to the flask, and pour the en-
tire contents of the sample bottle through a
glass-fiber filter (Section 6.5.6) in the
Buchner funnel, swirling the sample remain-
ing in the bottle to suspend any particles.
11.4.3.2 Rinse the sample bottle twice with
approximately 5 mL portions of reagent
water to transfer any remaining particles
onto the filter.
11.4.3.3 Rinse any particles off the sides of
the Buchner funnel with small quantities of
reagent water.
11.4.3.4 Weigh the empty sample bottle to
±1 g. Determine the weight of the sample by
difference. Save the bottle for further use.
11.4.3.5 Extract the filtrate using the
separatory funnel procedure ia Section 12.1.
11.4.3.6 Extract the filter containing the
particles using the SDS procedure in Section
12.3.
11,5 Preparation of Samples Containing
Greater Than 1% Solids.
11.5.1 Weigh a well-mixed aliquot of each
sample (of the same matrix type) sufficient
to provide 10 g of dry solids (based on the sol-
ids determination in Section 11.2) into a
clean beaker or glass jar.
11.6.2 Spike 1.0 mL of the diluted labeled
compound spiking solution (Section 7.10.3)
into the sample.
11.5.3 For each sample or sample batch (to
a maximum of 20 samples) to be extracted
during the same 12-hour shift, weigh two 10 g
aliquots of the appropriate reference matrix
(Section 7.6) into clean beakers or glass jars.
11.5.4 Spike 1.0 mL of the diluted labeled
compound spiking solution (Section 7.10.3)
into each reference matrix aliquot. One ali-
quot will serve as the method blank. Spike
1.0 mL of the PAR standard (Section 7.14)
into the other reference matrix aliquot. This
aliquot will serve as the OPE (Section 15.5).
11.5.5 Stir or tumble and equilibrate the
aliquots for one to two hours.
11.5.6 Decant excess water. If necessary to
remove water, filter the sample through a
glass-fiber filter and discard the aqueous liq-
uid.
11,5.7 If particles >lmm are present in the
sample (as determined in Section 11.3.2),
spread the sample on clean aluminum foil in
a hood. After the sample is dry, grind to re-
duce the particle size (Section 11.7).
11.5.8 Extract the sample and QC aliquots
using the SDS procedure in Section 12,3.
11.6 Multiphase Samples.
11.6.1 Using the percent solids determined
in Section 11.2.1 or 11.2.2, determine the vol-
ume of sample that will provide 10 g of sol-
ids, up to 1 L of sample.
11.6.2 Pressure filter the amount of sam-
ple determined in Section 11.6.1 through
Whatman GP/D glass-fiber filter paper (Sec-
tion 6.5.3). Pressure filter the blank and OPR
aliquots through GF/D papers also. If nec-
essary to separate the phases and/or settle
the solids, centrifuge these aliquots prior to
filtration.
11.6.3 Discard any aqueous phase (if
present). Remove any non-aqueous liquid
present and reserve the maximum amount
filtered from the sample (Section 11.6.1) or 10
g, whichever is less, for combination with
the solid phase (Section 12.3.5).
11.6.4 If particles >lmm are present in the
sample (as determined in Section 11.3,2) and
the sample is capable of being dried, spread
the sample and QC aliquots on clean alu-
minum foil in a hood. After the aliquots are
dry or if the sample cannot be dried, reduce
the particle size using the procedures in Sec-
tion 11.7 and extract the reduced particles
using tne SDS procedure in Section 12.3. If
particles >lmm are not present, extract the
particles and filter in the sample and QC
aliquots directly using the SDS procedure in
Section 12.3.
11.7 Sample grinding, homogenization, or
blending—Samples with particle sizes great-
er than 1 mm (as determined in Section
11.3.2) are subjected to grinding, homogeni-
zation, or blending. The method of reducing
particle size to less than 1 mm is matrix-de-
pendent. In general, hard particles can be re-
duced by grinding with a mortar and pestle.
Softer particles can be reduced by grinding
in a Wiley mill or meat grinder, by homog-
enization, or in a blender,
11.7.1 Each size-reducing preparation pro-
cedure on each matrix shall be verified by
running the tests in Section 9.2 before the
procedure is employed routinely.
253
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Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
11.7.2 The grinding, homogenization, or
blending procedures shall be carried out in a
glove box or fume hood to prevent particles
from contaminating the work environment.
11.7.3 Grinding—Certain papers and pulps,
slurries, and amorphous solids can be ground
in a Wiley mill or heavy duty meat grinder.
In some cases, reducing the temperature of
the sample to freezing or to dry ice or liquid
nitrogen temperatures can aid in the grind-
ing process. Grind the sample aliquots from
Section 11.5.7 or 11.6.4 in a clean grinder. Do
not allow the sample temperature to exceed
50 °C, Grind the blank and reference matrix
aliquots using a clean grinder.
11.7.4 Homogenization or blending—Par-
ticles that are not ground effectively, or par-
ticles greater than 1 mm in size after grind-
ing, can often be reduced in size by high
speed homogenization or blending. Homog-
enize and/or blend the particles or filter from
Section 11.5.7 or 11.6.4 for the sample, blank,
and OPR aliquots.
11.7.5 Extract the aliquots using the SDS
procedure in Section 12.3.
11.8 Pish and Otter Tissues—Prior to
processing tissue samples, the laboratory
must determine the exact tissue to be ana-
lyzed. Common requests for analysis of fish
tissue include whole fish—skin on, whole
fish—skin removed, edible fish fillets
(filleted in the field or by the laboratory),
specific organs, and other portions. Once the
appropriate tissue has been determined, the
sample must be homogenized.
11,8.1 Homogenization.
11.8.1.1 Samples are homogenized while
still frozen, where practical. If the labora-
tory must dissect the whole fish to obtain
the appropriate tissue for analysis, the un-
used tissues may be rapidly refrozen and
stored in a clean glass jar for subsequent use.
11,8.1.2 Each analysis requires 10 g of tis-
sue (wet weight). Therefore, the laboratory
should homogenize at least 20 g of tissue to
allow for re-extraction of a second aliquot of
the same homogenized sample, if re-analysis
is required. When whole fish analysis is nec-
essary, the entire fish is homogenized.
11.8.1.3 Homogenize the sample In a tissue
homogenizer (Section 8.3.3) or grind in a
meat grinder (Section 6,3.4). Cut tissue too
large to feed into the grinder into smaller
pieces. To assure homogeneity, grind three
times.
11.8,1.4 Transfer approximately 10 g (wet
weight) of homogenized tissue to a clean,
tared, 400-500 mL beaker. For the alternate
HC1 digestion/extraction, transfer the tissue
to a clean, tared 500-600 mL wide-mouth bot-
tle. Record the weight to the nearest 10 mg.
11.8.1.5 Transfer the remaining homog-
enized tissue to a clean jar with a
fluoropolymer-lmed lid. Seal the jar and
store the tissue at <-10 °C. Return any tis-
sue that was not homogenized to its original
container and store at <-10 °C.
11.8.2 QC aliquots.
11.8.2.1 Prepare a method blank by adding
approximately 10 g of the oily liquid ref-
erence matrix (Section 7.6.4) to a 400-500 mL
beaker. For the alternate HC1 digestion/ex-
traction, add the reference matrix to a 500-
600 mL wide-mouth bottle. Record the
weight to the nearest 10 mg.
11.8.2.2 Prepare a precision and recovery
aliquot by adding approximately 10 g of the
oily liquid reference matrix (Section 7.6.4) to
a separate 400-500 mL beaker or wide-mouth
bottle, depending on the extraction proce-
dure to be used. Eecord the weight to the
nearest 10 mg. If the initial precision and re-
covery test is to be performed, use four
aliquots; if the ongoing precision and recov-
ery test is to be performed, use a single ali-
quot.
11.8.3 Spiking
11.8.3.1 Spike 1.0 mL of the labeled com-
pound spiking solution (Section 7.10.3) into
the sample, blank, and OPR aliquot.
11.8.3.2 Spike 1.0 mL of the PAR standard
(Section 7.14) Into the OPR aliquot.
11.8.4 Extract the aliquots using the pro-
cedures in Section 12.4.
12.0 Extraction and Concentration
Extraction procedures include separatory
funnel (Section 12.1) and solid phase (Section
12.2) for aqueous liquids; Soxhlet/Dean-Stark
(Section 12.3) for solids, filters, and SPB
disks; and Soxhlet extraction (Section 12.4.1)
and HC1 digestion (Section 12.4.2) for tissues.
Acid/base back-extraction (Section 12.5) is
used for initial cleanup of extracts.
Macro-concentration procedures include
rotary evaporation (Section 12.6,1), heating
mantle (Section 12.6.2), and Kuderna-Danish
(K-D) evaporation (Section 12.6.3). Micro-
concentration uses nitrogen blowdown (Sec-
tion 12.7),
12.1 Separatory funnel extraction of fil-
trates and of aqueous samples visibly absent
particles.
12.1.1 Pour the spiked sample (Section
11.4.2.2) or filtrate (Section 11.4.3.5) into a 2 L
separatory funnel. Rinse the bottle or flask
twice with 5 mL of reagent water and add
these rinses to the separatory funnel.
12.1.2 Add 60 mL methylene chloride to
the empty sample bottle (Section 12.1.1),
seal, and shake 60 seconds to rinse the inner
surface. Transfer the solvent to the sepa-
ratory funnel, and extract the sample by
shaking the funnel for two minutes with
periodic venting. Allow the organic layer to
separate from the aqueous phase for a min-
imum of 10 minutes. If an emulsion forms
and is more than one-third the volume of the
solvent layer, employ mechanical techniques
to complete the phase separation (see note
below). Drain the methylene chloride extract
254
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Environmental Protection Agency
Pt 136, App, A, Meth. 1613
through a solvent-rinsed glass funnel ap-
proximately one-half full of granular anhy-
drous sodium sulfate (Section 7.2.1) sup-
ported on clean glass-fiber paper into a sol-
vent-rinsed concentration device (Section
12.6).
NOTE: If an emulsion forms, the analyst
must employ mechanical techniques to com-
plete the phase separation. The optimum
technique depends upon the sample, but may
include stirring, filtration through, glass
wool, use of phase separation paper, cen-
trifugation, use of an ultrasonic bath with
ice, addition of NaCl, or other physical meth-
ods. Alternatively, solid-phase or other ex-
traction techniques may be used to prevent
emulsion formation. Any alternative tech-
nique is acceptable so long as the require-
ments in Section 8 are met.
Experience with aqueous samples high in
dissolved organic materials (e.g., paper mill
effluents) has shown that acidification of the
sample prior to extraction may reduce the
formation of emulsions. Paper industry
methods suggest that the addition of up to
400 mL of ethanol to a 1 L effluent sample
may also reduce emulsion formation. How-
ever, studies by EPA suggest that the effect
may be a result of sample dilution, and that
the addition of reagent water may serve the
same function. Mechanical techniques may
still he necessary to complete the phase sep-
aration. If either acidification or addition of
ethanol is utilized, the laboratory must per-
form the startup tests described in Section
9.2 using the same techniques.
12.1.3 Extract the water sample two more
times with 60 mL portions of methylene
chloride. Drain each portion through the so-
dium sulfate into the concentrator. After the
third extraction, rinse the separatory funnel
with at least 20 mL of methylene chloride,
and drain this rinse through the sodium sul-
fate into the concentrator. Repeat this rinse
at least twice. Set aside the funnel with so-
dium sulfate if the extract is to be combined
with the extract from the particles.
12.1.4 Concentrate the extract using one
of the macro-concentration procedures in
Section 12.6.
12.1.4.1 If the extract is from a sample
visibly absent particles (Section 11.1.2.1), ad-
just the final volume of the concentrated ex-
tract to approximately 10 mL with hexane,
transfer to a 250 mL separatory funnel, and
back-extract using the procedure in Section
12.5.
12,1.4.2 If the extract Is from the aqueous
filtrate (Section 11.4.3.5), set aside the con-
centration apparatus for addition of the SDS
extract from the particles (Section 12.3.9.1.2).
12.2 SPB of Samples Containing Less
Than 1% Solids (Beferences 1S-20).
12.2.1 Disk preparation.
12.2.1.1 Place an SPE disk on the base of
the filter holder (Figure 4) and wet with tol-
uene. While holding a GMF 150 filter above
the SPE disk with tweezers, wet the filter
with toluene and lay the filter on the SPB
disk, making sure that air is not trapped be-
tween the filter and disk. Clamp the filter
and SPE disk between the 1 L glass reservoir
and the vacuum filtration flask,
12.2.1.2 Rinse the sides of the filtration
flask with approx 15 mL of toluene using a
squeeze bottle or syringe. Apply vacuum mo-
mentarily until a few drops appear at the
drip tip. Release the vacuum and allow the
filter/disk to soak for approx one minute.
Apply vacuum and draw all of the toluene
through the filter/disk. Repeat the wash step
with approx 15 mL of acetone and allow the
filter/disk to air dry.
12.2.1.3 Re-wet the filter/disk with ap-
proximately 15 mL of methanol, allowing the
filter/disk to soak for approximately one
minute. Pull the methanol through the fil-
ter/disk using the vacuum, but retain a layer
of methanol approximately 1 mm thick on
the filter. Do not allow the disk to go dry
from this point until the end of the extrac-
tion.
12.2.1.4 Rinse the filter/disk with two 50-
mL portions of reagent water by adding the
water to the reservoir and pulling most
through, leaving a layer of water on the sur-
face of the filter.
12.2.2 Extraction.
12.2.2.1 Pour the spiked sample (Section
11.4.2.2), blank (Section 11.4.2.4), or IPR/OPR
aliquot (Section 11.4.2.5) into the reservoir
and turn on the vacuum to begin the extrac-
tion. Adjust the vacuum to complete the ex-
traction in no less than 10 minutes. For sam-
ples containing a high concentration of par-
ticles (suspended solids), filtration times
may be eight hours or longer.
12.2.2.2 Before all of the sample has been
palled through the filter/disk, rinse the sam-
ple bottle with approximately 50 mL of rea-
gent water to remove any solids, and pour
into the reservoir. Pull through the filter/
disk. Use additional reagent water rinses
until all visible solids are removed.
12.2.2.3 Before all of the sample and rinses
have been pulled through the filter/disk,
rinse the sides of the reservoir with small
portions of reagent water.
12.2.2.4 Allow the filter/disk to dry, then
remove the filter and disk and place in a
glass Petri dish. Extract the filter and disk
per Section 12.3.
12.3 SDS Extraction of Samples Con-
taining Particles, and of Filters and/or
Disks.
12.3.1 Charge a clean extraction thimble
(Section 6.4,2.2) with 5.0 g of 100/200 mesh sili-
ca (Section 7.5.1.1) topped with 100 g of
quartz sand (Section 7.3.2).
NOTE: Do not disturb the silica layer
throughout the extraction process.
255
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Pt, 136, App. A, Meth, 1613
40 CFR Ch. I (7-1-04 Edition)
12.3,2 Place the thimble In a clean extrac-
tor. Place 30-40 mL of toluene in the receiver
and; 200-250 mL of toluene in the flask.
12.3.3 Pre-extract the glassware by heat-
ing the flask until the toluene is boiling1.
When properly adjusted, one to two drops of
toluene will fall per second from the con-
denser tip into the receiver. Extract the ap-
paratus for a minimum of three hours.
12.3.4 After pre-extractlon, cool and dis-
assemble the apparatus. Rinse the thimble
with toluene and allow to air dry.
12.3.5 Load the wet sample, filter, and/or
disk from Section 11.4.3.6, 11.5.8, 11.6.4, 11.7.3,
11.7.4, or 12.2.2.4 and any nonaqueous liquid
from Section 11.6.3 into the thimble and
manually mix into the sand layer with a
clean metal spatula, carefully breaking up
any large lumps of sample.
12.3.6 Reassemble the pre-extracted SBS
apparatus, and add a fresh charge of toluene
to the receiver and reflux flask. Apply power
to the heating mantle to begin refluxlng. Ad-
just the reflux rate to match the rate of per-
colation through the sand and silica beds
until water removal lessens the restriction
to toluene flow. Frequently check the appa-
ratus for foaming during the first two hours
of extraction. If foaming occurs, reduce the
reflux rate until foaming subsides.
12.3.7 Drain the water from the receiver
at one to two hours and eight to nine hours,
or sooner if the receiver fills with water.
Reflux the sample for a total of 16-24 hours.
Cool and disassemble the apparatus. Record
the total volume of water collected.
12.3.8 Remove the distilling flask. Drain
the water from the Dean-Stark receiver and
add any toluene in the receiver to the ex-
tract in the flask.
12.3.9 Concentrate the extract using one
of the macro-concentration procedures in
Section 12.6 per the following:
12.3.9.1 Extracts from the particles in an
aqueous sample containing less than 1% sol-
ids (Section 11.4.3.6).
12.3.9.1.1 Concentrate the extract to ap-
proximately 5 mL using the rotary evapo-
rator or heating mantle procedures in Sec-
tion 12.6.1 or 12.6.2.
12.3.9.1.2 Quantitatively transfer the ex-
tract through the sodium sulfate (Section
12.1.3) into the apparatus that was set aside
(Section 12.1.4.2) and reconcentrate to the
level of the toluene.
12.3.9.1.3 Adjust to approximately 10 mL
with hexane, transfer to a 250 mL separatory
funnel, and proceed with back-extraction
(Section 12.5).
12.3.9.2 Extracts from particles (Sections
11.5 through 11.6) or from the SPE filter and
disk (Section 12.2.2.4)—Concentrate to ap-
proximately 10 mL using the rotary evapo-
rator or heating mantle (Section 12.6.1 or
12.6.2), transfer to a 250 mL separatory fun-
nel, and proceed with back-extraction (Sec-
tion 12.5).
12.4 Extraction of Tissue—Two procedures
are provided for tissue extraction.
12.4.1 Soxhlet extraction (Reference 21).
12.4.1.1 Add 30-40 g of powdered anhydrous
sodium sulfate to each of the beakers (Sec-
tion 11.8.4) and mix thoroughly. Cover the
beakers with aluminum foil and allow to
equilibrate for 12-24 hours. Remix prior to
extraction to prevent clumping.
12.4.1.2 Assemble and pre-extract the
Soxhlet apparatus per Sections 12.3.1
through 12.3.4, except use the methylene
Ohloride:hexane (1:1) mixture for the pre-ex-
traction and rinsing and omit the quartz
sand. The Dean-Stark moisture trap may
also be omitted, if desired.
12.4.1.3 Reassemble the pre-extracted
Soxhlet apparatus and add a fresh charge of
methylene chloride:hexane to the reflux
flask.
12.4.1.4 Transfer the sample/sodium sul-
fate mixture (Section 12.4.1.1) to the Soxhlet
thimble, and install the thimble in the Soxh-
let apparatus.
12.4.1.5 Rinse the beaker with several
portions of solvent mixture and add to the
thimble. Pill the thimble/receiver with sol-
vent. Extract for 18-24 hours.
12.4.1.6 After extraction, cool and dis-
assemble the apparatus.
12,4.1.7 Quantitatively transfer the ex-
tract to a macro-concentration device (Sec-
tion 12.6), and concentrate to near dryness.
Set aside the concentration apparatus for re-
use.
12.4.1.8 Complete the removal of the sol-
vent using the nitrogen blowdown procedure
(Section 12.7) and a water bath temperature
of 60 °C. Weigh the receiver, record the
weight, and return the receiver to the blow-
down apparatus, concentrating the residue
until a constant weight is obtained.
12.4.1.9 Percent lipid determination—The
lipid content is determined by extraction of
tissue with the same solvent system (meth-
ylene chloride:hexane) that was used in
EPA's National Dioxin Study (Reference 22)
so that lipid contents are consistent with
that study.
12.4.1.9.1 Redissolve the residue in the re-
ceiver in hexane and spike 1.0 mL of the
cleanup standard (Section 7.11) into the solu-
tion.
12.4.1.9.2 Transfer the residue/hexane to
the anthropogenic isolation column (Section
13.7.1) or bottle for the acidified silica gel
batch cleanup (Section 13.7.2), retaining the
boiling chips in the concentration apparatus.
Use several rinses to assure that all material
is transferred. If necessary, sonicate or heat
the receiver slightly to assure that all mate-
rial is re-dissolved. Allow the receiver to dry.
Weigh the receiver and boiling chips.
12.4.1.9.3 Calculate the lipid content to
the nearest three significant figures as fol-
lows:
256
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
Percent lipid =
Weight of residue (g)
Weight of tissue (g)
xlOO
12.4.1,9.4 It is not necessary to determine
the lipid content of the blank, IPR, or OPR
aliqnots,
12.4.2 HC1 digestion/extraction and con-
centration (References 23-26).
12.4.2.1 Add 200 mL of 6 N HC1 and 200 mL
of methylene ehloride:hexane (1:1) to the
sample and QC aliquots (Section 11.8.4).
12.4.2.2 Cap and shake each bottle one to
three times. Loosen the cap in a hood to vent
excess pressure. Shake each bottle for 10-30
seconds and vent.
12.4.2.3 Tightly cap and place on shaker.
Adjust the shaker action and speed so that
the acid, solvent, and tissue are in constant
motion. However, take oare to avoid such
violent action that the bottle may be dis-
lodged from the shaker. Shake for 12-24
hours.
12.4.2.4 After digestion, remove the bot-
tles from the shaker. Allow the bottles to
stand so that the solvent and acid layers sep-
arate.
12.4.2.5 Decant the solvent through a glass
funnel with glass-fiber filter (Sections 6.5.2
through 6,5.3) containing approximately 10 g
of granular anhydrous sodium sulfate (Sec-
tion 7.2.1) into a macro-concentration appa-
ratus (Section 12.6). Rinse the contents of
the bottle with two 25 mL portions of hexane
and pour through the sodium sulfate into the
apparatus.
12.4.2.6 Concentrate the solvent to near
dryness using a macro-concentration proce-
dure (Section 12.6).
12,4.2.7 Complete the removal of the sol-
vent using the nitrogen blowdown apparatus
(Section 12.7) and a water bath temperature
of 60 "C, Weigh the receiver, record the
weight, and return the receiver to the blow-
down apparatus, concentrating the residue
until a constant weight is obtained,
12.4,2.8 Percent lipid determination—The
lipid content is determined in the same sol-
vent system [methylene chloriderhexane
(1:1)] that was used in BPA's National Dioxln
Study (Reference 22) so that lipid contents
are consistent with that study.
12,4.2.8.1 Redissolve the residue in the re-
ceiver in hexane and spike 1.0 mL of the
cleanup standard (Section 7.11) into the solu-
tion.
12,4.2.8.2 Transfer the residue/hexane to
the narrow-mouth 100-200 mL bottle retain-
ing the boiling chips in the receiver. Use sev-
eral rinses to assure that all material is
transferred, to a maximum hexane volume of
approximately 70 mL. Allow the receiver to
dry. Weigh the receiver and boiling chips.
12.4.2.8.3 Calculate the percent lipid per
Section 12.4,1.9.3. It is not necessary to deter-
mine the lipid content of the blank, IPR, or
OPR aliquots.
12.4.2.9 Clean up the extract per Section
13.7.3.
12.5 Back-Extraction with Base and Acid.
12,5,1 Spike 1.0 mL of the cleanup stand-
ard (Section 7,11) Into the separatory funnels
containing the sample and QC extracts from
Section 12.1.4.1,12.3.9.1.3, or 12.3.9.2.
12.5,2 Partition the extract against 50 mL
of potassium hydroxide solution (Section
7.1,1), Shake for two minutes with periodic
venting into a hood. Remove and discard the
aqueous layer. Repeat the base washing until
no color is visible in the aqueous layer, to a
maximum of four washings. Minimize con-
tact time between the extract and the base
to prevent degradation of the CDDs/CDFs.
Stronger potassium hydroxide solutions may
be employed for back-extraction, provided
that the laboratory meets the specifications
for labeled compound recovery and dem-
onstrates acceptable performance using the
procedure in Section 9,2.
12.5.3 Partition the extract against 50 mL
of sodium chloride solution (Section 7.1.4) in
the same way as with base. Discard the aque-
ous layer.
12.5.4 Partition the extract against 50 mL
of sulfuric acid (Section 7.1.2) in the same
way as with base. Repeat the acid washing
until no color is visible in the aqueous layer,
to a maximum of four washings.
12.5.5 Repeat the partitioning against so-
dium chloride solution and discard the aque-
ous layer.
12,5,6 Pour each extract through a drying
column containing 7-10 cm of granular anhy-
drous sodium sulfate (Section 7.2.1). Rinse
the separatory funnel with 30-50 mL of sol-
vent, and pour through the drying column.
Collect each extract in a round-bottom flask.
Re-concentrate the sample and QC aliquots
per Sections 12.6 through 12.7, and clean up
the samples and QC aliquots per Section 13.
12.6 Macro-Concentration—Extracts in
toluene are concentrated using a rotary
evaporator or a heating mantle; extracts in
methylene chloride or hexane are con-
centrated using a rotary evaporator, heating
mantle, or Kuderna-Danish apparatus.
12.6,1 Rotary evaporation—Concentrate
the extracts in separate round-bottom
flasks.
12.6.1.1 Assemble the rotary evaporator
according to manufacturer's instructions,
and warm the water bath to 45 "C. On a daily
basis, preclean the rotary evaporator by con-
centrating 100 mL of clean extraction sol-
vent through the system. Archive both the
concentrated solvent and the solvent in the
catch flask for a contamination check if nec-
essary. Between samples, three 2-3 mL
aliquots of solvent should be rinsed down the
feed tube into a waste beaker.
12.6.1.2 Attach the round-bottom flask
containing the sample extract to the rotary
evaporator. Slowly apply vacuum to the sys-
tem, and begin rotating the sample flask.
257
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Pt. 136,App. A,Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
12,6,1.3 Lower the flask into the water
bath, and adjust the speed of rotation and
the temperature as required to complete con-
centration in 15-20 mimrtes. At the proper
rate of concentration, the flow of solvent
into the receiving flask will be steady, but
no bumping or visible boiling of the extract
will occur,
NOTE: If the rate of concentration is too
fast, analyte loss may occur.
12.6.1.4 When the liquid in the concentra-
tion flask has reached an apparent volume of
approximately 2 mL, remove the flask from
the water bath and stop the rotation. Slowly
and carefully admit air into the system. Be
sure not to open the valve so quickly that
the sample is blown out of the flask. Rinse
the feed tube with approximately 2 mL of
solvent.
12,6.1.5 Proceed to Section 12.6.4 for prepa-
ration for back-extraction or micro-con-
centration and solvent exchange.
12.6.2 Heating mantle—Concentrate the
extracts in separate round-bottom flasks.
12.6.2.1 Add one or two clean boiling chips
to the round-bottom flask, and attach a
three-ball macro Snyder column. Prewet the
column by adding approximately 1 mL of sol-
vent through the top. Place the round-bot-
tom flask In a heating mantle, and apply
heat as required to complete the concentra-
tion in 15-20 minutes. At the proper rate of
distillation, the balls of the column will ac-
tively chatter, but the chambers will not
flood.
12,6.2.2 When the liquid has reached an ap-
parent volume of approximately 10 mL, re-
move the round-bottom flask from the heat-
ing mantle and allow the solvent to drain
and cool for at least 10 minutes. Remove the
Snyder column and rinse the glass joint into
the receiver with small portions of solvent.
12.6.2.3 Proceed to Section 12.6.4 for prepa-
ration for back-extraction or micro-con-
centration and solvent exchange,
12.6.3 Kuderna-Danish (K-D)—Concentrate
the extracts in separate 500 mL K-D flasks
equipped with 10 mL concentrator tabes. The
K-D technique is used for solvents such as
methylene chloride and hexane. Toluene is
difficult to concentrate using the K-D tech-
nique unless a water bath fed by a steam
generator is used.
12.6,3.1 Add one to two clean boiling chips
to the receiver. Attach a three-ball macro
Snyder column. Prewet the column by add-
ing- approximately 1 mL of solvent through
the top. Place the K-D apparatus in a hot
water bath so that the entire lower rounded
surface of the flask is bathed with steam.
12.6,3.2 Adjust the vertical position of the
apparatus and the water temperature as re-
quired to complete the concentration in 15-20
minutes. At the proper rate of distillation,
the balls of the column will actively chatter
but the chambers will not flood.
12.6.3.3 When the liquid has reached an ap-
parent volume of 1 mL, remove the K-D ap-
paratus from the bath and allow the solvent
to drain and cool for at least 10 minutes. Re-
move the Snyder column and rinse the flask
and its lower joint into the concentrator
tube with 1-2 mL of solvent. A 5 mL syringe
is recommended for this operation.
12.6.3,4 Remove the three-ball Snyder col-
umn, add a fresh boiling chip, and attach a
two-ball micro Snyder column to the concen-
trator tube. Prewet the column by adding
approximately 0.5 mL of solvent through the
top. Place the apparatus in the hot water
bath.
12,6.3.5 Adjust the vertical position and
the water temperature as required to com-
plete the concentration in 5-10 minutes. At
the proper rate of distillation, the balls of
the column will actively chatter but the
chambers will not flood.
12.6.3.6 When the liquid reaches an appar-
ent volume of 0.5 mL, remove the apparatus
from the water bath and allow to drain and
cool for at least 10 minutes.
12,6.3.7 Proceed to 12.6,4 for preparation
for back-extraction or micro-concentration
and solvent exchange.
12,6,4 Preparation for back-extraction or
micro-concentration and solvent exchange.
12.6.4.1 For back-extraction (Section 12.5),
transfer the extract to a 250 mL separatory
funnel. Rinse the concentration vessel with
small portions of hexane, adjust the hexane
volume In the separatory funnel to 10-20 mL,
and proceed to back-extraction (Section
12.5).
12.6.4.2 For determination of the weight of
residue in the extract, or for clean-up proce-
dures other than back-extraction, transfer
the extract to a blowdown vial using two to
three rinses of solvent. Proceed with micro-
concentration and solvent exchange (Section
12.7),
12.7 Micro-Concentration and Solvent Ex-
change,
12.7,1 Extracts to be subjected to G-PC or
HPLC cleanup are exchanged into methylene
chloride. Extracts to be cleaned up using sili-
ca gel, alumina, carbon, and/or Florisil are
exchanged into hexane.
12,7.2 Transfer the vial containing- the
sample extract to a nitrogen blowdown de-
vice. Adjust the flow of nitrogen so that the
surface of the solvent is just visibly dis-
turbed.
NOTE: A large vortex in the solvent may
cause analyte loss.
12.7.3 Lower the vial into a 45 °C water
bath and continue concentrating.
12.7.3.1 If the extract is to be con-
centrated to dryness for weight determina-
tion (Sections 12.4.1.8, 12.4.2.7, and 13.7.1.4),
blow dry until a constant weight is obtained.
12,7.3.2 If the extract is to be con-
centrated for injection into the GO/MS or the
258
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Environmental Protection Agency
Pt, 136, App, A, Meth. 1613
solvent is to be exchanged for extract clean-
up, proceed as follows:
12.7.4 When the volume of the liquid is ap-
proximately 100 L, add 2-3 mL of the desired
solvent (methylene chloride for OPC and
HPLC, or hexane for the other cleanups) and
continue concentration to approximately 100
^L. Repeat the addition of solvent and con-
centrate onoe more.
12.7.5 If the extract Is to be cleaned up by
GPC, adjust the volume of the extract to 5.0
mL with methylene chloride. If the extract
is to be cleaned up by HPLC, further con-
centrate the extract to 30 uL. Proceed with
GPC or HPLC cleanup (Section 13.2 or 13.6,
respectively).
12.7,6 If tie extract is to be cleaned up by
column ehromatography (alumina, silica gel,
Carbopak/Celite, or Florisil), bring the final
volume to 1.0 mL with hexane. Proceed with
column cleanups (Sections 13.3 through 13.5
and 13.8).
12.7.7 If the extract is to be concentrated
for injection into the GC/MS (Section 14),
quantitatively transfer the extract to a 0.3
mL conical vial for final concentration, rins-
ing the larger vial with hexane and adding
the rinse to the conical vial. Reduce the vol-
ume to approximately 100 |iL. Add 10 jiL of
nonane to the vial, and evaporate the solvent
to the level of the nonane. Seal the vial and
label with the sample number. Store in the
dark at room temperature until ready for
GC/MS analysis. If GC/MS analysis will not
be performed on the same day, store the vial
at <-10°C,
13.0 Extract Cleanup
13,1 Cleanup may not be necessary for rel-
atively clean samples (e.g., treated effluents,
groundwater, drinking water). If particular
circumstances require the use of a cleanup
procedure, the analyst may use any or all of
the procedures below or any other appro-
priate procedure. Before using a cleanup pro-
cedure, the analyst must demonstrate that
the requirements of Section 9.2 can be met
using the cleanup procedure. If only 2,3,7,8-
TCDD and 2,3,7,8-TCDF are to be determined,
the cleanup procedures may be optimized for
isolation of these two compounds.
13.1.1 Gel permeation ehromatography
(Section 13.2) removes high molecular weight
interferences that cause OC column perform-
ance to degrade. It should be used for all soil
and sediment extracts and may be used for
water extracts that are expected to contain
high molecular weight organic compounds
(e.g., polymeric materials, humic acids).
13.1.2 Acid, neutral, and basic silica gel
(Section 13.3), alumina (Section 13.4), and
Florisil (Section 13.8) are used to remove
nonpolar and polar interferences. Alumina
and Florisil are used to remove
chlorodiphenyl ethers.
13.1.3 Carbopak/Celite (Section 13.5) is
used to remove nonpolar interferences.
13.1.4 HPLC (Section 13.6) is used to pro-
vide specificity for the 2,3,7,8-substituted and
other CDD and CDF isomers.
13.1.5 The anthropogenic isolation column
(Section 13.7.1), acidified silica gel batch ad-
sorption procedure (Section 13.7.2), and sul-
furic acid and base back-extraction (Section
13.7.3) are used for removal of lipids from tis-
sue samples.
13.2 Gel Permeation Chromatography
(GPC).
13.2.1 Column packing.
13.2.1.1 Place 70-76 g of SX-3 Bio-beads
(Section 6.7.1.1) in a 400-500 mL beaker,
13.2.1.2 Cover the beads with methylene
chloride and allow to swell overnight (a min-
imum of 12 hours).
13.2.1.3 Transfer the swelled beads to the
column (Section 6.7.1.1) and pump solvent
through the column, from bottom to top, at
4.5-5.5 mL/minute prior to connecting the
column to the detector.
13.2.1.4 After purging the column with sol-
vent for one to two hours, adjust the column
head pressure to 7-10 psig and purge for four
to five hours to remove air. Maintain a head
pressure of 7-10 psig. Connect the column to
the detector (Section 6,7.1.4).
13.2.2 Column calibration.
13.2.2.1 Load 5 mL of the calibration solu-
tion (Section 7.4) into the sample loop.
13.2.2,2 Inject the calibration solution and
record the signal from the detector. The
elution pattern will be corn oil, bis(2-ethyl
hexyDphthalate, pentaehlorophenol, pery-
lene, and sulfur.
13.2.2.3 Set the "dump time" to allow >85%
removal of the corn oil and >85% collection
of the phthalate,
13.2.2.4 Set the "collect time" to the peak
minimum between perylene and sulfur.
13.2.2.5 Verify the calibration with the
calibration solution after every 20 extracts.
Calibration is verified if the recovery of the
pentaehlorophenol is greater than 85%. If
calibration is not verified, the system shall
be recalibrated using the calibration solu-
tion, and the previous 20 samples shall be re-
extracted and cleaned up using the cali-
brated GPC system.
13.2.3 Extract cleanup—GPC requires that
the column not be overloaded. The column
specified in this method is designed to han-
dle a maximum of 0.5 g of high molecular
weight material in a 5 mL extract. If the ex-
tract is known or expected to contain more
than 0.5 g, the extract is split into aliquots
for GPC, and the aliquots are combined after
elution from the column. The residue con-
tent of the extract may be obtained gravi-
metrically by evaporating the solvent from a
50 }iL aliquot.
13.2.3.1 Filter the extract or load through
the filter holder (Section 6.7.1.3) to remove
the particles. Load the 5.0 mL extract onto
the column.
259
-------
Pf. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
13.2.3.2 Elute the extract using the cali-
bration data determined in Section 13.2.2.
Collect the eluate in a clean 400-500 mL
beaker.
13.2.3.3 Rinse the sample loading1 tube
thoroughly with methylene chloride between
extracts to prepare for the next sample.
13.2.3.4 If a particularly dirty extract is
encountered, a 5.0 mL methylene chloride
blank shall be run through the system to
check for carry-over.
13.2.3.5 Concentrate the eluate per Sec-
tions 12.6 and 12.7 for further cleanup or in-
jection into the GC/MS,
13.3 Silica Gel Cleanup.
13.3.1 Place a glass-wool plug in a 15 mm
ID ohromatography column (Section 6.7.4.2).
Pack the column bottom to top with: 1 g sili-
ca gel (Section 7.5.1.1), 4 g basic silica gel
(Section 7.5.1.3), 1 g silica gel, 8 g acid silica
gel (Section 7.5.1.2), 2 g silica gel, and 4 g
granular anhydrous sodium sulfate (Section
7.2.1). Tap the column to settle the adsorb-
ents.
13.3.2 Pre-elute the column with 50-100
mL of hexane, Close the stopcock when the
hexane is within 1 mm of the sodium sulfate.
Discard the eluate. Check the column for
channeling. If channeling Is present, discard
the column and prepare another.
13.3.3 Apply the concentrated extract to
the column. Open the stopcock until the ex-
tract is within 1 mm of the sodium sulfate.
13.3.4 Rinse the receiver twice with 1 mL
portions of hexane, and apply separately to
the column. Elute the CDDs/CDFs with 100
mL hexane, and collect the eluate.
13.3.5 Concentrate the eluate per Sections
12.6 and 12.7 for further cleanup or injection
into the HPLC or GC/MS.
13.3.6 For extracts of samples known to
contain large quantities of other organic
compounds (such as paper mill effluents), it
may be advisable to increase the capacity of
the silica gel column. This may be accom-
plished by increasing the strengths of the
acid and basic silica gels. The acid silica gel
(Section 7.5.1.2) may be increased in strength
to as much as 44% w/w (7.9 g sulfuric acid
added to 10 g silica gel). The basic silica gel
(Section 7.5.1.3) may be increased in strength
to as much as 33% w/w (50 mL IN NaOH
added to 100 g silica gel), or the potassium
silicate (Section 7.5.1.4) may be used.
NOTE: The use of stronger acid silica gel
(44% w/w) may lead to charring of organic
compounds in some extracts. The charred
material may retain some of the analytes
and lead to lower recoveries of CDDs/CDFs.
Increasing the strengths of the acid and
basic silica gel may also require different
volumes of hexane than those specified above
to elute the analytes off the column. There-
fore, the performance of the method after
such modifications must be verified by the
procedure in Section 9.2.
13.4 Alumina Cleanup.
13.4.1 Place a glass-wool ping in a 15 mm
ID chromatogrraphy column (Section 6.7.4.2).
13.4.2 If using acid alumina, pack the col-
umn by adding 6 g acid alumina (Section
7.5.2.1). If using basic alumina, substitute 6 g
basic alumina (Section 7.5.2.2). Tap the col-
umn to settle the adsorbents.
13.4.3 Pre-elute the column with 50-100
mL of hexane. Close the stopcock when the
hexane is within 1 mm of the alumina.
13.4.4 Discard the eluate. Check the col-
umn for channeling. If channeling is present,
discard the column and prepare another.
13.4.5 Apply the concentrated extract to
the column. Open the stopcock until the ex-
tract is within 1 mm of the alumina.
13.4.6 Rinse the receiver twice with 1 mL
portions of hexane and apply separately to
the column. Elate the interfering compounds
with 100 mL hexane and discard the eluate.
13.4.7 The choice of eluting solvents will
depend on the choice of alumina (acid or
basic) made in Section 13.4.2.
13.4.7.1 If using acid alumina, elute the
CDDs/CDFs from the column with 20 mL
methylene ehloride:hexane (20:80 v/v). Collect
the eluate.
13.4.7.2 If using basic alumina, elute the
CDDs/CDFs from the column with 20 mL
methylene chloride:hexane (50:50 v/v). Collect
the eluate,
13.4.8 Concentrate the eluate per Sections
12.6 and 12.7 for further cleanup or injection
into the HPLC or GC/MS.
13.5 Carbon Column.
13.5.1 Cut both ends from a 10 mL dispos-
able serological pipet (Section 6.7.3.2) to
produce a 10 cm column. Fire-polish both
ends and flare both ends if desired. Insert a
glass-wool plug at one end, and pack the col-
umn with 0.55 g of Carbopak/Celite (Section
7.5.3.3) to form an adsorbent bed approxi-
mately 2 cm long. Insert a glass-wool plug on
top of the bed to hold the adsorbent in place.
13.5.2 Pre-elute the column with 5 mL of
toluene followed by 2 mL of methylene chlo-
ride: methanol:toluene (15:4:1 v/v), 1 mL of
methylene enloride:eyelohexane (1:1 v/v), and
5 mL of hexane. If the flow rate of eluate ex-
ceeds 0.5 mL/minute, discard the column.
13.5.3 When the solvent is within 1 mm of
the column packing, apply the sample ex-
tract to the column. Rinse the sample con-
tainer twice with 1 mL portions of hexane
and apply separately to the column. Apply 2
mL of hexane to complete the transfer.
13,5.4 Elute the interfering compounds
with two 3 mL portions of hexane, 2 inL of
methylene ehloride:cyclohexane (1:1 v/v), and
2 mL of methylene chlo-
ride:methanol:toluene (15:4:1 v/v). Discard
the eluate.
13.5.5 Invert the column, and elute the
CDDs/CDFs with 20 mL of toluene. If carbon
particles are present in the eluate, filter
through glass-fiber filter paper.
260
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
13,5.6 Concentrate the eluate per Sections
12,6 and 12.7 for further cleanup or injection
Into the HPLC or GC/MS.
13.6 HPLC (Reference 6).
13.6,1 Column calibration.
13.6.1.1 Prepare a calibration standard
containing the 2,3,7,8-substituted isomers
and/or other isomers of interest at a con-
centration of approximately 500 pg/nL in
methylene chloride,
13.6.1.2 Inject 30 nL of the calibration so-
lution into the HPLC and record the signal
from the detector. Collect the eluant for
reuse. The elution order will be the tetra-
through octa-isomers.
13.6.1.3 Establish the collection time for
the tetra-isomers and for the other isomers
of interest. Following calibration, flush the
injection system with copious quantities of
methylene chloride, including a minimum of
five 50 uL injections while the detector is
monitored, to ensure that residual CDDs/
CDPs are removed from the system.
13.6.1.4 Verify the calibration with the
calibration solution after every 20 extracts.
Calibration is verified if the recovery of the
CDDs/CDPs from the calibration standard
(Section 13.6,1.1) is 75-125% compared to the
calibration (Section 13,6.1.2), If calibration is
not verified, the system shall be recalibrated
usingr the calibration solution, and the pre-
vious 20 samples shall be re-extracted and
cleaned up using the calibrated system.
13.6.2 Extract cleanup—HPLC requires
that the column not be overloaded. The col-
umn specified in this method is designed to
handle a maximum of 30 uL of extract. If the
extract cannot be concentrated to less than
30 (iL, it is split into fractions and the frac-
tions are combined after elution from the
column.
13.6.2.1 Rinse the sides of the vial twice
with 30 nL of methylene chloride and reduce
to 30 |ii with the evaporation apparatus
(Section 12.7),
13.6.2.2 Inject the 30 (iL extract into the
HPLC.
13.6.2,3 Blute the extract using the cali-
bration data determined in Section 13.6.1,
Collect the fraetion(s) in a clean 20 mL con-
centrator tube containing 5 mL of
hexane;acetone (1:1 v/v).
13.6.2.4 If an extract eoataining greater
than 100 ng/mL of total ODD or CDF is en-
countered, a 30 |iL methylene chloride blank
shall be run through the system to check for
carry-over.
13.6.2.5 Concentrate the eluate per Sec-
tion 12.7 for injection into the GC/MS,
13.7 Cleanup of Tissue Lipids—Lipids are
removed from the Soxhlet extract using ei-
ther the anthropogenic isolation column
(Section 13,7.1) or acidified silica gel (Section
13.7.2), or are removed from the HC1 digested
extract using sulfuric acid and base back-ex-
traction (Section 13.7,3),
13,7.1 Anthropogenic isolation column
(References 22 and 27)—Used for removal of
lipids from the Soxhlet/SDS extraction (Sec-
tion 12.4.1),
13.7.1.1 Prepare the column as given in
Section 7.5.4.
13.7.1.2 Pre-elute the column with 100 mL
of hexane. Drain the hexane layer to the top
of the column, but do not expose the sodium
sulfate,
13.7.1.3 Load the sample and rinses (Sec-
tion 12.4.1,9.2) onto the column by draining
each portion to the top of the bed. Elute the
CDDs/CDFs from the column into the appa-
ratus used for concentration (Section
12.4.1.7) using 200 mL of hexane.
13.7.1.4 Concentrate the cleaned up ex-
tract (Sections 12.6 through 12.7) to constant
weight per Section 12.7.3.1. If more than 500
mg of material remains, repeat the cleanup
using a fresh anthropogenic isolation col-
umn.
13.7,1.5 Redissolve the extract in a solvent
suitable for the additional cleanups to be
used (Sections 13.2 through 13.6 and 13.8).
13.7.1.6 Spike 1.0 mL of the cleanup stand-
ard (Section 7.11) into the residue/solvent.
13.7.1.7 Clean up the extract using the pro-
cedures in Sections 13.2 through 13.6 and 13,8.
Alumina (Section 13.4) or Florisil (Section
13,8) and carbon (Section 13.5) are rec-
ommended as minimum additional cleanup
steps.
13.7.1.8 Following cleanup, concentrate
the extract to 10 p.L as described in Section
12.7 and proceed with the analysis in Section
14.
13.7.2 Acidified silica gel (Reference 28)—
Procedure alternate to the anthropogenic
isolation column (Section 13.7.1) that is used
for removal of lipids from the Soxhlet/SDS
extraction (Section 12.4.1).
13.7.2,1 Adjust the volume of hexane in
the bottle (Section 12.4.1.9.2) to approxi-
mately 200 mL.
13.7.2.2 Spike 1.0 mL of the cleanup stand-
ard (Section 7,11) into the residue/solvent.
13.7.2.3 Drop the stirring bar into the bot-
tle, place the bottle on the stirring plate,
and begin stirring.
13.7.2.4 Add 30-100 g of acid silica gel (Sec-
tion 7,5.1.2) to the bottle while stirring,
keeping the silica gel in motion. Stir for two
to three hours.
NOTE: 30 grams of silica gel should be ade-
quate for most samples and will minimize
contamination from this source.
13.7.2.5 After stirring, pour the extract
through approximately 10 g of granular an-
hydrous sodium sulfate (Section 7.2.1) con-
tained in a funnel with, glass-fiber filter into
a macro contration device (Section 12.6).
Einse the bottle and sodium sulfate with
hexane to complete the transfer.
261
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Pf. 136, App. A, Meth. 1613
40 CFR Ch. 1 (7-1-04 Edition)
13.7.2.6 Concentrate the extract per Sec-
tions 12.6 through 12.7 and clean up the ex-
tract using the procedures in Sections 13.2
through 13.6 and 13.8. Alumina (Section 13.4)
or Plorisil (Section 13.8) and carbon (Section
13.5) are recommended as minimum addi-
tional cleanup steps.
13.7.3 Sulfuric acid and base back-extrac-
tion. Used with HC1 digested extracts (Sec-
tion 12.4.2).
13.7.3.1 Spike 1.0 mL of the cleanup stand-
ard (Section 7.11) into the residue/solvent
(Section 12.4.2.8.2).
13.7.3.2 Add 10 mL of concentrated sul-
furic acid to the bottle. Immediately cap and
sbake one to three times. Loosen cap in a
hood to vent excess pressure. Cap and shake
the bottle so that the residue/solvent is ex-
posed to the acid for a total time of approxi-
mately 45 seconds.
13.7.3.3 Decant the hexane into a 250 mL
separatory funnel making sure that no acid
is transferred. Complete the quantitative
transfer with several hexane rinses.
13.7.3.4 Back extract the solvent/residue
with 50 mL of potassium hydroxide solution
per Section 12.5.2, followed by two reagent
water rinses.
13.7.3.5 Drain the extract through a filter
funnel containing approximately 10 g of
granular anhydrous sodium sulfate in a
glass-fiber filter into a macro concentration
device (Section 12.6).
13.7,3.6 Concentrate the cleaned up ex-
tract to a volume suitable for the additional
cleanups given in Sections 13.2 through 13.6
and 13.8. Gel permeation chromatograptty
(Section 13.2), alumina (Section 13.4) or
Florisil (Section 13.8), and Carbopak/Celite
(Section 13.5) are recommended as minimum
additional cleanup steps.
13.7.3.7 Following cleanup, concentrate
the extract to 10 L as described in Section
12.7 and proceed with analysis per Section 14.
13.8 Plorisil Cleanup (Reference 29).
13.8.1 Pre-elute the activated Florisil col-
umn (Section 7.5.3) with 10 mL of methylene
chloride followed by 10 mL of
hexane:methylene chloride (98:2 v/v) and dis-
card the solvents.
13.8.2 When the solvent is within 1 mm of
the packing, apply the sample extract (in
hexane) to the column. Einse the sample
container twice with 1 mL portions of
hexane and apply to the column.
13.8.3 Elute the interfering compounds
with 20 mL of hexane:methylene chloride
(98:2) and discard the eluate.
13.8.4 Elute the CDDs/CDFs with 35 mL of
methylene chloride and collect the eluate.
Concentrate the eluate per Sections 12.6
through 12.7 for further cleanup or for injec-
tion into the HPLC or GO/MS.
14.0 HRGC/HRMS Analysis
14.1 Establish the operating conditions
given in Section 10.1.
14.2 Add 10 uL of the appropriate internal
standard solution (Section 7.12) to the sam-
ple extract immediately prior to injection to
minimize the possibility of loss by evapo-
ration, adsorption, or reaction. If an extract
is to be reanalyzed and evaporation has oc-
curred, do not add more instrument internal
standard solution. Rather, bring the extract
back to its previous volume (e.g., 19 L) with
pure nonane only (18 L if 2 L injections are
used).
14.3 Inject 1.0 |iL or 2.0 |iL of the con-
centrated extract containing the internal
standard solution, using on-column or
splitless injection. The volume injected must
be identical to the volume used for calibra-
tion (Section 10). Start the GC column ini-
tial isothermal hold upon injection. Start
MS data collection after the solvent peak
elutes. Stop data collection after the OCDD
and OCDP have eluted. If only 2,3,7,8-TCDD
and 2,3,7,8-TCDF are to be determined, stop
data collection after elution of these com-
pounds. Return the column to the initial
temperature for analysis of the next extract
or standard.
75.0 System and Laboratory Performance
15.1 At the beginning of each 12-hour shift
during which analyses are performed, GC/MS
system performance and calibration are
verified for all CDDs/CDFs and labeled com-
pounds. For these tests, analysis of the CSS
calibration verification (VER) standard (Sec-
tion 7.13 and Table 4) and the isomer speci-
ficity test standards (Section 7.15 and Table
5) shall be used to verify all performance cri-
teria. Adjustment and/or recalibration (Sec-
tion 10) shall be performed until all perform-
ance criteria are met. Only after all perform-
ance criteria are met may samples, blanks,
IPRs, and OPRs be analyzed.
15.2 MS Resolution—A static resolving
power of at least 10,000 (10% valley defini-
tion) must be demonstrated at the appro-
priate m/z before any analysis is performed.
Static resolving power checks must be per-
formed at the beginning and at the end of
each 12-hour shift according to procedures in
Section 10,1.2. Corrective actions must be
implemented whenever the resolving power
does not meet the requirement.
15.3 Calibration Verification.
15.3.1 Inject the VER standard using the
procedure in Section 14.
15.3.2 The m/z abundance ratios for all
CDDs/CDFs shall be within the limits in
Table 9; otherwise, the mass spectrometer
shall be adjusted until the m/z abundance ra-
tios fall within the limits specified, and the
verification test shall be repeated. If the ad-
justment alters the resolution of the mass
spectrometer, resolution shall be verified
(Section 10.1.2) prior to repeat of the
verification test.
15.3.3 The peaks representing each CDD/
CDF and labeled compound in the VBR
262
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
standard must be present with S/N of at least
10; otherwise, tlie mass spectrometer shall be
adjusted and the verification test repeated.
15.3.4 Compute the concentration of each,
CDD/CDP compound by Isotope dilution
(Section 10.5) for those compounds that have
labeled analogs (Table 1). Compute the con-
centration of the labeled compounds by the
internal standard method (Section 10.6).
These concentrations are computed based on
the calibration data in Section 10.
15.3.5 For each compound, compare the
concentration with the calibration
verification limit in Table 8. If only 2,3,7,8-
TCDD and 2,3,7,8-TCDF are to be determined,
compare the concentration to the limit in
Table 6a. If all compounds meet the accept-
ance criteria, calibration has been verified
and analysis of standards and sample ex-
tracts may proceed. If, however, any com-
pound fails its respective limit, the measure-
ment system is not performing properly for
that compound. In this event, prepare a fresh
calibration standard or correct the problem
causing the failure and repeat the resolution
(Section 15.2) and verification (Section 15.3)
tests, or recalibrate (Section 10).
15.4 Retention Times and GC Resolution.
15.4.1 Retention times.
15.4.1.1 Absolute—The absolute retention
times of the I3C12-1,2,3,4-TCDD and "C,2-
1,2,3,7,8,9-HxCDD GCMS internal standards
in the verification test (Section 15.3) shall be
within ±15 seconds of the retention times ob-
tained during- calibration (Sections 10.2.1 and
10.2.4).
15.4.1.2 Relative—The relative retention
times of CBDs'CDFs and labeled compounds
in the verification test (Section 15.3) shall be
within the limits given in Table 2.
15.4.2 GC resolution.
15.4.2.1 Inject the isomer specificity
standards (Section 7.15) on their respective
columns.
15.4.2.2 The valley height between 2,3,7,8-
TCDD and the other tetra-dioxin isomers at
m/z 319.8965, and between 2,3,7,8-TCDF and
the other tetra-furan isomers at m/z 303.9016
shall not exceed 25% on their respective col-
umns (Figures 6 and 7).
15.4.3 If the absolute retention time of
any compound is not within the limits speci-
fied or if the 2,3,7,8-isomers are not resolved,
the O-C is not performing properly. In this
event, adjust the GC and repeat the
verification test (Section 15.3) or recalibrate
(Section 10), or replace the GC column and
either verify calibration or recalibrate.
15.5 Ongoing Precision and Recovery.
15.5.1 Analyze the extract of the ongoing
precision and recovery (OPR) aliquot (Sec-
tion 11.4.2.5, 11.5.4, 11.6.2, 11.7.4, or 11.8.3,2)
prior to analysis of samples from the same
batch.
15.5.2 Compute the concentration of each
CDD/CDF by isotope dilution for those com-
pounds that have labeled analogs (Section
10.5). Compute the concentration of
1,2,3,7,8,9-HxCDD, OCDF, and each labeled
compound by the internal standard method
(Section 10.8).
15.5.3 For each CDD/CDF and labeled com-
pound, compare the concentration to the
OPR limits given in Table 6. If only 2,3,7,8-
TCDD and 2,3,7,8-TCDF are to be determined,
compare the concentration to the limits in
Table 6a. If all compounds meet the accept-
ance criteria, system performance is accept-
able and analysis of blanks and samples may
proceed. If, however, any individual con-
centration falls outside of the range given,
the extraction'concentratlon processes are
not being performed properly for that com-
pound. In this event, correct the problem, re-
prepare, extract, and clean up the sample
batch and repeat the ongoing precision and
recovery test (Section 15.5).
15.5.4 Add results that pass the specifica-
tions in Section 15.5.3 to initial and previous
ongoing data for each compound in each ma-
trix. Update QC charts to form a graphic rep-
resentation of continued laboratory perform-
ance. Develop a statement of laboratory ac-
curacy for each CDD/CDF in each matrix
type by calculating the average percent re-
covery (R) and the standard deviation of per-
cent recovery (SR). Express the accuracy as a
recovery interval from R-2Su to R=2SR, For
example, if R=95% and SR=5%, the accuracy
is 85-105%.
15.6 Blank—Analyze the method blaak ex-
tracted with each sample batch immediately
following analysis of the OPR aliquot to
demonstrate freedom from contamination
and freedom from carryover from the OPR
analysis. The results of the analysis of the
blank must meet the specifications in Sec-
tion 9.5.2 before sample analyses may pro-
ceed.
16.0 Qualitative Determination
A ODD, CDF, or labeled compound is iden-
tified in a standard, blank, or sample when
all of the criteria in Sections 16.1 through
16.4 are met.
16.1 The signals for the two exact m/z's in
Table 8 must be present and must maximize
within the same two seconds.
16.2 The signal-to-noise ratio (S/N) for the
GO peak at each exact m/z must be greater
than or equal to 2.5 for each ODD or CDF de-
tected in a sample extract, and greater than
or equal to 10 for all CDDs/CDFs in the cali-
bration standard (Sections 10.2.3 and 15.3.3).
16.3 The ratio of the integrated areas of
the two exact m/z's specified in Table 8 must
be within the limit in Table 9, or within ±10%
of the ratio in the midpoint (CSS) calibration
or calibration verification (VER), whichever
is most recent.
16.4 The relative retention time of the
peak for a 2,3,7,8-substituted CDD or CDF
must be within the limit in Table 2. The re-
tention time of peaks representing non-
263
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Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
2,3,7,8-substituted CDDs/CBFs must be with-
in the retention time windows established in
Section 10.3.
16.5 Confirmatory Analysis—Isomer speci-
ficity for 2,3,7,8-TCDF cannot be achieved on
the DB-5 column. Therefore, any sample in
which 2,3,7,8-TCDF is identified by analysis
on a DB-5 column must have a confirmatory
analysis performed on a DB-225, SP-2330, or
equivalent GC column. The operating condi-
tions In Section 10.1.1 may be adjusted to op-
timize the analysis on the second GC col-
umn, but the GC/MS must meet the mass
resolution and calibration specifications in
Section 10.
16.6 If the criteria for identification in
Sections 16.1 through 16.5 are not met, the
CDD or CDP has not been Identified and the
results may not be reported for regulatory
compliance purposes. If interferences pre-
clude identification, a new aliquot of sample
must be extracted, further cleaned up, aad
analyzed.
17.0 Quantitative Determination
17.1 Isotope Dilution Quantitation—By
adding a known amount of a labeled com-
pound to every sample prior to extraction,
correction for recovery of the CDD/CDF can
be made because the CDD/CDF and its la-
beled analog exhibit similar effects upon ex-
traction, concentration, and gas chroma-
tography, Relative response (BB) values are
used in conjunction with the initial calibra-
tion data described in Section 10.5 to deter-
mine concentrations directly, so long as la-
beled compound spiking levels are constant,
using the following equation:
Cex (ng/mL) =
(Aln+A2n)C1
(Ali+A2,)RR
where:
Cex = The concentration of the CDD/CDF in
the extract, and the other terms are as de-
fined in Section 10.5.2.
17.1.1 Because of a potential interference,
the labeled analog of OCDF is not added to
the sample. Therefore, OCDF is quantitated
against labeled OCDD. As a result, the con-
centration of OCDF is corrected for the re-
covery of the labeled OCDD. la instances
where OCDD and OCDF behave differently
during sample extraction, concentration, and
cleanup procedures, this may decrease the
accuracy of the OCDF results. However,
given the low toxicity of this compound rel-
ative to the other dloxins aad furaas, the po-
tential decrease in accuracy is not consid-
ered significant.
17.1.2 Because 13C,2-l,2,3,7,8,9-HxCDD is
used as an instrument internal standard (i.e.,
not added before extraction of the sample), it
cannot be used to quantitate the 1,2,3,7,8,9-
HxCDD by strict isotope dilution procedures.
Therefore, 1,2,3,7,8,9-HxCDD is qnantitated
using the averaged response of the labeled
analogs of the other two 2,3,7,8-substituted
HxCDD's: 1,2,3,4,7,8-HxCDD and 1,2,3,6,7,8-
HxCDD. As a result, the conceatration of
1,2,3,7,8,9-HxCDD is corrected for the average
recovery of the other two HxCDD's.
17.1.3 Any peaks representing non-2,3,7,8-
substitnted CDDs/CDFs are quantitated
using an average of the response factors from
all of the labeled 2,3,7,8-isomers at the same
level of chloriaation.
17.2 Internal Standard Quantitation and
Labeled Compound Recovery.
17.2,1 Compute the concentrations of
1,2,3,7,8,9—HxCDD, OCDF, the "C-labeled
analogs and the 37C-labeled cleanup standard
in the extract using the response factors de-
termined from the initial calibration data
(Section 10.6) and the following equation:
Cex (ng/mL):
(Als+A2g)Cis
(Alis+A2is)RF
where:
Ce» = The concentration of the CDD/CDF in
the extract, and the other terms are as de-
fined in Section 10.6.1.
NOTE: There is only one m/z for the 37Cl-la-
beled standard.
17.2.2 Using the concentration in the ex-
tract determined above, compute the percent
recovery of the 13C-labeled compounds and
the 37C-labeled cleanup standard using the
following equation:
Recovery (%) =
Concentration found (jig/mL)
Concentration spiked (^ig/mL)
xlOO
17,3 The concentration of a CDD/CDF in
tie solid phase of the sample is computed
using the concentration of the compound in
the extract and the weight of the solids (Sec-
tion 11.5.1), as follows:
264
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Environmental Protection Agency
Concentration in solid (ng/kg) =
Pt. 136, App. A, Meth. 1613
(CexxVex)
where:
Ge, = The concentration of the compound in
the extract,
V«x = The extract volume in mL.
W, = The sample weight (dry weight) in kg.
17.4 The concentration of a CDD/CDF in
the aqueous phase of the sample is computed
using the concentration of the compound in
the extract and the volume of water ex-
tracted (Section 11.4 or 11.5), as follows:
Concentration in aqueous phase (pg/L) =
where:
C<.» = The concentration of the compound in
the extract.
Ve» = The extract volume in mL.
V, = The sample volume in liters.
17.5 If the SICP area at either quantita-
tion m/z for any compound exceeds the cali-
bration range of the system, a smaller sam-
ple aliquot is extracted.
17.5.1 For aqueous samples containing 1%
solids or less, dilute 100 mL, 10 mL, etc., of
sample to 1 L with reagent water and re-pre-
pare, extract, clean up, and analyze per Sec-
tions 11 through 14.
17.5.2 For samples containing greater
than 1% solids, extract an amount of sample
equal to "">, 1"°°, etc., of the amount used in
Section 11.5.1. Re-prepare, extract, clean up,
and analyze per Sections 11 through 14.
17.5.3 If a smaller sample size will not be
representative of the entire sample, dilute
the sample extract by a factor of 10, adjust
the concentration of the instrument internal
standard to 100 pg/uL in the extract, and ana-
lyze an aliquot of this diluted extract by the
internal standard method.
17.6 Results are reported to three signifi-
cant figures for the CDDs/CDPs and labeled
compounds found in all standards, blanks,
and samples.
17.6.1 Reporting units and levels.
17.6.1.1 Aqueous samples—Report results
in pg/L (parts-per-quadrillion).
17.8.1.2 Samples containing greater than
1% solids (soils, sediments, filter cake, com-
post)—Report results in ng/kg based on the
dry weight of the sample. Report the percent
solids so that the result may be corrected.
17.6.1.3 Tissues—Report results in ng/kg of
wet tissue, not on the basis of the lipid con-
tent of the sample. Report the percent lipid
content, so that the data user can calculate
the concentration on a lipid basis if desired.
17.6.1.4 Reporting level.
17.6.1.4.1 Standards (VER, IPR, OPR) and
samples—Report results at or above the min-
imum level (Table 2). Report results below
the minimum level as not detected or as re-
quired by the regulatory authority.
17.6.1.4.2 Blanks—Report results above
one-third the ML.
17.6.2 Results for CDDs/CDFs in samples
that have been diluted are reported at the
least dilute level at which the areas at the
quantitation m/z's are within the calibration
range (Section 17,S).
17.6.3 For CDDs/CDFs having a labeled
analog, results are reported at the least di-
lute level at which the area at the quantita-
tion m/z is within the calibration range (Sec-
tion 17.5) and the labeled compound recovery
is within the normal range for the method
(Section 9.3 and Tables 6, 6a, 7, and 7a).
17.6.4 Additionally, if requested, the total
concentration of all isomers in an individual
level of chlorination (i.e., total TCDD, total
TCDF, total Paced, etc.) may be reported by
summing the concentrations of all isomers
identified in that level of chlorination, in-
cluding both 2,3,7,8-substituted and non-
2,3,7,8-substituted isomers.
18.0 Analysis of Complex Samples
18.1 Some samples may contain high lev-
els (>10 ng/L: >1000 ng/kg) of the compounds
of interest, interfering compounds, and/or
polymeric materials. Some extracts will not
concentrate to 10 jiL (Section 12.7); others
may overload the GO column and/or mass
spectrometer.
18.2 Analyze a smaller aliquot of the sam-
ple (Section 17.5) when the extract will not
concentrate to 10 nL after all cleanup proce-
dures have been exhausted.
18.3 Chlorodiphenyl Ethers—If
chromatographic peaks are detected at the
retention time of any CDDs/CDFs in any of
the m/z channels being monitored for the
265
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Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edl«on>
chlorodiphenyl ethers (Table 8), cleanup pro-
cedures must be employed until these inter-
ferences are removed. Alumina (Section 13.4)
and Plorisil (Section 13,8) are recommended
for removal of chlorodiphenyl ethers.
18.4 Recovery of Labeled Compounds—In
most samples, recoveries of the labeled com-
pounds will be similar to those from reagent
water or from the alternate matrix (Section
7.6).
18.4.1 If the recovery of any of the labeled
compounds is outside of the normal range
(Table 7), a diluted sample shall be analyzed
(Section 17.5).
18.4.2 If the recovery of any of the labeled
compounds in the diluted sample is outside
of normal range, tie calibration verification
standard (Section 7.13) shall be analyzed and
calibration verified (Section 15.3).
18.4.3 If the calibration cannot be verified,
a new calibration must be performed and the
original sample extract reanalyzed.
18.4.4 If the calibration is verified and the
diluted sample does not meet the limits for
labeled compound recovery, the method does
not apply to the sample being: analyzed and
the result may not be reported for regu-
latory compliance purposes. In this case, al-
ternate extraction and cleanup procedures in
this method must be employed to resolve the
interference. If all cleanup procedures in this
method have been employed and labeled
compound recovery remains outside of the
normal range, extraction and/or cleanup pro-
cedures that are beyond this scope of this
method will be required to analyze these
samples.
79.0 Pollution Prevention
19.1 The solvents used in this method pose
little threat to the environment when man-
aged properly. The solvent evaporation tech-
niques used in this method are amenable to
solvent recovery, and it is recommended that
the laboratory recover solvents wherever
feasible.
19.2 Standards should be prepared in vol-
umes consistent with laboratory use to mini-
mize disposal of standards.
20.0 Waste Management
20.1 It is the laboratory's responsibility to
comply with all federal, state, and local reg-
ulations governing waste management, par-
ticularly tie hazardous waste identification
rules and land disposal restrictions, and to
protect the air, water, and land by mini-
mizing' and controlling all releases from
fume hoods and bench operations. Compli-
ance is also required with any sewage dis-
charge permits and regulations.
20.2 Samples containing HC1 to pH <2 are
hazardous and must be neutralized before
being poured down a drain or must be han-
dled as hazardous waste.
20.3 The CDDs/CDFs decompose above 800
°C. Low-level waste such as absorbent paper,
tissues, animal remains, and plastic gloves
may be burned in an appropriate incinerator.
Gross quantities (milligrams) should be
packaged securely and disposed of through
commercial or governmental channels that
are capable of handling extremely toxic
wastes.
20.4 Liquid or soluble waste should be dis-
solved in methanol or ethanol and irradiated
with ultraviolet light with a wavelength
shorter than 290 nm for several days. Use F40
BL or equivalent lamps. Analyze liquid
wastes, and dispose of the solutions when the
CDDs/CDFs can no longer be detected.
20.5 For further information on waste
management, consult "The Waste Manage-
ment Manual for Laboratory Personnel* and
"Less is Better—Laboratory Chemical Man-
agement for Waste Reduction," available
from the American Chemical Society's De-
partment of Government Relations and
Science Policy, 1155 16th Street N.W., Wash-
ington, B.C. 20036.
21.0 Method Performance
Method performance was validated and
performance specifications were developed
using data from EPA's international inter-
laboratory validation study (References 30-
31) and the EPA/paper industry Long-Term
Variability Study of discharges from the
pulp and paper industry (58 FR 66078).
22.0 References
1. Tondeur, Yves. "Method 8290: Analytical
Procedures and Quality Assurance for Multi-
media Analysis of Polychlorinated Dibenzo-
p-dioxins and Dibenzofurans by High Resolu-
tion Gas Chromatography/High Resolution
Mass Spectrometry," USEPA EMSL, Las
Vegas, Nevada, June 1987.
2, "Measurement of 2,3,7,8-Tetraehlorinated
Dibenzo-p-dioxin (TCDD) and 2,3,7,8-
Tetraehlorinated Dibenzofuran (TCDF) in
Pulp, Sludges, Process Samples and
Wastewaters from Pulp and Paper Mills,"
Wright State University, Dayton, OH 45435,
June 1988.
3. "NCASI Procedures for the Preparation
and Isomer Specific Analysis of Pulp and
Paper Industry Samples for 2,3,7,8-TCDD and
2,3,7,8-TCDF," National Council of the Paper
Industry for Air and Stream Improvement
Inc., 260 Madison Avenue, New York, NY
10016, Technical Bulletin No. 551, Pre-Release
Copy, July 1988.
4. "Analytical Procedures and Quality As-
surance Plan for the Determination of
PCDD/PCDF in Fish," USEPA, Environ-
mental Research Laboratory, 6201 Congdon
Boulevard, Duluth, MN 55804, April 1988.
5. Tondeur, Yves. "Proposed GC/MS Meth-
odology for the Analysis of PCDDs and
266
-------
Environmental Protection Agency
Ft. 136, App. A, Meth. 1613
PCDFs in Special Analytical Services Sam-
ples," Triangle Laboratories, Inc., 801-10
Capitola Dr, Research Triangle Park, NC
27713, January 1988; updated by personal
communication September 1988,
6. Lamparski, L.L. and Nestrick, T.J. "De-
termination of Tetra-, Hexa-, Hepta-, and
Octachlorodibenzo-p-dioxin Isomere in Par-
ticulate Samples at Parts per Trillion Lev-
els," Analytical Chemistry, 52: 2045-2054, 1980.
7, Lamparski, L.L. and Nestiick, T.J.
"Novel Extraction Device for the Determina-
tion of Chlorinated Dibenzo-p-dioxins
(PCDDs) and Dibenzofurans (PCDPs) in Mat-
rices Containing Water," Chemosphere. 19:27-
31, 1989.
8. Patterson, D.G., et. al. "Control of Inter-
ferences in the Analysis of Human Adipose
Tissue for 2,3,7,8-Tetrachlorodibenzo-p-
dioxin," Environmental Toxicological Chem-
istry, 5:355-360, 1986.
9, Stanley, John S. and Sack, Thomas M.
"Protocol for the Analysis of 2,3,7,8-
Tetrachlorodlbenzo-p-dioxin by High Resolu-
tion Gas Chromatography/High Resolution
Mass Spectrometry," TISBPA EMSL, Las
Vegas, Nevada 89114, EPA 600/4-86-004, Janu-
ary 1986.
10. "Working with Carcinogens," Depart-
ment of Health, Education, Si Welfare, Public
Health Service, Centers for Disease Control,
NIOSH. Publication 77-206, August 1977,
NTIS PB-277256.
11. "OSHA Safety and Health Standards,
General Industry," OSHA 2206, 29 CPR 1910.
12, "Safety in Academic Chemistry Labora-
tories," ACS Committee on Chemical Safety,
1979.
13. "Standard Methods for the Examination
of Water and Wastewater," 18th edition and
later revisions, American Public Health As-
sociation, 1015 15th St, N.W., Washington, DC
20006, 1-35: Section 1090 (Safety), 1992.
14. "Method 613—2,3,7,8-Tetrachlorodibenzo-
p-dioxin," 40 CPR 136 (49 PR 43234), October
26,1984, Section 4.1.
15. Provost, L.P. and Elder, R.S. "Interpre-
tation of Percent Recovery Data," American
Laboratory, 15: 56-83, 1983.
16. "Standard Practice for Sampling
Water," ASTM Annual Book of Standards,
ASTM, 1916 Race Street, Philadelphia, PA
19103-1187, 1980.
17. "Methods 330.4 and 330.5 for Total Resid-
ual Chlorine," USEPA, EMSL, Cincinnati,
OH 45268, EPA 600/4-79-020, March 1979.
IB. "Handbook of Analytical Quality Con-
trol in Water and Wastewater Laboratories,"
USEPA EMSL, Cincinnati, OH 45268, EPA-
600/4-79-019, March 1979.
19. Williams, Rick. Letter to Bill Telliard,
June 4, 1993, available from the EPA Sample
Control Center operated by DynCorp Viar,
Inc., 300 N Lee St, Alexandria, VA 22314, 703-
519-1140.
20. Barkowski, Sarah. Fax to Sue Price,
August 6, 1992, available from the EPA Sam-
ple Control Center operated by DynCorp
Viar, Inc., 300 N Lee St, Alexandria VA 22314,
703-519-1140.
21. "Analysis of Multi-media, Multi-con-
centration Samples for Dioxins and Purans,
PCDD/PCDF Analyses Data Package", Nar-
rative for Episode 4419, MRI Project No. 3091-
A, op.cit. February 12, 1993, Available from
the EPA Sample Control Center operated by
DynCorp Viar Inc, 300 N Lee St, Alexandria,
VA 22314 (703-519-1140).
22. "Analytical Procedures and Quality As-
surance Plan for the Determination of
PCDD/PCDF in Fish", U.S. Environmental
Protection Agency, Environmental Research
Laboratory, Duluth, MN 55804, EPA/600/3-90/
022, March 1990.
23. Afghan, B.K., Carron, J., Goulden, P.O.,
Lawrence, J., Leger, D., Onuska, P., Sherry,
J., and Wilkenson, R.J., "Recent Advances in
Ultratrace Analysis of Dioxins and Related
Halogenated Hydrocarbons", Can J. Chem.,
65: 1086-1097, 1987.
24. Sherry, J.P. and Tse, H. "A Procedure
for the Determination of Polychlorinated
Dibenzo-p-dioxins in Pish", Chemosphere, 20:
866-872,1990.
25. "Preliminary Pish Tissue Study", Re-
sults of Episode 4419, available from the EPA
Sample Control Center operated by DynCorp
Viar, Inc., 300 N Lee St, Alexandria. VA
22314, 703-519-1140.
26. Nestrick, Terry L. DOW Chemical Co..
personal communication with D,R.
Rushneck, April 8, 1993. Details available
from the U.S. Environmental Protection
Agency Sample Control Center operated by
DynCorp Viar Inc, 300 N Lee St, Alexandria,
VA 22314, 703-519-1140.
27. Barnstadt, Michael. "Big Fish Column",
Triangle Laboratories of RTF, Inc., SOP 129-
90, 27 March 27, 1992,
28. "Determination of Polychlorinated
Dibenzo-p-Dioxins (PCDD) and Dibenzofurans
(PCDF) in Environmental Samples Using
EPA Method 1613", Chemical Sciences De-
partment, Midwest Research Institute, 425
Volker Boulevard, Kansas City, MO 44110-
2299, Standard Operating Procedure No. CS-
153, January 15, 1992.
29. Ryan, John J. Raymonde Lizotte and
William H. Newsome, J, Chromatog. 303
(1984) 351-360.
30. Telliard, William A., McCarty, Harry
B., and Riddick, Lynn S. "Results of the
Intel-laboratory Validation Study of USEPA
Method 1613 for the Analysis of Tetra-
through Octachlorinated Dioxins and Furans
by Isotope Dilution GO/MS," Chemosphere.
27, 41-46 (1993).
31. "Results of the International Interlab-
oratory Validation Study of USEPA Method
1613", October 1994, available from the EPA
Sample Control Center operated by DynCorp
Viar, Inc., 300 N Lee St, Alexandria, VA
22314, 703-519-1140.
23.0 Tables and Figures
267
-------
Pt. 136, App. A, Meth. 1613
40 CfR Ch. I (7-1-04 Edition)
TABLE 1—CHLORINATED DIBENZO-P-DIOXINS AND FURANS DETERMINED BY ISOTOPE DILUTION AND
INTERNAL STANDARD HIGH RESOLUTION GAS CHROMATOGRAPHY (HRGC)/HiGH RESOLUTION
MASS SPECTROMETRY (HRMS)
CDDs/COFs1
2,3,7,8-TCDD ,
Total TCDD
2,3,7,8-TCDF
Totai-TCDF
1,2,3,7,8-PeCOD
Total-PeCDD ...... ....
1237 8-PeCDF
23478-PeCDF ... .. .......
Total-PeCDF
1 2 3 4 7,8-HxCDD ...
1,2,3,6,7,8-HxCDD
12378 9-HxCDD .
Total-HxCDD
1,2,3,4,7,8-HxCDF
1 ,2,3 6 7,8-HxCDF
12378 9-HxCDF
2,3,4,6,7,8-HxCDF
Total-HxCOF
1 ,2 3 4 6,7,8-HpCDD
Total-HpCDD
1 2 3 4 6,7,8-HpGDF ., .. .
1,2,3,4,7,8,9-HpCDF
Total-HpCDF
OCDD
OCDF
CAS registry
1746-01-6
41903-57-5
51207-31-9
55722-27-5
40321-76-4
36088-22-9
57117-41-6
57117-31-4
30402-15-4
39227-28-6
57653-85-7
19408-74-3
34465-46-8
70648-26-9
57117-44-9
72918-21-9
60851-34-5
55684-94-1
35822-46-9
37871-00-4
67562-39-4
55673-«9-7
38998-75-3
3268-87-9
39001-02-0
Labeled analog
"C,2-23,7,8-TC0D
"CI4-2,3,7,8-TCDD
13C,2"2,3,7,8-TCDF
IJC)2-1,2,3,7,8-PeCDD
!3Ci2-1 237 8-PeCDF
"Ci2-2 3 4,7,8-PeCDF , .
"0,2-1 2 3,4 7 8-HxGDD
"Ci2-1,2 3,6,7 ,8-HxCDD ., ,
"0,2-1 2378 9-HxCDD
l-"'Ci2-1,2,3,4,7,8-HxCDF
«Ci2-1 2 3 6,7,8-HxCDF ..
"0,2-1 2378 9-HxCDF
13Ci2-2,34,6,7,8-HxCDF ,
"0,2-1 2 3,4,6,7 8-HpCDD . ..
I3C,2-1 2 3,4 6 7 8-HpCDF
l3Ci2-1,2,3,4,7,8,B-HpCDF
»Ci2-OCDD
Not used.
CAS registry
76523-40-5
85508-50-5
89059-46-1
109719-79-1
109719-77 9
116843-02-8
109719-80-4
109719-81-5
109719-82-6
114423-98-2
116843-03-9
116843-04-0
116843-05-1
109719-83-7
109719-84-8
109719-94-0
114423-97-1
1 Chlorinated dibenzo-p-djoxins and chlorinated dibenzofurans.
TCDD = Telrachlorodibenzo-p-dioxln.
TCDF = Tetrachlorodibenzofuran.
PeCDD = Pentachlorodibertzo-p-dioxin.
PeCDF = Pentaehlorodibenzofuran.
HxCDD - Hexachtorodibenzo-p-dioxin.
HxCDF s= Hexachiorodibenzofuran.
HpCDD = Heptachlorodibenzo-p-dioxin.
HpCDF - Heptachlorodibenzofuran.
OCDD = Qctachlorodibertzo-p-dioxin.
OCDF = Qctachlorodibenzafuran.
TABLE 2—RETENTION TIME REFERENCES, QUANTITATION REFERENCES, RELATIVE RETENTION TIMES,
AND MINIMUM LEVELS FOR CDDS AND DCFS
CDD/CDF
Retention time and quantitation
reference
Relative reten-
tion time
Minimum level 1
Water
!pg/L;
ppq)
Solid (no/
kg; opt)
Extract
(Pg4»L;
ppb)
Compounds using "C12-1,2,3,4-TCDD as the Injection Internal Standard
2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-Pe
2,3,4,7,8-PeCDF
12378-PeCDD
3Ci2-2,3,7,8-TCDF
JCn-2,3,7,8-TCDD
'Ci2-2,3,7,8-TCDD
'C,r1, 2,3,7 ,8-PeCDF
3Ci2-2 3,4,7 ,8-PeCDF ...
^C,,-1.2,3.7.8-PeCDF
5C,2-2,3,7,8-TCDF
3C12-2,3,7,8-TCDD
-'Ci2-1,2,3,7,8-PeCDF
3 Ci2-2,3,4,7,8-PeCDF
' C,2-1 ,2,3 7 8-PeCDD
3Cn-1,2,3,4-TCDD
3Ci2-1,2,3,4-TCDD
'C,2-1,2,3,4-TCDD
'Cn-1,2,3,4-TCDD
'C,2-1,234-TCDD
'C,,-1.2.3,4-TCDD
0.999-1.003
0.999-1 .002
0.999-1.002
0.999-1.002
0999-1 008
0.923-1.103
0.976-1.043
0.989-1 052
1.000-1.425
1 001-1 526
1.000-1.567
10
10
50
50
50
1
1
5
5
5
0.5
0.5
2.5
2.5
25
Compounds using 'C12-1,2,3,7,8.9-HxCDUa8 the Injection Internal Standard
1,2347,8-HxCDF
12367 8-HxCDF
12378 9-HxCDF
2,3,4,6,7,8-HxCDF
1 2 3 4 7,8-HxCDD
1,2,3,6,7,8-HxCDD
1 ,2,3 7 8,9-HxCDD
1.2.3.4.6.7.8-H0CDF
'C)2-1,2,3,478-HxCDF
3C,2-1 2367 8-HxCDF
3 0 ,2-1 2 3 7 8 9-HxCDF
-*C,2-2,3,4,6,7,8-HxCDF
'Ci2-1 2347 8-HxCDD
3C,2-1,2,3,6,7.8-HxCDD
(2) ....
"C,,-1.2.3.4,6.7,8-HDCDF
0 999-1 001
0 997-1 005
0 999-1 001
0.999-1.001
0 999-1 001
0.998-1 .004
1.000-1 019
0.999-1.001
50
50
50
50
50
50
50
50
5
5
5
I
I
5
5
2.5
25
25
2.5
25
25
25
2.5
268
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
TABLE 2—RETENTION TIME REFERENCES, QUANTITATION REFERENCES, RELATIVE RETENTION TIMES,
AND MINIMUM LEVELS FOR ODDS AND DCFS—Continued
CDD/CDF
1,2,3,4,7,8,9-HpCDF
123467 8-HpCDO
OCDF
OCDD
1 2 3,4 6,7,8,-HxCDF
>'Ci2l,2,3,7,8,9-HxCDF
i->C,22,3,4,8,7,8,-HxCDF
"Cij1 2347,8-HxCDF ..
"Cp1 23678-HxCDF
"C]i1,2,3,4,6,7,8-HxCDF
"Cut 23478 9-HxCDF
"Ci-,1,2,3,4,6,7,8-HxCDF
I'CoOCDD
Retention time and quantitation
reference
"C, -1,2,3,4,7,8,9-HpCDF
"C, -1,2,3,4,6,7,8-HpCOD
«'C, -OCDD
13Ci -OCDD
"C, -1,2,3,7,8,9-HpCDD
"Ci -1 2,3,7 8 9-HpCDD
»C, -1,2,3,7,8,9-HpCDD
"Ci -1,2,3,7 8 9-HpCDD
13C, -1,2,3,7,8,9-HpCDD
13 Ci -1,2,3,7,8,9-HpCDO
"d -1,2,3,7,8,9-HpCDD
"Ci -1,2,3,7,8,9-HpCDD
"C,,-1,2.3,?.8.9-HDCDD
Relative reten-
tion time
0.999-1.001
0.999-1.001
0.999-1 001
0.999-1.001
0.949-0.975
0.977-1.047
0.959-1 .021
0.977-1.000
0.981-1.003
1 .043-1 .085
1.057-1.151
1.086-1,110
1.032-1.311
Minimum leve! 1
Water
(pgfl-;
ppq)
50
50
100
100
Solid (ngl
kg; ppt)
5
5
10
10
Extract
!P94*L;
ppb)
2.5
2.5
5.0
5.0
1 The Minimum Level (ML) for each analyte is defined as the level at which the entire analytical system must give a recogniz-
able signal and acceptable calibration point. It is equivalent to tile concentration of the lowest calibration standard, assuming that
ail method-specified sample weights, volumes, and cleanup procedures have been employed.
2The retention time reference for 1,2,3,7,8,9-HxCDD is "Ci2-1,2,3,6r7,8-HxCDD, and 1,2,3,7.8,9-HxCDD is quantified using
the averaged responses for "0,2-1,2,3,4,7,8-HxCDD and "Ci,-1,2,3,6,7,8-HxCDD.
TABLE 3—CONCENTRATION OF STOCK AND SPIKING SOLUTIONS CONTAINING CDDS/CDFS AND
LABELED COMPOUNDS
CDD/CDF
2378-TCDD
237 8-TGDF
1 ,2,3.7 8-PeCDD
1 2378-PeCDF . .
2347 8-PeGDF
1 2,3,4,7,8-HxCDD
1 2367,8-HxCDD
12378 9-HxCDD
1 2,3.4 7.8-HxCDF
12367 8-HxCDF . ... ... ....
1 2,3,7,8,9-HxCDF
23467 8-HxCDF
1 23467 8-HpCDD
1 2 3 4 6,7,8-HpCDF
123478 9-HpCDF
OCDD
OCDF
'C,a-237,B-TCDD
'Cu-2 3 7 8-TCDF
'0,,-1,2,3,7,8-PeCDD
'0,2-1 2,3,7,8-PeCDF
'Cu-2 3 4 7,8-PsCDF
'0,2-1 2347 8-HxCDD
•'C,-.-1 2 3,6,7,8-HxCDD . .... ...
•-1.2.3.7.8.9-HxCDD
Labeled com-
pound stock
solution 1
jng/mL)
100
100
100
100
100
100
100
100
100
100
100
100
100
100
200
08
200
200
Labeled
compound
spiking solu-
tion2
(ng/mL)
2
2
2
2
2
2
2
2
2
2
2
2
2
4
PAR stock
solution3
(ng/mLS
40
40
200
200
200
200
200
200
200
200
200
200
200
200
200
400
400
PAR spiking
solution *
(ng/mL)
0.8
08
4
4
4
4
4
4
4
4
4
4
4
g
a
1 Section 7.10—prepared: in nonane and diluted to prepare spiking solution.
2 Section 7.1Q.3--preparecl in acetone from stock solution daily.
269
-------
Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
3 Section 7.9—prepared in nonane and diluted to prepare spiking solution.
4 Section 7.14—-prepared in acetone from stock solution daily.
5 Sectjon 7.11—prepared in nonane and added to extract prior to cleanup.
"Section 7.12—prepared in nonane and added to the concentrated extract immediately prior to injection info the GC (Section
14.2).
TABLE A—CONCENTRATION OF CDDS/CDFS IN CALIBRATION AND CALIBRATION VERIFICATION
SOLUTIONS1 (SECTION 1S.3)
CDD/CDF
CS2
(ng/mL)
CS3
(ng/mL)
CS4
(ng/mL)
CSS
(ng/mL)
2,3,7,8-TCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDD
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCOF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDD
OCDF
"Cir2,3,7,8-TCDD
»C,2-2,3,7,8-TCDF
»Cn-1,2,3,7,8-PeCDO
"Cu-PeCDF
«Cj2-2,3,4,7,8-PeCDF
uCi,-1,2,3,4,7,8-HxCDO
i-'C,2-1,2,3,6,7,8-HxCDD
"C,2-1,2,3,4,7,8-HxCDF
"C,2-1,2,3,6,7,8-HxCDF
"Ci2-1,2,3,7,8,9-HxCDF
»Ci2-1.2,3.4,6.7,8-HpCDO ....
i=>C,2-1,2,3,4,6,7,8-HpCOF ....
"Cn-1,2,3,4,7,8,9-HpCDF ...
I'Ciz-OCDD
Cleanup Standard:
«C1,t-2,3,7,8-TCDD
Internal Standards:
»C,2-1,2,3,4-TCDD
"Ca-1,2,3,7,8,9-HxCDD
0,5
0.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
5.0
5.0
100
100
100
100
100
100
100
100
100
100
100
100
100
200
0.5
100
100
2
2
10
10
10
10
10
10
10
10
10
10
10
10
10
20
20
100
100
100
100
100
100
100
100
100
100
100
100
100
200
100
100
10
10
50
50
50
50
50
50
50
50
50
50
50
50
50
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
200
10
100
100
40
40
200
200
200
200
200
200
200
200
200
200
200
200
200
400
400
100
100
100
100
100
100
100
100
100
100
100
100
100
200
40
100
100
200
200
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
2000
2000
100
100
100
100
100
100
100
100
100
100
100
100
100
200
200
100
100
TABLE 5—GC RETENTION TIME WINDOW DEFINING SOLUTION AND ISOMER SPECIFICITY TEST
STANDARD (SECTION 7.15)
DB-5 column GC retention-time window defining solution
CDD/CDF
First eluted
Last eluted
TCDF ...
TCDD ...
PeCDF .
PeCDD
HxCDF .
HxCDD
HpCDF .
HpCDD
1,3,6,8- ...
1,3,6,8- ...
1,3,4,6,8-
1,2,4,7,9-
1,2,3,4,6,8- ...
1,2,4,6,7,9- ...
1,2,3,4,6,7,8-
1,2,3,4,6,7.9-
1,2,8,9-
1,2,8,9-
1,2,3,8,9-
1,2,3,8,9-
1,2,3,4,8,3-
1,2,3,4,6,7-
1,2,3,4,7,8,9-
1,2,3,4,6,7,8-
DB-5 Column TCDD Specificity Test Standard
1,2,3,7=1,2,3,8-TCDD
2,3,7,8-TCDD
1,2,3,9-TCDD
DB-225 Column TCDF Isomer Specificity Test Standard
2,3,4,7-TCDF
2,3,7,8-TCDF
1,2,3,9-TCDF
270
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Environmental Protection Agency
Pi 136, App. A, Meth. 1613
TABLE 6—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS WHEN ALL CDDS/CDFS ARE TESTED 1
CDD/CDF
237,8-TCDD . ..
237 8-TCDF
1 ,2 3 7,8-PeCDD
12378-PeCDF
2,3,4,7,8-PeCDF
1 2,3,4 7 8-HxCDD
12367 8-HxCDD . . ..
1 ,2,3,7,8,9-HxCDO
12347 B-HxCDF
1 ,2,3,6 7 8-HxCDF
1.2,3,7.8,9-HxCDF ,
2,3,4 6 7 8-HxCDF
123467 8-HpCDD
1 ,2,3,4,6,7,8-HpCDF
1 2 3 4 7 8 9-HpCDF
OCDD
OCDF
IACi-.-2,3,7,8-TCDD
"Ciz-2 3 7 8-TCDF
i'Cii-1 2 3 7 8-PeCDD
i3C,2-1,2,3.7,8-PeCDF
"Ci2-23478-PeCDF
nGp-1 2347 8-HxCDD
»C,2-1, 2,3,6,7 ,8-HxCDD
"Ci2-1 2 3478-HxCDF
"Cp-1,2 3,6,7,8-HxCDF
"Cu-1,2,3,7,8,9-HxCDF
°C, 2-2 3,4,6, 7,8,-HxCDF
"C,i-1,2.3,4.6,7.8-HpCDD
"Ci2-1,2,3,4,6,7,8-HpCDF
i'Cp-1 2 3 4 7 8 9-HpCDF
"Ci2-OCDD
"CI4-2,3,7,8-TCOD
Test cone.
(ng/rnL)
10
10
so
50
50
50
50
50
50
50
50
50
50
SO
50
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
200
10
IPR"
s I X
(na/mL) | (ng/mL)
r2.8
2.0
7.S
7.5
8.6
9.4
7.7
11.1
8.7
6.7
6.4
7.4
7.7
6.3
8.1
19
27
37
35
39
34
38
41
38
43
35
40
37
35
41
40
95
3.6
8.3-12.9
8.7-13.7
38-66
43-62
36-75
39-76
42-62
37-71
41-59
46-60
42-61
37-74
38-65
45-56
43-63
89-127
74-146
28-134
31-113
27-184
27-156
16-279
29-147
34-122
27-152
30-122
24-157
29-136
34-129
32-110
28-141
41-276
3.9-15.4
OPH
(ng/mL)
6.7-15.8
7.5-15.8
35-71
40-67
34-80
35-82
38-67
32-81
36-67
42-65
39-65
35-78
35-70
41-61
39-69
78-144
63-170
20-175
22-152
21-227
21-192
13-328
21-193
25-163
19-202
21-159
17-205
22-176
26-166
21-158
20-186
26-397
3.1-19.1
VER
(ng/mL)
7.8-12.9
8.4-12.0
39-65
41-60
41-61
39-64
39-64
41-61
45-56
44-57
45-56
44-57
43-58
45-55
43-58
79-126
63-159
82-121
71-140
62-160
76-130
77-130
85-117
85-118
76-131
70-143
74-135
73-137
72-138
78-129
77-129
96-115
7.9-12.7
1 Ali specifications are given as concentration in the final extract, assuming a 20 pL volume.
2 s = standard deviation of the concentration.
3X = average concentration.
TABLE 6A—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS WHEN ONLY TETRA COMPOUNDS ARE
TESTED'
CDD/CDF
2,3,7 8-TCDO
2,3,7,8-TCDF
»Ci-.-2,3,7,8-TCDD
"Cn-2,3, 7, 8-TCDF
•"Cu-2.3.7.8-TCDD
Test Cone.
(ng/mL)
10
10
100
100
10
IPR23
s (ng/mL) | X
2.7
2.0 I
35 i
34 i
3.4 i
(ng/mL)
8.7-12.4
9.1-13.1
32-115
35-99
4.5-13.4
OPR
(ng/mL)
7.314.6
8.0-14.7
25-141
26-126
3.7-15.8
V6R
(ng/mL)
8.2-12.3
8.6-11.6
85-117
76-131
8.3-12.1
' Ail specifications are given as concentration in the finai extract, assuming a 20 fit volume,
2s = standard deviation of the concentration,
^X = average concentration.
TABLE 7—LABELED COMPOUNDS RECOVERY IN SAMPLES WHEN ALL CDDS/CDFS ARE TESTED
Compound
"Ci2-2378-TCDD
"Cn-2 3 7 8-TCDF
>-
-------
Pt. 136, App. A, Mefh. 1613
40 CFR Ch, I (7-1-04 Edition)
TABLE 7—LABELED COMPOUNDS RECOVERY IN SAMPLES WHEN ALL CDDS/CDFS ARE TESTED—
Continued
Compound
>Ci3-1,2,3,7,8,9-HxCDF
'Ci2-2,3,4,6,7,8-HxCDF
»C,2-1,2,3,4,6,7,8-HpGDD
3C«-1 ,2,3,4,6,7,8-HpCDF ,
'C,2-1,2,3,4,7,8,9-HpCDF
'Cn-OCDD
'CL-2.3.7.8-TCDD
Test cone.
(ns/mL)
100
100
100
100
100
200
10
Labeled compound
recovery
(ng/mL) '
29-147
28-136
23-140
28-143
26-138
34-313
3.5-19.7
(%)
29-147
28-136
23-140
28-143
26-138
17-157
35-197
! Specification given as concentration in the final extract, assuming a 20-jiL volume.
TABLE ?A—LABELED COMPOUND RECOVERY IN SAMPLES WHEN ONLY TETRA COMPOUNDS ARE
TESTED
Compound
13Ci2-2,3,7,8-TCDD
13C|2-2 3 7 8-TCDF
"CL-2.3.7.8-TCDD
Test cone.
(ng/mL)
100
100
10
Labeled compound
recovery
(no/mL)'
31-137
29-140
4.2-16.4
(%)
31-137
29-140
42-164
1 Specification given as concentration in the final extract, assuming a 20 nL volume.
TABLE 8—DESCRIPTORS, EXACT M/Z's, M/Z TYPES, AND ELEMENTAL COMPOSITIONS OF THE CDDs
AND CDFs
Descriptor
1
2
3
4
Exact M/Z'
292.9825
303.9016
305.8987
315.9419
317.9389
319.8965
321.8936
327.8847
330.9792
331 .9368
333.9339
375.8364
339.8597
341.8567
351.9000
353.8970
354.9792
355.8546
357.8516
387.8949
369.8919
409.7974
373.8208
375.8178
383 8639
385.8610
389.8157
391.8127
392 9780
401 .8559
403.8529
430.9729
445.7555
407.7818
409 7789
417.8253
419.8220
423.7768
425.7737
M/Z type
Lock
M
M-2
M
M-2
M
M-2
M
QC
M
M=2
M=2
M-2
M=4
M-2
M=4
Lock
M-2
M=»
M-2
M-4
M=2
M-2
M-4
M
M-2
M-2
M-4
Lock
M-2
M-4
QC
M=4
M=2
M-4
M
M-2
M-2
M=4
Elemental composition
C7FM
CuHjttCUO
Ci2H4»CM7CIQ
"CiilV'CUO
"Ciir"U"Cb37QO
CnH*™CUQi
C|2H«MCIV"CIO!
CizrV'CUOj
C,F,,
"CljtVCltOl
"CiiH^'CijWCIOz
Ci>H,BCU"CIO
CnHi^cycio
CnH^'Ch^CbO
"CiiH^'CyCIO
i-'Ci2H3-«Ch»CI2O
C,Fn
Ci2H,«Cl437CIO2
CnHH^cycisOs
''CnHaMCyciOi
"CijH,MCh"Cl2&>
daHj'sWCIO
Ci2H2MCls37CIO
Cl2Hi*5Cl43''Cl!O
"CiiHz33Cl6O
'3Ci2Hr"Cls37CIO
Ci2H23sa5:!7ciO2
C,2H2«Cl4:nCf2O2
C,F,S
"Ci2H2'5Cl5'7CI02
l3C,2H235Clj"Cl2O2
C«Fn
C|2H2»Cl637Cl2O
Ci2H«Cl637CIO
CuWCyChO .. . .,
"CuH'JChO
l3CnH»CI
-------
Environmental Protection Agency
Pt, 136, App. A, Meth. 1613
TABLE 8—DESCRIPTORS, EXACT M/Z's, M/Z TYPES, AND ELEMENTAL COMPOSITIONS OF THE CDDs
AND CDFs—Continued
Descriptor
5 ..
Exact M/Z1
430 9729
435.8169
437.8140
4797165
441 .7428
442 9728
443 7399
457 7377
459.7348
469.7779
471 7750
513.6775
M/Z type
Lock
M=2
M=4
M=4
M=2
Lock
M-4
M=2
M-4
M=2
M=4
M=4
Elemental composition
C,Fn
"C,->H"CVCIO2
>1C,2H"Ck;"ChOi
CioHMCl737CWD
Cj^CM'CIO
Cij»CI6"CI-.O
Cr-i5CM7CIO2
C,215CI««CliO,
"Ci235Clr"CIO2
"Ci^*ci(,"Ch02
c,,wei«"CK>
Substance 2
PFK
HpCDD3
HpCDD3
NCDPE
OCDF
PFK
OCDF
OCDD
OCDD
OCDD3
OCDD3
DCDPi
1 Nuclidic masses used:
H = 1.007825.
O = 15.994915.
C = 12.00000.
"Cl = 34.968853.
"C = 13.003355.
"Cl = 36.965903.
F = 18.9984.
2TCDD = Tetrachlorodibenzo-p-dioxin,
PeCDD = Pentachlorodlbenzo-p-dioxin.
HxCDD = Hexachiorodibenzo-p-dioxin,
HpCDD = Heptachtorpdibenzo-p-dioxin,
OCDD « OctaehlorodibenzQ-p-dioxin.
HxCDPE = HexacWorodiphenyl ether.
OCDPE = Octachlorodipnertyl ether.
DCDPE = Decachlorodiphenyl ether.
TCDF = Tetrachtorodibenzofuran.
PeCDF = Pentachlorodibenzofuran.
HxCDF = Hexachlorodibenzofuran.
HpCDF = Hsptachlorpdibenzofuran.
OCDF = Octachtorodibenzofuran.
HpCDPE = Heptachlorodiphenyl ether.
NCDPE = Nonachlorodiphenyl ether.
PFK = Perfluorokerosene.
3 Labeled compound.
4 There is only one m/z for "Cl4-2,3,7,8,-TCDD (cleanup standard).
TABLE 9—THEORETICAL ION ABUNDANCE RATIOS AND QC LIMITS
Number of chlorine atoms
42
5
6
63
7"
a
M/Z's forming ratio
M/(M-2)
(M=2)/(M=4)
(M=2)/(M=4)
M/(M-2)
(M=2V(M=4)
M/(M=2)
(M-2)«M-4i
Theoretical
ratio
0.77
1.55
1.24
0.51
1.05
0.44
0.89
QC limit '
Lower Upper
0.65
1.32
1.05
0.43
0.88
0.37
0.76
0.89
1.78
1.43
0.59
1.20
0.51
1.02
1 QC limits represent ±15% windows around the theoretical ion abundance ratios.
2 Does not apply to "Clr2,3,7,8-TCDD (cleanup standard).
aUsed tor "Ciz-HxCDF only.
"Used for "Cu-HpCDF only.
TABLE 10—SUGGESTED SAMPLE QUANTITIES To BE EXTRACTED FOR VARIOUS MATRICES'
Sample Matrix *
Single-phase:
Solid
Example
Treated wastewater
Compost
Ash
Waste solvent
Waste oil
Fish
Human adipose
Percent solids
<1
>20
<1
Phase
(3)
Solid
Quantity ex-
tracted
1000 mL
10 g
10 9.
10 g.
273
-------
Pf. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
TABLE 10—SUGGESTED SAMPLE QUANTITIES To BE EXTRACTED FOR VARIOUS MATRICES 1—
Continued
Sample Matrix2
Multi-phase:
Liquid/Solid:
LiquidrtJquid:
Aqueous/organic/
solid.
Example
Wet soil
Untreated effluent.
Digested municipal sludge.
Filter cake.
Paper pulp.
In-process effluent
Untreated effluent
Drum waste
Percent solids
1-30
1-100
<1
>1
Phase
Solid
Both
Organic
Organic and solid
Quantity ex-
tracted
10 g.
10 g.
10 g.
10 g.
1 The quantity of sample to be extracted is adjusted to provide 10 g of solids (dry weight). One liter of aqueous samples con-
taining 1% solids will contain 10 g of solids. For aqueous samples containing greater than 1% solids, a lesser volume is used so
that 10 g of solids (dry weight) will be extracted.
2The sample matrix may be amorphous for some samples. In general, when the CDDs/CDFs are in contact with a multiphase
system in wnich one of the phases Is water, they will be preferentially dispersed in or adsorbed on the alternate phase because
of their tow solubility in water.
3 Aqueous samples are filtered after spiking with the labeled compounds. The filtrate and the materials trapped on the filter are
extracted separately, and the extracts are combined for cleanup and analysts.
274
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
* 1h» K-0 conctrtrattoi procedure h §12.63 can b»
uwfitheiR ' -
Figure 1. Bow Chart for Analysis of Aqueous and Solid Samples
275
-------
Pt. 136, App. A, Meth. 1613
40 CFi Ch. I (7-1-04 Edition)
Dtjori
cantwiMdiltoffrii
Aqueout
wM)tliMby«itNin
Mtmni%
T
fwfiis
PnwnM*
*|uo(p«f §11.6.2
I |
/NSoMl
/PnM«\j
\i»
Rtduc*p*r§11.7
Caatriatt
p«f §12.6 -§12.7
1
i
p«r §12.6 -§12.7
NoMquxxa
M 'ZIjl'j,,.
amount frwnH
sample,
i
Tnmhrlhni
I
MacKKxncmlraliMr
§12.6.1-|12.8Z
1
B**-e«r»flp«r§12.5
,
. Timittftlwi
NijSOi
Antlyw
* PWJ14-SW
gmrafcr.
Figure 2. Flow Chart for Analysis of Muib-Ptiase Samples
276
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
R«di»ot«>artspke
cleanup ed
Itamhrtmi
.
CmcMMtptr
1
OmMippirflU-
V 3 A §13.8
Bsck-wtrartpw
512.52
i
TmnslwttiniNBjSO,
i
ConcMAMpw
|W^-|12,T
Figure 3. Flow Chart for Analysis of Tissue Samples
277
-------
Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
90-mnGMF 150 Filter
1-LHer Suction Ftesk
Figure 4. Solid-Phase Extraction Apparatus
278
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
Figures. SoxtMDean-SterkExtractor
279
203-160 D-10
-------
Pt. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
38 DKCoton
100-1
40-
20-
1
JLJV.
24:00 2530
FMmtion Ttai (ninutti)
27:00
Figure 6. isomer-Spectfic of 2,3,7,&-TCDD on DB-5 Column
mm®
280
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1613
6-May-88 Sir;
Sample 11njection 1 Group 1
Text: Column Performance
Sys;DB5US
Mass 305.8987
2,3,4,8-TCOF
60-
20-
2,3,4,7-TCDF
Norm; 3466
1,3,9-TCDF
16:10 1620 16:30 1ft40 16:80 17:00 17:1ff 1720 17:30 17:40 17:40 18:00
Retention Hint (ininutM)
Figure 7, Isomer-Specific Separation of 2,3,7,8-TCDF on DB-5 Column
52-OZ7-4A
24.0 Glossary of Definitions and Purposes
These definitions and purposes are specific
to this method but have been conformed to
common usage as much as possible,
24.1 Units of weight and Measure and
Their Abbreviations.
24.1.1 Symbols;
°C—degrees Celsius
HL—microliter
Hin—micrometer
<—less tlian
>—greater than
%—percent
24.1.2 Alphabetical abbreviations:
amp—ampere
cm—centimeter
g—gram
h—hour
D—inside diameter
in.—inch
L—liter
M—Molecular ion
m—meter
mg—milligram
mln—minute
mL—millillter
mm—millimeter
m/z—mass-to-charge ratio
281
-------
Pf. 136, App. A, Meth. 1613
40 CFR Ch. I (7-1-04 Edition)
N—normal; gram molecular weight of solute
divided by hydrogen equivalent of solute,
per liter of solution
OD—outside diameter
pg—picogram
ppb—part-per-billion
ppm—part-per-million
ppq—part-per-quadrillion
ppt—part-per-trillion
psig—pounds-per-square inch gauge
v/v—volume per unit volume
w/v—weight per unit volume
24.2 Definitions and Acronyms (in Alpha-
betical Order).
Analyte—A ODD or CDF tested for by this
method. The analytes are listed in Table 1.
Calibration Standard (CAL)—A solution
prepared from a secondary standard and/or
stock solutions and used to calibrate the re-
sponse of the instrument with respect to
analyte concentration.
Calibration Verification Standard (VER>—
The mid-point calibration standard (CS3)
that is used in to verify calibration. See
Table 4.
CDD—Chlorinated Dibenzo-p-ioxin^The
isomers and congeners of tetra-tlirough octa-
chlorodlbenzo-p-dioxin.
CDF—Chlorinated Dibenzofuran—The iso-
mers and congeners of tetra-through oeta-
chlorodibenzofuran.
CS1, CS2, CSS, CS4, CSS—See Calibration
standards and Table 4.
Field Blank—An aliquot of reagent water
or other reference matrix that is placed in a
sample container in the laboratory or the
field, and treated as a sample in all respects,
including exposure to sampling site condi-
tions, storage, preservation, and all analyt-
ical procedures. The purpose of the field
blank is to determine if the field or sample
transporting procedures and environments
have contaminated the sample.
QC—Gas chromatograph or g-as chroma-
tography.
GPC—del permeation ehromatograph or
gel permeation chromatography.
HPLO—High performance liquid chro-
matograph or hig-h performance liquid chro-
ma tography.
HRGC—High resolution GC.
HRMS^High resolution MS.
IPR—Initial precision and recovery; four
aliquots of the diluted PAR standard ana-
lyzed to establish the ability to generate ac-
ceptable precision and accuracy. An IPR is
performed prior to the first time this method
is used and any time the method or instru-
mentation is modified,
K-D—Kuderna-Danish concentrator; a de-
vice used to concentrate the analytes in a
solvent.
Laboratory Blank—See method blank.
Laboratory Control sample (LCS)—See on-
going precision and recovery standard (OPR).
Laboratory Reagent Blank—See method
blank.
May—This action, activity, or procedural
step is neither required nor prohibited.
May Not—This action, activity, or proce-
dural step is prohibited.
Method Blank—An aliquot of reagent
water that is treated exactly as a sample in-
cluding exposure to all glassware, equip-
ment, solvents, reagents, internal standards,
and surrogates that are used with samples.
The method blank is used to determine if
analytes or interferences are present in the
laboratory environment, the reagents, or the
apparatus.
Minimum Level (ML)—The level at which
the entire analytical system must give a rec-
ognizable signal and acceptable calibration
point for the analyte. It is equivalent to the
concentration of the lowest calibration
standard, assuming that all method-specified
sample weights, volumes, and cleanup proce-
dures have been employed.
MS—Mass spectrometer or mass spectrom-
etry.
Must—This action, activity, or procedural
step is required.
OPR—Ongoing precision and recovery
standard (OPR); a laboratory blank spiked
with known quantities of analytes. The OPR
is analyzed exactly like a sample. Its purpose
is to assure that the results produced by the
laboratory remain within the limits speci-
fied in this method for precision and recov-
ery.
PAR—Precision and recovery standard;
secondary standard that is diluted and
spiked to form the IPR and OPR.
PFK—Perfluorokerosene; the mixture of
compounds used to calibrate the exact m/z
scale in the HRMS.
Preparation Blank—See method Wank.
Primary Dilution Standard—A solution
containing the specified analytes that Is pur-
chased or prepared from stock solutions and
diluted as needed to prepare calibration solu-
tions and other solutions.
Quality Control Check Sample (QCS)—A
sample containing all or a subset of the
analytes at known concentrations. The QCS
is obtained from a source external to the lab-
oratory or is prepared from a source of
standards different from the source of cali-
bration standards. It Is used to check labora-
tory performance with test materials pre-
pared external to the normal preparation
process.
Reagent Water—Water demonstrated to be
free from the analytes of interest and poten-
tially Interfering substances at the method
detection limit for the analyte.
Relative Standard Deviation (RSD)—The
standard deviation times 100 divided by the
mean. Also termed "coefficient of variation."
RF—Response factor. See Section 10.6.1.
RR—Relative response. See Section 10.5.2.
RSD—See relative standard deviation.
282
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1624
SDS—Soxhlet/Dean-Stark extractor; an ex-
traction device applied to the extraction of
solid and semi-solid materials (Reference ?).
Should—This action, activity, or proce-
dural step is suggested but not required,
SICP—Selected ion current profile; the
line described by the signal at an exact m/z.
SPE—Solid-phase extraction; an extrac-
tion technique in which an analyte is ex-
tracted from an aqueous sample by passage
over or through a material capable of revers-
ibly adsorbing the analyte. Also termed liq-
uid-solid extraction,
Stock Solution—A solution containing an
analyte that is prepared using a reference
material traceable to EPA, the National In-
stitute of Science and Technology (NIST), or
a source that will attest to the purity and
authenticity of the reference material.
TCDD—Tetrachlorodibenzo-p-dioxin.
TCDF—Tetrachlorodibenzofuran.
VBH—See calibration verification stand-
ard.
METHOD 1624 REVISION B—VOLATILE ORGANIC
COMPOUNDS BY ISOTOPE DILUTION GC/MS
1. Scope and Application
1.1 This method is designed to determine
the volatile toxic organic pollutants associ-
ated with the 1976 Consent Decree and addi-
tional compounds amenable to purge and
trap gas ehromatography-mass spectrometry
(GC/MS).
1.2 The chemical compounds listed in
table 1 may be determined in municipal and
industrial discharges by this method. The
methmd is designed to meet the survey re-
quirements of Effluent Guidelines Division
(EGD) and the National Pollutants Dis-
charge Elimination System (NPDBS) under
40 CFR 136.1 and 136.5. Any modifications of
this method, beyond those expressly per-
mitted, shall be considered as major modi-
fications subject to application and approval
of alternate test procedures under 40 CFB
136,4 and 136.5.
1.3 The detection limit of this method is
usually dependent on the level of interfer-
ences rather than instrumental limitations.
The limits in table 2 represent the minimum
quantity that can be detected with no inter-
ferences present,
1.4 The GC/MS portions of this method
are for use only by analysts experienced with
GC/MS or under the close supervision of such
qualified persons. Laboratories unfamiliar
with the analyses of environmental samples
by GC/MS should run the performance tests
in reference 1 before beginning.
2, Summary of Method
2.1 Stable isotopically labeled analogs of
the compounds of interest are added to a 5
rnL water sample. The sample is purged at
20-25 °C with an inert gas in a specially de-
signed chamber. The volatile organic com-
pounds are transferred from the aqueous
phase into the gaseous phase where they are
passed into a sorbent column and trapped.
After purging is completed, the trap is
backflushed and heated rapidly to desorb the
compounds into a gas chromatograph (GO,
The compounds are separated by the GC and
detected by a mass spectrometer (MS) (ref-
erences 2 and 3). The labeled compounds
serve to correct the variability of the analyt-
ical technique.
2,2 Identification of a compound (quali-
tative analysis) is performed by comparing
the GC retention time and the background
corrected characteristic spectral masses
with those of authentic standards.
2.3 Quantitative analysis is performed by
GC/MS using extracted ion current profile
(EICP) areas. Isotope dilution is used when
labeled compounds are available; otherwise,
an internal standard method is used,
2,4 Quality is assured through reproduc-
ible calibration and testing of the purge and
trap and GC/MS systems.
3. Contamination and Interferences
3.1 Impurities in the purge gas, organic
compounds out-gassing from the plumbing
upstream of the trap, and solvent vapors in
the laboratory account for the majority of
contamination problems. The analytical sys-
tem is demonstrated to be free from inter-
ferences under conditions of the analysis by
analyzing blanks initially and with each
sample lot (samples analyzed on the same 8
hr shift), as described in Section 8.5.
3,2 Samples can be contaminated by diffu-
sion of volatile organic compounds (particu-
larly methylene chloride) through the bottle
seal during shipment and storage. A field
blank prepared from reagent water and car-
ried through the sampling and handling pro-
tocol serves as a check on such contamina-
tion.
3.3 Contamination by carry-over can
occur when high level and low level samples
are analyzed sequentially. To reduce carry-
over, the purging device and sample syringe
are rinsed between samples with reagent
water. When an unusually concentrated sam-
ple is encountered, it is followed by analysis
of a reagent water blank to check for carry-
over. For samples containing large amounts
of water soluble materials, suspended solids,
high boiling compounds, or high levels or
purgeable compounds, the purge device is
washed with soap solution, rinsed with tap
and distilled water, and dried in an oven at
100-125 °C. The trap and other parts of the
system are also subject to contamination;
therefore, frequent bakeout and purging of
the entire system may be required.
3,4 Interferences resulting from samples
will vary considerably from source to source,
depending on the diversity of the industrial
complex or municipality being sampled.
283
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Pt. 136, App. A, Meth. 1624
40 CFR Ch. I (7-1-04 Ediflon)
4. Safety
4.1 The toxlcity or earcinogenieity of
each compound or reagent used in this meth-
od has not been precisely determined; how-
ever, each chemical compound should be
treated as a potential health hazard. Expo-
sure to these compounds should be reduced
to the lowest possible level. The laboratory
is responsible for maintaining a current
awareness file of OSHA regulations regard-
ing the safe handling of the chemicals speci-
fied in this method. A reference file of data
handling sheets should also be made avail-
able to all personnel involved in these anal-
yses. Additional information on laboratory
safety can be found in references 4-6.
4.2 The following compounds covered by
this method have been tentatively classified
as known or suspected human or mammalian
carcinogens: benzene, carbon tetrachloride,
chloroform, and vinyl chloride. Primary
standards of these toxic compounds should
be prepared in a hood, and a NIOSH/MESA
approved toxic gas respirator should be worn
when high concentrations are handled.
5. Apparatus and Materials
5.1 Sample bottles for discrete sampling,
5.1.1 Bottle—25 to 40 mL with screw cap
(Pierce 13075, or equivalent). Detergent wash,
rinse with tap and distilled water, and dry at
>105 °0 for one hr minimum before use.
5.1.2 Septum—Teflon-faced silicone
(Pierce 12722, or equivalent), cleaned as
above and baked at 100-200 °C, for one hour
minimum.
5.2 Purge and trap device—consists of
purging device, trap, and desorber. Complete
devices are commercially available.
5.2.1 Purging device—designed to accept 5
mL samples with water column at least 3 cm
deep. The volume of the gaseous head space
between the water and trap shall be less than
15 mL. The purge gas shall be introduced less
than 5 mm from the base of the water col-
umn and shall pass through the water as
bubbles with a diameter less than 3 mm. The
purging device shown in Figure 1 meets these
criteria.
5.2.2 Trap—25 to 30 cm x 2.5 mm i.d. min-
imum, containing the following:
5.2.2.1 Methyl silicone packing—one ±0,2
cm, 3 percent OV-1 on 60/80 mesh Chromosorb
W, or equivalent.
5.2.2.2 Porous polymer—15 ±1.0 cm, Tenax
G-C (2,6-diphenylene oxide polymer), 60/80
mesh, chromatographic grade, or equivalent.
5.2.2.3 Silica gel—8 ±1.0 cm, Davison
Chemical, 35/60 mesh, grade 15, or equivalent.
The trap shown in Figure 2 meets these spec-
ifications.
5.2.3 Desorber—shall heat the trap to 175
±5 °C in 45 seconds or less. The polymer sec-
tion of the trap shall not exceed 180 °C, and
the remaining sections shall not exceed 220
"C. The desorber shown in Figure 2 meets
these specifications.
5.2,4 The purge and trap device may be a
separate unit or coupled to a GC as shown in
Figures 3 and 4.
5.3 Gas chromatograph—shall be linearly
temperature programmable with initial and
final holds, shall contain a glass Jet sepa-
rator as the MS interface, and shall produce
results which meet the calibration (Section
7), quality assurance (Section 8), and per-
formance tests (Section 11) of this method.
5,3,1 Column—2.8 ±0.4 m x 2 ±0.5 mm i. d.
glass, paekekd with one percent SP-1000 on
Carbopak B, 60/80 mesh, or equivalent.
5.4 Mass spectrometer—70 eV electron im-
pact ionization; shall repetitively scan from
20 to 250 amu every 2-3 seconds, and produce
a unit resolution (valleys between m/z 174-176
less than 10 percent of the height of the m/z
175 peak), background corrected mass spec-
trum from 50 ng 4-bromo-fluorobenzene
(BFB) injected into the GC. The BFB spec-
trum shall meet the mass-intensity criteria
in Table 3. All portions of the GC column,
transfer lines, and separator which connect
the GC column to the ion source shall re-
main at or above the column temperature
during analysis to preclude condensation of
less volatile compounds.
5.5 Data system—shall collect and record
MS data, store mass intensity data in spec-
tral libraries, process GO/MS data and gen-
erate reports, and shall calculate and record
response factors.
5.5.1 Data acquisition—mass spectra shall
be collected continuously throughout the
analysis and stored on a mass storage device.
5.5.2 Mass spectral libraries—user created
libraries containing mass spectra obtained
from analysis of authentic standards shall be
employed to reverse search GC/MS runs for
the compounds of interest (Section 7.2),
5.5,3 Data processing—the data system
shall be used to search, locate, identify, and
quantify the compounds of interest in each
GC/MS analysis. Software routines shall be
employed to compute retention times and
EICP areas. Displays of spectra, mass
chromatograms, and library comparisons are
required to verify results.
5.5.4 Response factors and multipoint
calibrations—the data system shall be used
to record and maintain lists of response fac-
tors (response ratios for isotope dilution) and
generate multi-point calibration curves (Sec-
tion 7). Computations of relative standard
deviation (coefficient of variation) are useful
for testing calibration linearity. Statistics
on initial and on-going performance shall be
maintained (Sections 8 and 11).
5.6 Syringes—5 mL glass hypodermic,
with Luer-lok tips.
5.7 Micro syringes—10, 25, and 100 uL.
5.8 Syringe valves—2-way, with Luer ends
(Telfon or Kel-F).
284
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1624
5.9 Syringe—5 mL, gas-tight, with shut-
off valve,
5.10 Bottles—16 mL., serew-eap with
Telfon liner.
5.11 Balance—analytical, capable of
weighing 0,1 mg.
6. Reagents and Standards
6,1 Reagent water—water in which the
compounds of interest and interfering com-
pounds are not detected by this method (Sec-
tion 11.7). It may be generated by any of the
following methods:
6,1,1 Activated carbon—pass tap water
through a carbon bed (Calgon Piltrasorb-300,
or equivalent).
6.1.2 Water purifier—pass tap water
through a purifier (Millipore Super Q, or
equivalent).
6.1.3 Boil and purge—heat tap water to 90-
100 "C and bubble contaminant free inert gas
through it for approx one hour. While still
hot, transfer the water to screw-cap bottles
and seal with a Teflon-lined cap.
6,2 Sodium thiosulfate—ACS granular.
6,3 Metnanol—pesticide quality or equiva-
lent.
6.4 Standard solutions—purchased as so-
lution or mixtures with certification to their
purity, concentration, and authenticity, or
prepared from materials of known purity and
composition. If compound purity is 96 per-
cent or greater, the weight may be used
without correction to calculate the con-
centration of the standard.
6.5 Preparation of stock solutions—pre-
pare in methanol using liquid or gaseous
standards per the steps below. Observe the
safety precautions given in Section 4.
6.5.1 Place approx 9.8 mL of methanol in a
10 mL ground glass stoppered volumetric
flask. Allow the flask to stand unstoppered
for approximately 10 minutes or until all
methanol wetted surfaces have dried. In each
case, weigh the flask, immediately add the
compound, then immediately reweigh to pre-
vent evaporation losses from affecting the
measurement.
6.5.1.1 Liquids—using a 100 (iL syringe,
permit 2 drops of liquid to fall into the meth-
anol without contacting the leek of the
flask. Alternatively, inject a known volume
of the compound into the methanol in the
flask using a micro-syringe.
6.5.1.2 Gases (chloromethane, bromome-
thane, chloroethane, vinyl chloride)—fill a
valved 5 mL gas-tight syringe with the com-
pound. Lower the needle to approximately 6
mm above the methanol meniscus. Slowly
introduce the compound above the surface of
the meniscus. The gas will dissolve rapidly
in the methanol.
6.5.2 Fill the flask to volume, stopper,
then mix by inverting several times. Cal-
culate the concentration in mg/mL (jig/jiL )
from the weight gain (or density if a known
volume was injected).
6.5.3 Transfer the stock solution to a Tef-
lon sealed screw-oap-bottle. Store, with
minimal headspace, in the dark at -10 to
-20°C.
6.5,4 Prepare fresh standards weekly for
the gases and 2-chloroethylvinyl ether. All
other standards are replaced after one
month, or sooner if comparison with check
standards indicate a change in concentra-
tion. Quality control check standards that
can be used to determine the accuracy of
calibration standards are available from the
US Environmental Protection Agency, Envi-
ronmental Monitoring and Support Labora-
tory, Cincinnati, Ohio.
6.6 Labeled compound spiking solution—
from stock standard solutions prepared as
above, or from mixtures, prepare the spiking
solution to contain a concentration such
that a 5-10 jiL spike into each 5 mL sample,
blank, or aqueous standard analyzed will re-
sult in a concentration of 20 jig/L of each la-
beled compound. For the gases and for the
water soluble compounds (acrolein, acrylo-
nitrile, acetone, diethyl ether, and MEK), a
concentration of 100 ug/L may be used. In-
clude the internal standards (Section 7.5) in
this solution so that a concentration of 20 ng/
L in each sample, blank, or aqueous standard
will be produced.
6.7 Secondary standards—using stock so-
lutions, prepare a secondary standard in
methanol to contain each pollutant at a con-
centration of 500 jig/mL For the gases and
water soluble compounds (Section 6.6), a con-
centration of 2.5 mg/mL may be used.
6,7.1 Aqueous calibration standards—
using a 25 nL syringe, add 20 nL of the sec-
ondary standard (Section 6.7) to 50, 100, 200,
500, and 1000 mL of reagent water to produce
concentrations of 200, 100, 50, 20, and 10 ug/L,
respectively. If the higher concentration
standard for the gases and water soluble
compounds was chosen (Section 6,6), these
compounds will be at concentrations of 1000,
500, 250, 100, and 50 (ig/L in the aqueous cali-
bration standards.
6.7.2 Aqueous performance standard—an
aqueous standard containing all pollutants,
internal standards, labeled compounds, and
BPB is prepared daily, and analyzed each
shift to demonstrate performance (Section
11). This standard shall contain either 20 or
100 (tg/L of the labeled and pollutant gases
and water soluble compounds, 10 ug/L BPB,
and 20 jig/L of all other pollutants, labeled
compounds, and internal standards. It may
be the nominal 20 nif/L aqueous calibration
standard (Section 6.7.1).
6.7.3 A methanolic standard containing
all pollutants and internal standards is pre-
pared to demonstrate recovery of these com-
pounds when syringe injection and purge and
trap analyses are compared. This standard
shall contain either 100 ng/mL or 500 ng/mL
of the gases and water soluble compounds,
and 100 (ig/mL of the remaining pollutants
285
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Pt, 136, App. A, Meth. 1624
40 CFR Ch. I (7-1-04 Edition)
and internal standards (consistent with the
amounts in the aqueous performance stand-
ard in 6.7.2).
6.7.4 Other standards which may be need-
ed are those for test of BFB performance
(Section 7.1) and for collection of mass spec-
tra for storage in spectral libraries (Section
7.2).
7. Calibration
7.1 Assemble the gas ohromatographic ap-
paratus and establish operating conditions
given in table 2. By injecting: standards into
the S5C, demonstrate that the analytical sys-
tem meets the detection limits in table 2 and
the mass-intensity criteria in table 3 for 50
ngr BFB,
7.2 Mass spectral libraries—detection and
identification of the compound of interest
are dependent upon the spectra stored in
user created libraries.
7.2.1 Obtain a mass spectrum of each pol-
lutant and labeled compound and each inter-
nal standard by analyzing an authentic
standard either singly or as part of a mix-
ture in which there is no interference be-
tween closely eluted components. That only
a single compound is present is determined
by examination of the spectrum. Fragments
not attributable to the compound under
study indicate the presence of an interfering
compound. Adjust the analytical conditions
and scan rate (for this test only) to produce
an undistorted spectrum at the QC peak
maximum. An undistorted spectrum will
usually be obtained if five complete spectra
are collected across the upper half of the OC
peak. Software algorithms designed to "en-
hance" the spectrum may eliminate distor-
tion, but may also eliminate authentic m/z*s
or introduce other distortion.
7.2.3 The authentic reference spectrum is
obtained under BFB tuning conditions (Sec-
tion 7.1 and table 3) to normalize It to spec-
tra from other instruments.
7.2.4 The spectrum is edited by saving the
5 most intense mass spectral peaks and all
other mass spectral peaks greater than 10
percent of the base peak. This spectrum is
stored for reverse search and for compound
confirmation.
7.3 Assemble the purge and trap device.
Pack the trap as shown in Figure 2 and con-
dition overnight at 170-180 °C by
backflushing with an inert gas at a flow rate
of 20-30 mli/min. Condition traps daily for a
minimum of 10 minutes prior to use.
7.3.1 Analyze the aqueous performance
standard (Section 6.7.2) according to the
purge and trap procedure In Section 10. Com-
pute the area at the primary m/z (table 4) for
each compound. Compare these areas to
those obtained by injecting one \iL of the
methanolie standard (Section 6.7.3) to deter-
mine compound recovery. The recovery shall
be greater than 20 percent for the water solu-
ble compounds, and 60-110 percent for all
other compounds. This recovery is dem-
onstrated initially for each purge and trap
GC/MS system. The test is repeated only if
the purge and trap or GC/MS systems are
modified in any way that might result in a
change in recovery.
7.3.2 Demonstrate that 100 ng toluene (or
toluene-d8) produces an area at m/z 91 (or 99)
approx one-tenth that required to exceed the
linear range of the system. The exact value
must be determined by experience for each
instrument. It is used to match the calibra-
tion range of the Instrument to the analyt-
ical range and detection limits required.
7.4 Calibration by isotope dilution—the
isotope dilution approach is used for the
purgeable organic compounds when appro-
priate labeled compounds are available and
when interferences do not preclude the anal-
ysis. If labeled compounds are not available,
or interferences are present, internal stand-
ard methods (Section 7.5 or 7.6) are used. A
calibration curve encompassing the con-
centration range of interest is prepared for
each compound determined. The relative re-
sponse (RR) vs concentration (ug/L) is plot-
ted or computed using a linear regression.
An example of a calibration curve for tol-
uene using toluene-d8 is given in figure 5.
Also shown are the ±10 percent error limits
(dotted lines). Relative response is deter-
mined according to the procedures described
below. A minimum of five data points are re-
quired for calibration (Section 7.4.4).
7.4.1 The relative response (RR) of pollut-
ant to labeled compound is determined from
isotope ratio values calculated from acquired
data. Three isotope ratios are used in this
process:
Rx=the Isotope ratio measured in the pure
pollutant (figure 8A).
Ry=the isotope ratio of pure labeled com-
pound (figure 6B).
Rm=the isotope ratio measured in the ana-
lytical mixture of the pollutant and la-
beled compounds (figure 6C).
The correct way to calculate RR is:
RR=(Ry-R»,} (Kx+lV(Rm-Rx){Ry+l) If Rm is
not between 2R, and 0.5Rx, the method does
not apply and the sample is analyzed by in-
ternal or external standard methods (Section
7.5 or 7.6).
7.4.2 In most cases, the retention times of
the pollutant and labeled compound are the
same and isotope ratios (R*s) can be cal-
culated from the BICP areas, where: R=(area
at mi/z)/(area at mz/z) If either of the areas is
zero, it is assigned a value of one in the cal-
culations; that is, if: area of mi/z-50721, and
area of ni2/z=0, then R=50721/l=50720. The m/
z's are always selected such that RX>R».
When there is a difference in retention times
(RT) between the pollutant and labeled com-
pounds, special precautions are required to
determine the isotope ratios.
Rx, Ry, and Rm are defined as follows:
286
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Environmental Protection Agency
Pt. 136, App. A, Meth, 1624
Rx=farea nVz (at RTO]/1
By=l/[area m^'z (at RT2)]
Rm=[area m,/z (at RT,)]/[area m2/z (at RT2)]
7.4.3 An example of the above calculations
can be taken from the data plotted In figure
6 for toluene and toluene-d8. For these data,
Rx=168920/l=16890Q, R,=l/80960=0.00001640, and
Rm=96868/82508=1.174. The RR for the above
data is then calculated using the equation
given in Section 7.4.1. For the example,
BR=1.174,
NOTE: Not all labeled compounds elute be-
fore their pollutant analogs.
7.4.4 To calibrate the analytical system
by isotope dilution, analyze a 5 mL aliquot
of each of the aqueous calibration standards
(Section 6.7.1) spiked with an appropriate
constant amount of the labeled compound
spiking solution (Section 6.6), using the
purge and trap procedure In section 10. Com-
pute the RR at each concentration,
7,4.5 Linearity—if the ratio of relative re-
sponse to concentration for any compound is
constant (less than 20 percent coefficient of
variation) over the 5 point calibration range,
an averaged relative response/concentration
ratio may be used for that compound; other-
wise, the complete calibration curve for that
compound shall be used over the 5 point cali-
bration range.
7.5 Calibration by internal standard—used
when criteria for isotope dilution (Section
7.4) cannot be met. The method is applied to
pollutants having no labeled analog and to
the labeled compounds. The internal stand-
ards used for volatiles analyses are bromo-
chlorometliane, 2-bromo-l-chloropropane,
and 1,4-diehlorobutane, Concentrations of
the labeled compounds and pollutants with-
out labeled analogs are computed relative to
the nearest eluted internal standard, as
shown in table 2.
7.5.1 Response factors—calibration re-
quires the determination of response factors
(RF) which are defined by the following
equation:
RF=(A«xCi,)/(AisxCs), where A5 is the EICP
area at the characteristic m/z for the com-
pound in the daily standard. A,s is the EICP
area at the characteristic m/z far the inter-
nal standard.
Cis is the concentration (ug/L) of the inter-
nal standard
Cs is the concentration of the pollutant in
the daily standard.
7.5.2 The response factor is determined at
10, 20, 50, 100, and 200 ug/L for the pollutants
(optionally at five times these concentra-
tions for gases and water soluble pollut-
ants—see Section 6.7), in a way analogous to
that for calibration by isotope dilution (Sec-
tion 7.4.4). The RF is plotted against con-
centration for each compound in the stand-
ard (Cj to produce a calibration curve,
7.5.3 Linearity—if the response factor
(RP) for any compound is constant (less than
35 percent coefficient of variation) over the 5
point calibration range, an averaged re-
sponse factor may be used for that com-
pound; otherwise, the complete calibration
curve for that compound shall be used over
the 5 point range.
7.6 Combined calibration—by adding the
isotopically labeled compounds and internal
standards (Section 6.6) to the aqueous cali-
bration standards (Section 6.7.1), a single set
of analyses can be used to produce calibra-
tion curves for the isotope dilution and in-
ternal standard methods. These curves are
verified each shift (Section 11.5) by purging
the aqueous performance standard (Section
6.7.2). Recalibration is required only if cali-
bration and on-going performance (Section
11.5) criteria cannot be met.
8. Quality Assurance/Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality assur-
ance program. The minimum requirements
of this program consist of an initial dem-
onstration of laboratory capability, analysis
of samples spiked with labeled compounds to
evaluate and document data quality, and
analysis of standards and blanks as tests of
continued performance. Laboratory perform-
ance is compared to established performance
criteria to determine if the results of anal-
yses meet the performance characteristics of
the method.
8.1.1 The analyst shall make an initial
demonstration of the ability to generate ac-
ceptable accuracy and precision with this
method. This ability is established as de-
scribed in Section 8.2.
8.1.2 The analyst is permitted to modify
this method to improve separations or lower
the costs of measurements, provided all per-
formance specifications are met. Bach time a
modification is made to the method, the ana-
lyst is required to repeat the procedure in
Section 8.2 to demonstrate method perform-
ance.
8.1.3 Analyses of blanks are required to
demonstrate freedom from contamination
and that the compounds of interest and
interfering compounds have not been carried
over from a previous analysis (Section 3).
The procedures and criteria for analysis of a
blank: are described in Sections 8.5 and 11.7.
8.1.4 The laboratory shall spike all sam-
ples with labeled compounds to monitor
method performance. This test is described
in Section 8.3. When results of these spikes
indicate atypical method performance for
samples, the samples are diluted to bring
method performance within acceptable lim-
its (Section 14.2).
8,1,5 The laboratory shall, on an on-going
basis, demonstrate through the analysis of
the aqueous performance standard (Section
8.7.2) that the analysis system is in control.
This procedure is described in Sections 11.1
and 11.5.
287
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Pt. 136, App. A, Mefh. 1624
40 CFR Ch. I (7-1-04 Edition)
8.1.6 The laboratory shall maintain, rec-
ords to define the quality of data that is gen-
erated. Development of accuracy statements
is described in Sections 8.4 and 11.5.2.
8.2 Initial precision and accuracy—to es-
tablish the ability to generate acceptable
precision and accuracy, the analyst shall
perform the following operations:
8.2.1 Analyze two sets of four 5-mL
aliquots (8 aliquots total) of the aqueous per-
formance standard (Section 6.7.2) according
to the method beginning in Section 10.
8.2.2 Usingr results of the first set of four
analyses in Section 8.2.1, compute the aver-
age recovery (X) in \\gfL and the standard de-
viation of the recovery (s) in |ig/L for each
compound, by isotope dilution for pollul-
tants with a labeled analog, and by internal
standard for labeled compounds and pollut-
ants with no labeled analog.
8.2.3 Por each compound, compare s and X
with the corresponding limits for Initial pre-
cision and accuracy found in table 5. If s and
X for all compounds meet the acceptance cri-
teria, system performance is acceptable and
analysis of _blanks and samples may begin. If
individual X falls outside the range for accu-
racy, system performance is unacceptable
for that compound.
NOTE: The large number of compounds in
table 5 present a substantial probability that
one or more will fail one of the acceptance
criteria when all compoulds are analyzed. To
determine if the analytical system is out of
control, or if the failure can be attributed to
probability, proceed as follows:
8.2.4 Usingr the results of the second set of
four analyses, compute s and X for only
those compounds which failed the test of the
first set of four analyses (Section 8.2.3). If
these compounds now pass, system perform-
ance is acceptable for all compounds and
analysis of blanks and samples may begin. If,
however, any of the same compounds fail
again, the analysis system is not performing
properly for the compound(s) in question. In
this event, correct the problem and repeat
the entire test (Section 8.2.1).
8.3 The laboratory shall spike all samples
with labeled compounds to assess method
performance on the sample matrix.
8.3.1 Spike and analyze each sample ac-
cording to the method beginning in Section
10.
8.3.2 Compute the percent recovery (P) of
the labeled compounds using the internal
standard method (Section 7.5).
8.3.3 Compare the percent recovery for
each compound with the corresponding la-
beled compound recovery limit in table 5. If
the recovery of any compound falls outside
its warning limit, method performance is un-
acceptable for that compound in that sam-
ple. Therefore, the sample matrix is complex
and the sample is to be diluted and reana-
lyzed, per Section 14.2.
8.4 As part of the QA program for the lab-
oratory, method accuracy for wastewater
samples shall tie assessed and records shall
be maintained. After the analysis of five
wastewater samples for which the labeled
compounds pass the tests in Section 8.3.3,
compute the average percent recovery (P)
and the standard deviation of the percent re-
covery (Sp) for the labeled compounds only.
Express the accuracy assessment as a per-
cent recovery interval from P —2sp to P+2sp.
Por example, if P=90% and Sp=10%, the accu-
racy interval is expressed as 70-110%. Update
the accuracy assessment for each compound
on a regular basis (e.g. after each 5-10 new
accuracy measurements).
8,5 Blanks—reagent water blanks are ana-
lyzed to demonstrate freedom from carry-
over (Section 3) and contamination.
8.5.1 The level at which the purge and
trap system will carry greater than 5 \tg/Li of
a pollutant of interest (table 1) into a suc-
ceeding blank shall be determined by ana-
lyzing successively larger concentrations of
these compounds. When a sample contains
this concentration or more, a blank shall be
analyzed immediately following this sample
to demonstrate no carry-over at the 5 iigfLi
level.
8.5.2 With each sample lot (samples ana-
lyzed on the same 8 hr shift), a blank shall be
analyzed immediately after analysis of the
aqueous performance standard (Section 11.1)
to demonstrate freedom from contamina-
tion. If any of the compounds of interest
(table 1) or any potentially interfering com-
pound is found in a blank at greater than 10
jtg/L (assuming a response factor of 1 relative
to the nearest eluted internal standard for
compounds not listed in table 1), analysis of
samples is halted until the source of con-
tamination is eliminated and a blank shows
no evidence of contamination at this level.
8.6 The specifications contained in this
method can be met if the apparatus used is
calibrated properly, then maintained in a
calibrated state.
The standards used for calibration (Section
7), calibration verification (Section 11,5) and
for initial (Section 8.2) and on-going (Section
11.5) precision and accuracy should be iden-
tical, so that the most precise results will be
obtained. The GC/MS instrument in par-
ticular will provide the most reproducible re-
sults if dedicated to the settings and condi-
tions required for the analyses of volatiles
by this method.
8.7 Depending on specific program re-
quirements, field replicates may be collected
to determine the precision of the sampling
technique, and spiked samples may be re-
quired to determine the accuracy of the
analysis when internal or external standard
methods are used.
288
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1624
9. Sample Collection, Preservation, and
Handling
9,1 Grab samples are collected in glass
containers having a total volume greater
than 20 mL, Pill sample bottles so that no
air bubbles pass through tie sample as the
bottle is filled. Seal each bottle so that no
air bubbles are entrapped. Maintain the her-
metic seal on tie sample bottle until time of
analysis.
9.2 Samples are maintained at 0-4 °C from
the time of collection until analysis. If the
sample contains residual chlorine, add so-
dium thiostilfate preservative (10 mg/40 mL)
to the empty sample bottles just prior to
shipment to the sample site. EPA Methods
330.4 and 330.5 may be used for measurement
of residual chlorine (Reference 8). If preserv-
ative has been added, shake bottle vigor-
ously for one minute immediately after fill-
ing-.
9.3 Experimental evidence indicates that
some aromatic compounds, notably benzene,
toluene, and ethyl benzene are susceptible to
rapid biological degradation under certain
environmental conditions. Refrigeration
alone may not be adequate to preserve these
compounds in wastewaters for more than
seven days. For this reason, a separate sam-
ple should be collected, acidified, and ana-
lyzed when these aromatics are to be deter-
mined. Collect about 500 ml/ of sample in a
clean container.
Adjust the pH of the sample to about 2 by
adding HC1 (1+1) while stirring. Cheek pH
with narrow range {1.4 to 2.8) pH paper. Pill
a sample container as described in Section
9,1. If residual chlorine is present, add so-
dium thiosulfate to a separate sample con-
tainer and fill as in Section 9.1.
9.4 All samples shall be analyzed within 14
days of collection.
10. Purge, Trap, and GC/MS Analysis
10.1 Remove standards and samples from
cold storage and bring to 20-25 °.
10.2 Adjust the purge gas flow rate to 40 ±4
mL/min. Attach the trap inlet to the purging
device and set the valve to the purge mode
(figure 3). Open the syringe valve located on
the purging device sample introduction nee-
dle (figure 1).
10.3 Remove the plunger from a 5-mL sy-
ringe and attach a closed syringe valve. Open
the sample bottle and carefully pour the
sample into the syringe barrel until it over-
flows. Replace the plunger and compress the
sample. Open the syringe valve and vent any
residual air while adjusting the sample vol-
ume to 5.0 mL. Because this process of tak-
ing an aliquot destroys the validity of the
sample for future analysis, fill a second sy-
ringe at this time to protect against possible
loss of data. Add an appropriate amount of
the labeled compound spiking solution (Sec-
tion 6.6) through the valve bore, then close
the valve.
10.4 Attach the syringe valve assembly to
the syringe valve on the purging device.
Open both syringe valves and inject the sam-
ple into the purging chamber.
10.5 Close both valves and purge the sam-
ple for 11.0 ±0.1 minutes at 20-25 °C.
10.6 After the 11 minute purge time, at-
tach the trap to the chromatograph and set
the purge and trap apparatus to the desorb
mode (figure 4). Desorb the trapped com-
pounds into the GC column by heating the
trap to 170-180 "C while backflushing with
carrier gas at 20-60 mL/min for four minutes.
Start MS data acquisition upon start of the
desorb cycle, and start the GC column tem-
perature program 3 minutes later. Table 1
summarizes the recommended operating con-
ditions for the gas chromatograph. Included
in this table are retention times and detec-
tion limits that were achieved under these
conditions. Other columns may be used pro-
vided the requirements in Section 8 can be
met. If the priority pollutant gases produce
GC peaks so broad that the precision and re-
covery specifications (Section 8,2) cannot be
met, the column may be cooled to ambient
or sub-ambient temperatures to sharpen
these peaks.
10.7 While analysis of the desorbed com-
pounds proceeds, empty the purging chamber
using the sample introduction syringe. Wash
the chamber with two 5-mL portions of rea-
gent water. After the purging device has
been emptied, allow the purge gas to vent
through the chamber until the frit is dry, so
that it is ready for the next sample.
10.8 After desorbing the sample for four
minutes, recondition the trap by returning
to the purge mode. Walt 15 seconds, then
close the syringe valve on the purging device
to begin gas flow through the trap. Maintain
the trap temperature at 170-180 "C. After ap-
proximately seven minutes, turn off the trap
heater and open the syringe valve to stop the
gas flow through the trap. When cool, the
trap is ready for the next sample.
11. System Performance
11.1 At the beginning of each 8 hr shift
during which analyses are performed, system
calibration and performance shall be verified
for all pollutants and labeled compounds.
For these tests, analysis of the aqueous per-
formance standard (Section 6.7.2) shall be
used to verify all performance criteria. Ad-
justment and/or recalibration (per Section 7)
shall be performed until all performance cri-
teria are met. Only after all performance cri-
teria are met may blanks and samples be
analyzed.
11.2 BFB spectrum validity—the criteria
in table 3 shall be met.
11.3 Retention times—the absolute reten-
tion times of all compounds shall approxi-
mate those given in Table 2.
289
-------
Pt. 136, App. A, Meth. 1624
40 CFR Ch. I (7-1-04 Edition)
11.4 GC resolution—the valley height be-
tween toluene and toluene-da (at m/z 91 and
99 plotted on the same graph) shall be less
than 10 percent of the taller of the two
peaks,
11,5 Calibration verification and on-going
precision and accuracy—compute the con-
centration of each polutant (Table 1) by iso-
tope dilution (Section 7.4) for those
compmunds which have labeled analogs.
Compute the concentration of each pollutant
(Table 1) which has no labeled analog by the
internal standard method (Section 7.S). Com-
pute the concentration of the labeled com-
pounds by the internal standard method.
These concentrations are computed based on
the calibration data determined in Section 7.
11.5.1 For each pollutant and labeled com-
pound, compare the concentration with the
corresponding limit for on-going accuracy in
Table 5. If all compmunds meet the accept-
ance criteria, system performance is accept-
able and analysis of blanks and samples may
continue. If any Individual value falls out-
side the range given, system performance ie
unacceptable for that compound.
NOTE: The large number of compounds in
Table 6 present a substantial probability
that one or more will fail the acceptance cri-
teria when all compounds are analyzed. To
determine if the analytical system is out of
control, or if the failure may be attributed
to probability, proceed as follows:
11,5.1.1 Analyze a second aliquot of the
aqueous performance standard (Section
6.7.2).
11.5.1.2 Compute the concentration for
only those compounds which failed the first
test (Section 11.5.1), If these compounds now
pass, system performance is acceptable for
all compounds and analyses of blanks and
samples may proceed. If, however, any of the
compounds fail again, the measurement sys-
tem is not performing properly for these
compounds. In this event, locate and correct
the problem or recalibrate the system (Sec-
tion 7), and repeat the entire test (Section
11.1) for all compounds.
11,5.2 Add results which pass the speci-
fication in 11.5.1,2 to initial (Section 8.2) and
previous on-going data, Update QG charts to
form a graphic representation of laboratory
performance (Figure 7). Develop a statement
of accuracy for each pollutant and labeled
compound by calculating the average per-
centage recovery (R) and the standard devi-
ation of percent recovery (ST). Express the ac-
curacy as a recovery interval from R — 2s, to
R+2sr. For example, if R=95% and Sr=5%, the
accuracy is 85-105 percent.
12. Qualitative Determination—Accomplished
by Comparison of Data from Analysis of a
Sample or Blank with Data from Analysis of
the Shift Standard (Section 11.1). Identifica-
tion is Confirmed When Spectra and Reten-
tion Times Agree Per the Criteria Below
12,1 Labeled compounds and pollutants
having no labeled analog:
12.1.1 The signals for all characteristic
masses stored in the spectral library (Sec-
tion 7.2.4) shall be present and shall maxi-
mize within the same two consecutive scans.
12.1.2 Either (1) the background corrected
EICP areas, or (2) the corrected relative in-
tensities of the mass spectral peaks at the
OC peak maximum shall agree within a fac-
tor of two (0.5 to 2 times) for all masses
stored in the library.
12.1.3 The retention time relative to the
nearest eluted internal standard shall be
within ±7 scans or ±20 seconds, whichever is
greater.
12,2 Pollutants having a labeled analog:
12,2.1 The signals for all characteristic
masses stored in the spectral library (Sec-
tion 7.2.4) shall be present and shall maxi-
mize within the same two consecutive scans.
12.2.2 Either (1) the background corrected
EICP areas, or (2) the corrected relative in-
tensities of the mass spectral peaks at the
GC peak maximum shall agree within a fac-
tor of two for all masses stored in the spec-
tral library.
12.2.3 The retention time difference be-
tween the pollutant and its labeled analog
snail agree within ±2 scans or ±6 seconds
(whichever is greater) of this difference in
the shift standard (Section 11,1).
12.3 Masses present in the experimental
mass spectrum that are not present in the
reference mass spectrum shall be accounted
for by contaminant or background ions. If
the experimental mass spectrum is contami-
nated, an experienced spectrometrist (Sec-
tion 1.4) is to determine the presence or ab-
sence of the compound,
13. Quantitative Determination
13,1 Isotope dilution—by adding a known
amount of a labeled compound to every sam-
ple prior to purging, correction for recovery
of the pollutant can be made because the pol-
lutant and its labeled analog exhibit the
same effects upon purging, desorption, and
gas chromatography. Relative response (RR)
values for sample mixtures are used in con-
junction with calibration curves described in
Section 7.4 to determine concentrations di-
rectly, so long as labeled compound spiking
levels are constant. For the toluene example
given In Figure 6 (Section 7.4.3), RR would be
equal to 1.174. For this RR value, the toluene
calibration curve given in Figure 5 indicates
a concentration of 31.8 (ig/L.
290
-------
Environmental Protection Agency
ft. 136, App. A, Meth. 1624
13.2 Internal standard—calculate the con-
centration using the response factor deter-
mined from calibration data (Section 7.5)
and the following equation:
Concentration =(AB x CiS)/(Ais x BF) where
the terms are as defined in Section 7.5.1,
13.3 If the EICP area at the quantitetion
mass for any compound exceeds the calibra-
tion range of the system, the sample is di-
luted by successive factors of 10 and these di-
lutions are analyzed until the area is within
the calibration range,
13.4 Report results for all pollutants and
labeled compounds (Table 1) found in all
standards, blanks, and samples, in ng/L to
three significant figures. Results for samples
which have been diluted are reported at the
least dilute level at which the area at the
quantitation mass is within the calibration
range (Section 13.3) and the labeled com-
pound recovery is within the normal range
for the Method (Section 14,2).
14. Analysis of Complex Samples
14.1 Untreated effluents and other sam-
ples frequently contain high levels (>1000 (ig/
L) of the compounds of interest and of inter-
fering compounds. Some samples will foam
excessively when purged: others will over-
load the trap/or GC column.
14.2 Dilute 0.5 mL of sample with 4.5 mL
of reagent water and analyze this diluted
sample when labeled compound recovery is
outside the range given in Table 5. If the re-
covery remains outside of the range for this
diluted sample, the aqueous performance
standard shall be analyzed (Section 11) and
calibration verified (Section 11.5). If the re-
covery for the labeled compniund in the
aqueous performance standard is outside the
range given in Table 5, the analytical system
is out of control. In this case, the instrumelt
shall be repaired, the performance specifica-
tiOQS in Section 11 shall be met, and the
analysis of the undiluted sample shall be re-
peated. If the recovery for the aqueous per-
formance standard is within the range given
in Table 5, the method does not work on the
sample being analyzed and the result may
not be reported for regulatory compliance
purposes.
14,3 Reverse search computer programs
can misinterpret the spectrum of ehroma-
tographically unresolved pollutant and la-
beled compound pairs with overlapping spec-
tra when a high level of the pollutant is
present. Examine each ehromatograrn for
peaks greater than the height of the internal
standard peaks. These peaks can obscure the
compounds of interest.
15. Method Performance
15.1 The specifications for this method
were taken from the inter-laboratory valida-
tion of EPA Method 624 (reference 9). Method
1624 has been shown to yield slightly better
performance on treated effluents than Meth-
od 624. Additional method performance data
can be found in Reference 10.
References
1. "Performance Tests for the Evaluation of
Computerized Gas Chromatography/Mass
Spectrornetry Equipment and Laboratories,"
USEPA, EMSL/Cincinnati, OH 45268, EPA-
600/4-80-025 (April 1980).
2. Bellar, T,A. and Liehtenberg, J.J.,
"Journal American Water Works Associa-
tion," 66, 739 (1974).
3. Bellar, T,A, and Liehtenberg, J.J.,
"Semi-automated Headspace Analysis of
Drinking Waters and Industrial Waters for
Purgeable Volatile Organic Compounds," in
Measurement of Organic Pollutants Water and
Waste-water, C.E. VanHall, ed., American So-
ciety for Testing Materials, Philadelphia,
PA, Special Technical Publication 686, (1978).
4. "Working with Carcinogens," DHBW,
PHS, NIOSH, Publication 77-206 (1977).
5. "OSHA Safety and Health Standards,
General Industry," 29 CFR part 1910, OSHA
2206, (1976).
6. "Safety in Academic Chemistry Labora-
tories," American Chemical Society Publica-
tion, Committee on Chemical Safety (1979).
7. "Handbook of Analytical Quality Control
in Water and Wastewater Laboratories,"
USEPA, EMSL/Clncinnati, OH 45268. EPA-4-
79-019 (March 1979),
8. "Methods 330,4 and 330.5 for Total Resid-
ual Chlorine," USEPA, EMSL/Cincinnati, OH
45268, EPA^I-79-020 (March 1979).
9. "EPA Method Study 29 EPA Method 624—
Purgeables," EPA 600/4-84-054, National Tech-
nical Information Service, PB84-209915,
Springfield, Virginia 22161, June 1984.
10, "Colby, B.N., Beimer, R.G., Rushneck,
D,B,, and Telliard, W.A., "Isotope Dilution
Gas Chromatography-Mass Spectrornetry for
the Determination of Priority Pollutants in
Industrial Effluents," USEPA, Effluent
Guidelines Division, Washington, DC 20460
(1980).
TABLE 1— VOLATILE ORGANIC COMPOUNDS ANALYZED BY ISOTOPE DILUTION Gc/MS
Compound
BromodicWofomeihane .,
Store!
81552
34210
34215
34030
32101
CAS reg-
istry
§7-@4_ •)
107-02-8
107-13-1
71 43-2
75-27-4
EPA-
EGD
516 V
002 V
003 V
004 V
048V
NPDES
001 V
002V
003 V
012V
291
-------
Pt. 136, App. A, Meth. 1624
40 CFR Ch. I (7-1-04 Edition)
TABLE 1— VOLATILE ORGANIC COMPOUNDS ANALYZED BY ISOTOPE DILUTION Gc/MS—Continued
Compound
1 1 2 2-tefrachloroethane ..,,,,., ,. ,
Store!
32104
34413
32102
34301
34311
34576
32106
34418
32105
34496
34536
34501
34546
34541
34704
34699
81576
81582
34371
34423
81595
34516
34475
34010
34506
34511
39180
39175
CAS reg-
istry
75-25-2
74-83-9
56-23-5
108-90-7
75-00-3
110-75-0
67-66-1
74-87-3
124-48-1
75-34-3
107-06-2
75-3S-4
156-60-5
78-87-5
10061-01-5
10061-02-6
60-29-7
123-91-1
100-41-4
75-09-2
78-93-3
79-34-5
127-18-4
108-88-3
71-55-6
79-00-5
79-01-6
75-01 -4
EPA-
EGD
047 V
046V
006V
007 V
016 V
019V
023V
045 V
051 V
013V
010V
029 V
030V
032V
033 V
515 V
527V
038V
044 V
SUV
015V
085V
086V
011 V
014V
087V
088V
NPDES
005 V
020V
006V
007 V
009 V
010V
011 V
021 V
008V
014V
015V
016V
026V
017V
019V
022V
023V
024V
025V
027V
028V
029V
031 V
TABLE 2—GAS CHROMATOGRAPHY OF
PUHGEABLE ORGANIC COMPOUNDS BY ISO-
TOPE DILUTION GC/MS
TABLE 2—GAS CHROMATOGRAPHY OF
PURGEABLE ORGANIC COMPOUNDS BY ISO-
TOPE DILUTION GC/MS—Continued
286
388
244
230
330
614
Compound
Bromochloromethane (I.S.)
Chloromethane-d3
Chioromethane *
Bramomethane-d3
Bromomethane .... .
Vinyl chloride-CIS
Vinyl chloride
Chioroothane-dS
Chloroethane
Methylene chlorlde-d2 .
Methytene chloride
Acetone-d6 . .....
Acetone
Acrolein . . ,
Acrylonitrile-d3
Acrylonitfile
I,1-dichloroethene-d2
1,1-dichloroethgne
1 ,1 -dichloroetnane-d3
1 1 -dichioroethane
Diethyl ether-d1G
Diethyl ether
Trans-1 ,2-dichloroethene~d2 ....
Trans-1,2-dichloroethene
Methyl ethyl ketone-d3 . .
Methyl ethyl ketooe
Chloroform-1 3C1
Chloroform . . .... ,
1 ^-dichioroethane^
1 ,2-dichloroethane
Ref
EGD
No.
181
181
245
181
246
181
288
181
216
181
244
181
616
181
181
203
181
229
181
213
181
615
181
230
181
614
181
223
181
210
Mean
re-
ten-
tion
time
(sec)
730
147
148
243
246
301
304
378
386
512
517
554
565
566
606
612
696
696
778
786
804
820
821
821
840
848
861
881
901
910
Mln-
mum
level
(2)
Jtf
10
50
50
50
50
50
10
50
50
10
10
50
50
50
50
50
10
10
10
10
50
50
10
10
50
50
10
10
10
10
EGD
No.
m
211
311
527
206
306
248
348
232
332
233
333
287
387
204
304
251
351
214
314
019
182
247
347
215
315
285
385
183
286
386
Compound
1,1,1-trichioroethane-13C2
1 1 1 -trichloroethane
p-dioxane
Carbon tetrachioride-13C1
Carbon tetrachloride . ......
Bromodichloromethane-13Cl ...
Bromodichloromethane
1 ,2-dichioropropane-d6
1 ,2-dichloropropane
Trans-1 ,3-dichloropropene-d4 ..
Trans-1 ,3-dichioropropene
Trichloroethene-13C1
Trichloroethene
Benzene-d6
Benzene
Chlorodibromemethane-13C1 ..
Chtorodibromornethane
1,1,2-trlchloroethane-13C2
1,1,2-trichloroelhane
2-chloroethylvinyl ether
2-bromo-1-ch!oropropane 0-S.)
Bromoform-13C1
Bromoform
1,1,2,2-tetrachloroethane-d2 ....
1 ,1 ,2,2-tetrachloroethane
Tetrach!oroetherte-13C2
Tetrachloroethene
1 ,4-dichlorobutale (int std)
Toiuene-d8
Toluene
Hef
EQD
No.
181
211
181
182
206
182
248
182
232
182
233
182
287
182
204
182
251
182
214
182
182
182
247
183
215
183
285
183
183
286
Mean
re-
ten-
tion
time
(sec)
989
999
1001
1018
1018
1045
1045
1123
1134
1138
1138
1172
1187
1200
1212
1222
1222
1224
1224
1278
1306
1386
1386
1525
1525
1528
1528
1555
1603
1619
Min-
rnum
level
(2)
([f
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
292
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Environmental Protection Agency
Ft. 136, App. A, Meth. 1624
TABLE 2—GAS CHROMATOGRAPHY OF
PURGEABLE ORGANIC COMPOUNDS BY ISO-
TOPE DILUTION GC/MS—Continued
TABLE 4—VOLATILE ORGANIC COMPOUND
CHARACTERISTIC MASSES
E6D
NO.
(1)
207
307
238
338
185
Compound
Chlorobenzene
Bromoftuorobenzene
Ref
EQD
No.
183
207
183
238
183
Mean
re-
time
(sec)
1679
1679
1802
1820
1985
Min-
mum
level
(*)
(tr
10
10
10
10
10
(1) Reference numbers beginning with 0, 1 or 5 indicate a
pollutant quantified by the internal standard method; reference
numbers beginning with 2 or 6 indicate a labeled compound
quantified by th© internal standard method; reference numbers
beginning with 3 or 7 indicate a pollutant quantified by isotope
dilution.
(2) This is a minimum level at which the analytical system
shall give recognizable mass spectra (background corrected)
and acceptable calibration points- Column: 2.4m (8 ft) x 2 mm
i.d. glass, packed with one percent SP-1000 coated on 60/80
Carbopak B. Carrier gas: helium at 40 mL/min. Temperature
program: 3 min at 45 °C, 8 °C per min to 240 °C, hold at 240
SC for 15 minutes.
NOTE: The specifications in this table were developed from
data collected from three wastewater laboratories,
TABLE 3—BFB MASS-INTENSITY SPECIFICATIONS
Mass
50
75
95
96
173
174
175
176
177
Intensity required
15 to 40 percent of mass 95.
30 to 60 percent of mass 85.
base peak, 100 percent.
5 to 9 percent of mass 95.
<2 percent of mass 1 74.
>5Q percent of mass 95.
5 to 9 percent of mass 174
95 to 101 percent of mass 174
5 to 9 percent of mass 1 76.
Labeled compound
Chloroethan©
Chloroform ..... ,
Trans-1 ,2-dichloroethene
Cis-1 ,3-dtehloropropene
Trans-1 ,3-dichtoropropens
Diethyl ether
Ethylbenzene . ..
Methylene chloride
Methyt ethyi ketone -
Tetrachioroethene . .,
Trichloroethene .
Vinyl chloride
Analog
d6
d2
d3
d6
13C
13C
d3
13C
d5
d5
d7
13C
da
13C
d3
d4
d2
d2
d6
d4
d4
d10
da
d10
02
d3
d2
13C2
d8
d3
13C2
13C
d3
Primary m/
z's
58/84
56/58
53/56
78/84
83/86
173/176
96/99
47/46
112/117
64/71
106/113
85/86
50/53
129/130
63/66
62/67
61/65
61/65
63/67
75/79
75/79
74/84
88/96
106/116
84/88
72/?5
83/B4
166/172
92/88
97/1 02
83/84
95/133
62/65
TABLE 5—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS
Acceptance criteria at 20 jig/l
Compound
Carbon tetrachloride
Chlorobenzene
Chloroethane
Chloromethane
Trans-1 .2-dlchloroethene
Initial precision and accuracy
section 8.2.3
sftig/lj
90
82
70
25.0
6.9
8.2
14.8
360
79
26.0
79
67
, 77
11.7
7.4
Xftigrt.)
Labeled
compound On-going
recovery accuracy
sec. 8. 3 and sec. 11.5
14.2
P (percent)
Note 1
Note 2
Note 2
13.0-28.2 ns-196
6.5-31.5 ns-199
7.4-35.1 ns-214
d-54.3 ns-414
15.9-24.8 42-165
14.2-29.6 ns-205
2.1-46.7 ns-308
d-69.8 ns-554
11.6-26.3 18-172
d-55.5 ns-410
11.2-29.1 16-185
11.4-31.4 23-191
11.6-30.1 12-192
d-49.8 ns-315
10,5-31.5 15-195
R ftig/L)
4-33
4-34
6-36
d-61
12-30
4-35
d-51
d-79
8-30
d-64
8-32
9-33
8-33
d-S2
8-34
293
-------
Pt. 136, App. A, Math. 1624
40 CFR Ch. I (7-1-04 Edition)
TABLE 5—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS—Continued
Acceptance criteria at 20 ^ig/L
Compound
Gis-1 ,3-dichioropropene ..............„,.„...,.....,..,.,..
Dlelhyl ether ,.,.....,...,...,.,„.,...,„..„.„.,„.,.....,....,„..
1,1,2,2-tetrachlaroethane ,.,.,.,.,.,.-„.,.. ,.,.,...,.,.
Toluene « . ... ,. .... .
1,1,2-trichlQroethane ..,„,.„...,.,.,..„„...„.. ,...,..„,„..
Vinyl chloride ,...........,„„..„..........,,..,.....
Labeled
Initial precision and accuracy cSJpou",t3
***» 8.2.3 si If 2nd
14.2
s (ng/L)
... . ., 192
22.1
145
96
9,7
9.6
6.6
63
59
7.1
. 8,9
27.9
X(H9/L)
d-46.8
d-51 .0
d-40.2
Motel
Note 1
15.6-28.5
CM9.8
Notel
10.7-30.0
15.1-28.5
14.5-28.7
10.5-33.4
11.8-29.7
16.6-29.5
d-58.5
P (percent)
ns-343
ns-381
ns-284
ns-203
ns-316
5-199
31-181
4-193
12-200
21-184
35-196
ns-452
On-going
accuracy
sec. 11.5
R(ng/L)
d-51
d-56
d-44
5-35
d-50
7-34
11-32
6-33
8-35
9-32
12-34
d-65
d = detected; result must be greater than zero.
ns = no specification; limit would be below detection limit.
NOTE 1: Specifications not available for these compounds at time of release of this method.
NOTE 2: Specifications not developed for these compounds; use method 603.
294
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1624
FIGURE 1 Purging Device.
FIGURE 3 Schematic of Purge and Trap
Device—Purge Mode.
-t»»»aAi
FIGURE 2 Trap Packings and Construction to
Include Oesorb Capability.
FIGURE A Schematic of Purge and Trap
Device—Desorb Mode.
295
-------
M. 136, App. A, Meth. 1625
40 CFR Ch. I (7-1-04 Edfflon)
> 1-0
t~
2 10 20 SO 100 200
CONCENTRATION fciflrt.}
TOLUWIS-D,
*
• * »
* *
ANALYSIS NUMBER
l|
$0
«s
fcrfi
33
SP
'
0.90.
TOLUENE
» » *"" •
* « •
^
3s
6/1 8/1 8/1 9/1 B/2 8/2 ®3 B/3 6i4 S/S
DATE ANALYZES
FIQUHE 5 HelativB Hasponse Calibration Curve
for Toluene. The Dotted Lines Enclose a ±10
Percent Error Window.
FIGURE 7 Quality Control Charts Showing Area
(lop graph) and Relative Response of Toluene to
Toluene-d, (lower graph) Plotted as a Function of
Time or Analysis Number.
- M/Z 99
" M#Z §2
utlm , M868
M/Z 99 32508
FIGURE 6 Extracted Ion Current Profiles for
(A) Toluene, (B) Toluene-d,, and a Mixture of
ToluerJe arsd Toluene-d,.
METHOD 1625 RBVISION B—SBMIVOLATILE OE- additional compounds amenable to extrae-
GANIC COMPOUNDS BY ISOTOPE DILUTION GC/
MS
1, Scope and Application
1.1 This method is designed to determine
the semivolatile toxic organic pollutants as-
sociated with the 1976 Consent Decree and
tion and analysis by capillary column gms
chromatography-mass speotrometry (GC/
MS).
1.2 The chemical compounds listed in Ta-
bles 1 and 2 may be determined in municipal
and industrial discharges by this method.
The method is designed to meet the survey
296
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Environmental Protection Agency
Pt, 136, App. A, Mefh. 1625
requirements of Effluent Guidelines Division
(EGD) and the National Pollutants Dis-
charge Elimination System (NPDES) under
40 CPR 136.1. Any modifications of this meth-
od, beyond those expressly permitted, shall
be considered as major modifications subject
to application and approval of alternate test
procedures under 40 CPE 136.4 and 136.5.
1.3 The detection limit of this method is
usually dependent on the level of inter-
ferences rather than instrumental limita-
tions. The limits listed in Tables 3 and 4 rep-
resent the minimum quantity that can be de-
tected with no interferences present.
1.4 The GC/MS portions of this method
are for use only by analysts experienced with
GC/MS or under the close supervision of such
qualified persons. Laboratories unfamiliar
with analyses of environmental samples by
GC/MS should run the performance tests in
reference 1 before beginning.
2. Summary of Method
2.1 Stable isotopically labeled analogs of
the compounds of interest are added to a one
liter wastewater sample. The sample is ex-
tracted at pH 12-13, then at pH <2 with meth-
ylene chloride using continuous extraction
techniques. The extract is dried over sodium
sulfate and concentrated to a volume of one
mL. An Internal standard is added to the ex-
tract, and the extract is injected into the gas
chromatograph (GO. The compounds are
separated by GC and detected by a mass
spectrometer (MS). The labeled compounds
serve to correct the variability of the analyt-
ical technique.
2.2 Identification of a compound (quali-
tative analysis) is performed by comparing
the GC retention time and background cor-
rected characteristic spectral masses with
those of authentic standards.
2.3 Quantitative analysis is performed by
GC/MS using extracted ion current profile
(BICP) areas. Isotope dilution is used when
labeled compounds are available: otherwise,
an internal standard method is used.
2.4 Quality is assured through reproduc-
ible calibration and testing of the extraction
and GC/MS systems.
3. Contamination and Interferences
3.1 Solvents, reagents, glassware, and
other sample processing hardware may yield
artifacts and'or elevated baselines causing
misinterpretation of chromatograms and
spectra. All materials shall be demonstrated
to be free from interferences under the con-
ditions of analysis by running method blanks
initially and with each sample lot (samples
started through the extraction process on a
given 8 hr shift, to a maximum of 20). Spe-
cific selection of reagents and purification of
solvents by distillation in all-glass systems
may be required. Glassware and, where pos-
sible, reagents are cleaned by solvent rinse
and baking at 450 °C for one hour minimum.
3.2 Interferences coextracted from sam-
ples will vary considerably from source to
source, depending on the diversity of the in-
dustrial complex or municipality being sam-
ples.
4. Safety
4.1 The toxicity or carcinogenicity of
each compound or reagent used in this meth-
od has not been precisely determined; how-
ever, each chemical compound should be
treated as a potential health hazard. Expo-
sure to these compounds should be reduced
to the lowest possible level. The laboratory
is responsible for maintaining a current
awareness file of OSHA regulations regard-
ing the safe handling of the chemicals speci-
fied in this method. A reference file of data
handling sheets should also be made avail-
able to all personnel involved in these anal-
yses. Additional information on laboratory
safety can be found in references 2-t.
4.2 The following compounds covered by
this method have been tentatively classified
as known or suspected human or mammalian
carcinogens: benzidine benzo(a)anthracene,
3,3'-dichlorobenzidine, benzo(a)pyrene, diben-
zo(a,h)anthracene, N-nitrosodimethylamine,
and jj-naphtylamine. Primary standards of
these compounds shall be prepared in a hood,
and a NIOSH/MESA approved toxic gas res-
pirator should be worn when high concentra-
tions are handled.
5. Apparatus and Materials
5.1 Sampling equipment for discrete or
composite sampling,
5.1.1 Sample bottle, amber glass, 1.1 liters
minimum. If amber bottles are not available,
samples shall be protected from light. Bot-
tles are detergent water washed, then sol-
vent rinsed or baked at 450 °C for one hour
minimum before use.
5.1.2 Bottle caps—threaded to fit sample
bottles. Caps are lined with Teflon. Alu-
minum foil may be substituted if the sample
is not corrosive. Liners are detergent water
washed, then reagent water (Section 6.5} and
solvent rinsed, and baked at approximately
200 °C for one hour minimum before use.
5.1.3 Compositing equipment—automatic
or manual compositing system incorporating
glass containers for collection of a minimum
1.1 liters. Sample containers are kept at 0 to
4 °C during sampling. Glass or Teflon tubing
only shall be used. If the sampler uses a peri-
staltic pump, a minimum length of com-
pressible silicone rubber tubing may be used
in the pump only. Before use, the tubing is
thoroughly rinsed with methanol, followed
by repeated rinsings with reagent water
(Section 6.5) to minimize sample contamina-
tion. An integrating flow meter is used to
collect proportional composite samples.
297
-------
Pt. 136, App. A, Meth. 1625
40 CFR Ch, i (7-1-04 Edition)
5.2 Continuous liquid-liquid extractor—
Teflon or glass conneecting joints and stop-
cooks without lubrication (Hershberg-Wolf
Extractor) one liter capacity, Ace Glass 6841-
10, or equivalent.
5.3 Drying column—15 to 20 mm i.d, Pyrex
chromatographic column equipped with
coarse glass frit or glass wool plug.
5,4 Kuderna-Danish (K-D) apparatus
5.4.1 Concentrator tube—lOmL, graduated
(Kontes K-570Q50-1025, or equivalent) with
calibration verified. Ground glass stopper
(size 19/22 joint) is used to prevent evapo-
ration of extracts.
5.4.2 Evaporation flask—500 mL {Kontes
K-57QOQ1-Q500, or equivalent), attached to
concentrator tube with springs (Kontes K-
662750-0012).
5.4.3 Snyder column—three ball macro
(Kontes K-503000-0232, or equivalent).
5.4.4 Snyder column—two ball micro
(Kontes K-469002-0219, or equivalent).
5.4.5 Boiling chips—approx 10/40 mesh, ex-
tracted with methylene chloride and baked
at 450 °C for one hr minimum.
5.5 Water bath—heated, with concentric
ring cover, capable of temperature control ±2
"C, installed in a fume hood.
5.6 Sample vials—amber glass, 2-5 mL
with Teflon-lined screw cap.
5.7 Analytical balance—capable of weigh-
ing 0.1 mgr.
5.8 Gas chromatograph—shall have
splitless or on-column injection port for
capillary column, temperature program with
30 °C hold, and shall meet all of the perform-
ance specifications in Section 12.
5.8.1 Column—30±5 mx0.25±0.02 mm i.d. 5%
phenyl, 94% methyl, 1% vinyl silicone bond-
ed phase fused silica capillary column (J Sc W
DB-5, or equivalent).
5.9 Mass spectrometer—70 eV electron im-
pact ionization, shall repetitively scan from
35 to 450 amu in 0.95 to 1.00 second, and shall
produce a unit resolution (valleys between
m/z 441—442 less than 10 percent of the height
of the 441 peak), backgound corrected mass
spectrum from 50 ng decafluorotri-
phenylphosphine (DFTPP) introduced
through the GO inlet. The spectrum shall
meet the mass-intensity criteria in Table 5
(reference 5). The mass spectrometer shall be
interfaced to the GC such that the end of the
capillary column terminates within one cen-
timeter of the ion source but does not inter-
cept the electron or ion beams. All portions
of the column which connect the GC to the
ion source shall remain at or above the col-
umn temperature during analysis to preclude
condensation of less volatile compounds.
5.10 Data system—shall collect and record
MS data, store mass-intensity data in spec-
tral libraries, process GC/MS data, generate
reports, and shall compute and record re-
sponse factors.
5.10.1 Data acquisition—mass spectra
shall be collected continuously throughout
the analysis and stored on a mass storage de-
vice.
5.10.2 Mass spectral libraries—user cre-
ated libraries containing mass spectra ob-
tained from analysis of authentic standards
shall be employed to reverse search GC/MS
runs for the compounds of interest (Section
7.2).
5.10.3 Data processing—the data system
shall be used to search, locate, identify, and
quantify the compounds of Interest in each
GC/MS analysis. Software routines shall be
employed to compute retention times and
peak areas. Displays of spectra, mass
chromatograms, and library comparisons are
required to verify results.
5.10.4 Response factors and multipoint
calibrations—the data system shall be used
to record and maintain lists of response fac-
tors (response ratios for isotope dilution) and
multipoint calibration curves (Section 7).
Computations of relative standard deviation
(coefficient of variation) are useful for test-
ing calibration linearity. Statistics on ini-
tial (Section 8.2) and on-going (Section 12.7)
performance shall be computed and main-
tained.
6. Reagents and Standards
6.1 Sodium hydroxide—reagent grade, 6N
in reagent water.
6.2 Sulfuric acid—reagent grade, 6N in re-
agent water.
6.3 Sodium sulfate—reagent grade, granu-
lar anhydrous, rinsed with methylene chlo-
ride {20 mL/g) and conditioned at 450 °C for
one hour minimum.
6.4 Methylene chloride—distilled in glass
(Bnrdick and Jackson, or equivalent).
6.5 Reagent water—water in which the
compounds of Interest and interfering com-
pounds are not detected by this method.
6.6 Standard solutions—purchased as so-
lutions or mixtures with certification to
their purity, concentration, and authen-
ticity, or prepared from materials of known
purity and composition. If compound purity
is 96 percent or greater, the weight may be
used without correction to compute the con-
centration of the standard. When not being
used, standards are stored in the dark at — 20
to -10 °C in screw-capped vials with Teflon-
lined lids. A mark is placed on the vial at the
level of the solution so that solvent evapo-
ration loss can be detected. The vials are
brought to room temperature prior to use.
Any precipitate is redissolved and solvent is
added if solvent loss has occurred.
6.7 Preparation of stock solutions—pre-
pare in methylene chloride, benzene, p-
dioxane, or a mixture of these solvents per
the steps below. Observe the safety pre-
cautions in Section 4. The large number of
labeled and unlabeled acid, base/neutral, and
Appendix C compounds used for combined
calibration (Section 7) and calibration
verification (12.5) require high
298
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1625
coneentratimns (approx 40 mg/mL) when in-
dividual stock solutions are prepared, BO
that dilutions of mixtures will permit cali-
bration with all compounds in a single set of
solutions. The working range for most com-
pounds is 10-200 |ig/mL, Compounds with a re-
duced MS response may be prepared at high-
er concentrations.
6.7,1 Dissolve an appropriate amount of
assayed reference material in a suitable sol-
vent. For example, weigh 400 mg naphthalene
in a 10 mL ground glass stoppered volumetric
flask and fill to the mark with benzene.
After the naphthalene is completely dis-
solved, transfer the solution to a 15 mL vial
with Teflon-lined cap.
6.7.2 Stock standard solutions should be
checked for signs of degradation prior to the
preparation of calibration or performance
test standards. Quality control check sam-
ples that can be used to determine the accu-
racy of calibration standards are available
from the US Environmental Protection
Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio 45268.
6.7.3 Stock standard solutions shall be re-
placed after six months, or sooner if com-
parison with quality control check samples
indicates a change in concentration.
6.8 Labeled compound spiking solution—
from stock standard solutions prepared as
above, or from mixtures, prepare the spiking
solution at a concentration of 200 ^.g/mL, or
at a concentration appropriate to the MS re-
sponse of each compound.
6.9 Secondary standard—using stock solu-
tions (Section 6.7), prepare a secondary
standard containing all of the compounds in
Tables 1 and 2 at a concentration of 400 jig/
mL, or higher concentration appropriate to
the MS response of the compound.
6.10 Internal standard solution—prepare
2,2'-difluorobiphenyl (DFB) at a concentra-
tion of 10 mg/mL in benzene.
6.11 DFTPP solution—prepare at 50 (jg/mL
in acetone.
6.12 Solutions for obtaining authentic
mass spectra (Section 7.2)—prepare mixtures
of compounds at concentrations which will
assure authentic spectra are obtained for
storage in libraries.
6.13 Calibration solutions—combine 0.5
mL of the solution in Section 6.8 with 25, 50,
125, 250, and 500 uL of the solution in section
6.9 and bring to 1.00 mL total volume each.
This will produce calibration solutions of
nominal 10, 20, 50, 100, and 200 ng/mL of the
pollutants and a constant nominal 100 jig/mL
of the labeled compounds. Spike each solu-
tion with 10 (iL of the internal standard solu-
tion (Section 6.10). These solutions permit
the relative response (labeled to unlabeled)
to be measured as a function of concentra-
tion (Section 7.4).
6.14 Precision and recovery standard-
used for determination of initial (Section 8.2)
and on-going (Section 12.7) precision and re-
covery, This solution shall contain the pol-
lutants and labeled compounds at a nominal
concentration of 100 ug/mL.
6.15 Stability of solutions—all standard
solutions (Sections 6.8-6.14) shall be analyzed
within 48 hours of preparation and on a
monthly basis thereafter for signs of deg-
radation, Standards will remain acceptable
if the peak area at the quantitation mass
relative to the DFB internal standard re-
mains within ±15 percent of the area ob-
tained in the initial analysis of the standard.
7. Calibration
7.1 Assemble the GC/MS and establish the
operating conditions in Table 3. Analyze
standards per the procedure in Section 11 to
demonstrate that the analytical system
meets the detection limits in Tables 3 and 4,
and the mass-intensity criteria in Table 5 for
50 ng DFTPP.
7.2 Mass spectral libraries—detection and
identification of compounds of interest are
dependent upon spectra stored in user cre-
ated libraries.
7.2.1 Obtain a mass spectrum of each pol-
lutant, labeled compound, and the internal
standard by analyzing an authentic standard
either singly or as part of a mixture in which
there is no interference between closely
eluted components. That only a single com-
pound is present is determined by examina-
tion of the spectrum. Fragments not attrib-
utable to the compound under study indicate
the presence of an interfering compound.
7.2.2 Adjust the analytical conditions and
scan rate (for this test only) to produce an
undistorted spectrum at the GC peak max-
imum. An undistorted spectrum will usually
be obtained if five complete spectra are col-
lected across the upper half of the GC peak.
Software algorithms designed to "enhance"
the spectrum may eliminate distortion, but
may also eliminate authentic masses or in-
troduce other distortion.
7.2.3 The authentic reference spectrum is
obtained under DFTPP tuning conditions
(Section 7,1 and Table 5) to normalize it to
spectra from other instruments.
7.2.4 The spectrum is edited by saving the
5 most intense mass spectral peaks and all
other mass spectral peaks greater than 10
percent of the base peak. This edited spec-
trum is stored for reverse search and for
compound confirmation.
7,3 Analytical range—demonstrate that 20
ng anthracene or phenanthrene produces an
area at m/z 178 approx one-tenth that re-
quired to exceed the linear range of the sys-
tem. The exact value must be determined by
experience for each instrument. It is used to
match the calibration range of the instru-
ment to the analytical range and detection
limits required, and to diagnose instrument
sensitivity problems (Section 15.4). The 20
ug/mL calibration standard (Section 6.13) can
be used to demonstrate this performance.
299
-------
Pt. 136, App. A, Meth. 1625
40 CFR Ch. I (7-1-04 Edition)
7.3.1 Polar compound detection—dem-
onstrate that unlabeled pentachlorophenol
and benzidine are detectable at the 50 jig/mL
level (per all criteria in Section 13). The 50
tig/mi, calibration standard (Section 8.13) can
be used to demonstrate this performance.
7.4 Calibration with isotope dilution—iso-
tope dilution is used wlien (1) labeled com-
pounds are available, (2) interferences do not
preclude its use, and (3) the quantitation
mass extracted ion current profile (EICP)
area for the compound is in the calibration
range. If any of these conditions preclude
isotope dilution, internal standard methods
(Section 7.5 or 7.6) are used.
7,4,1 A calibration curve encompassing
the concentration range is prepared for each
compound to be determined. The relative re-
sponse (pollutant to labeled) vs concentra-
tion in standard solutions is plotted or com-
puted using a linear regression. The example
in Figure 1 shows a calibration curve for phe-
nol using phenol-d5 as the isotopic diluent.
Also shown are the ± 10 percent error limits
(dotted lines). Relative Reponse (RR) is de-
termined according to the procedures de-
scribed below. A minimum of five data
points are employed for calibration.
7.4.2 The relative response of a pollutant
to its labeled analog is determined from iso-
tope ratio values computed from acquired
data. Three isotope ratios are used in this
process:
BX = the isotope ratio measured for the
pure pollutant.
Ry = the isotope ratio measured for the la-
beled compound.
Rm = the isotope ratio of an analytical
mixture of pollutant and labeled compounds.
The m/z's are selected such that Rx> By. If
Rm is not between 2Ry and 0.5RX, the method
does not apply and the sample is analyzed by
internal or external standard methods.
7.4.3 Capillary columns usually separate
the pollutant-labeled pair, with the labeled
compound eluted first (Figure 2). For this
case, Rx = [area mi/z]/l, at the retention time
of the pollutant (RTz). Ry = l/[area m2/z, at
the retention time of the labeled compound
RTi), Rm = [area at mi/z (at RT2)]/[area at
RTi)], as measured to the mixture of the pol-
lutant and labeled compounds (Figure 2), and
RR = RID-
7.4.4 Special precautions are taken when
the pollutant-labeled pair is not separated,
or when another, labeled compound with
interfering' spectral masses overlaps the pol-
lutant (a case which can occur with isomeric
compounds). In this case, it is necessary to
determine the respective contributions of
the pollutant and labeled compounds to the
respective EICP areas. If the peaks are sepa-
rated well enough to permit the data system
or operator to remove the contributions of
the compounds to each other, the equations
in Section 7.4.3 apply. This usually occurs
when the height of the valley between the
two GC peaks at the same m/z is less than 10
percent of the height of the shorter of the
two peaks. If significant GC and spectral
overlap occur, RR is computed using the fol-
lowing equation:
RR = (R , - Rm) (Rx + 1)/(R™ - Bx) (Ry + 1),
where Rx is measured as shown in Figure 3A,
Ry is measured as shown in Figure SB, and
Rra is measured as shown to Figure 3C. For
example, Rx = 46100/4780 = 9.644, R, = 2650/
43600 = 0.0608, R,a = 49200/48300 = 1.019. amd RR
= 1.114.
7.4.5 To calibrate the analytical system
by isotope dilution, analyze a 1.0 uL aliquot
of each of the calibration standards (Section
6.13) using the procedure in Section 11, Com-
pute the RR at each concentration.
7,4.6 Linearity—if the ratio of relative re-
sponse to concentration for any compound is
constant (less than 20 percent coefficient of
variation) over the 5 point calibration range,
and averaged relative response/concentration
ratio may be used for that compound; other-
wise, the complete calibration curve for that
compound shall be used over the 5 point cali-
bration range.
7.5 Calibration by internal standard—used
when criteria for istope dilution (Section 7.4)
cannot be met. The internal standard to be
used for both acid and base/neutral analyses
is 2,2'-difluorobiphenyl. The internal stand-
ard method is also applied to determination
of compounds having no labeled analog, and
to measurement of labeled compounds for
mtra-laboratory statistics (Sections 8.4 and
12.7.4).
7.5.1 Response factors—calibration re-
quires the determination of response factors
(RF) which are defined by the following
equation:
RF = (As x C«)/(Ai5 x C,), where
A, is the area of the characteristic mass for
the compmund in the daily standard
AIS is the area of the characteristic mass
for the internal standard
CiS is the concentration of the internal
standard (ng/mL)
C, is the concentration of the compound in
the daily standard (ng/mL)
7.5.1.1 The response factor is determined
for at least five concentrations appropriate
to the response of each compound (Section
6.13); nominally, 10, 20, 50, 100, and 200 ng/mL,
The amount of internal standard added to
each extract is the same (100 ng/mL) so that
C/u remains constant. The RF is plotted vs
concentration for each compound in the
standard ,(C«) to produce a calibration curve.
7.5.1.2 Linearity—if the response factor
(RF) for any compound is constant (less than
35 percent coefficient of variation) over the 5
point calibration range, an averaged re-
sponse factor may be used for that com-
pound; otherwise, the complete calibration
300
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Environmental Protection Agency
Ph 136, App. A, Meth. 1625
curve for that compound shall be used over
the 5 point range.
7.6 Combined calibration—by using cali-
bration solutions (Section 6,13) containing
the pollutants, labeled compounds, and the
internal standard, a single set of analyses
can be used to produce calibration curves for
the isotope dilution and internal standard
methods. These curves are verified each shift
(Section 12.5) by analyzing the 100 ng/mL
calibration standard (Section 6.13). Re-
calibration is required only if calibration
verification (Section 12.5) criteria cannot be
met.
S. Quality Assurance/Quality Control
8.1 Each laboratory that uses this method
is required to operate a formal quality assur-
ance program. The minimum requirements
of this program consist of an initial dem-
onstration of laboratory capability, analysis
of samples spiked with labeled compounds to
evaluate and document data quality, and
analysis of standards and blanks as tests of
continued performance. Laboratory perform-
ance is compared to established performance
criteria to determine if the results of anal-
yses meet the performance characteristics of
the method.
8.1.1 Tie analyst shall make an initial
demonstration of the ability to generate ac-
ceptable accuracy and precision with this
method. This ability is established as de-
scribed in Section 8.2.
8.1.2 The analyst is permitted to modify
this method to improve separations or lower
the costs of measurements, provided all per-
formance specifications are met. Each time a
modification is made to the method, the ana-
lyst is required to repeat the procedure in
Section 8.2 to demonstrate method perform-
ance.
8.1.3 Analyses of blanks are required to
demonstrate freedom from contamination.
The procedures and criteria for analysis of a
blank are described In Section 8.5.
8.1.4 The laboratory snail spike all sam-
ples with labeled compounds to monitor
method performance. This test is described
in Section 8.3. When results of these spikes
indicate atypical method performance for
samples, the samples are diluted to bring
method performance within acceptable lim-
its (Section 15).
8.1.5 The laboratory shall, on an on-going
basis, demonstrate through calibration
verification and the analysis of the precision
and recovery standard (Section 6,14) that the
analysis system is in control. These proce-
dures are described in Sections 12.1, 12.5, and
12.7.
8.1.6 The laboratory shall maintain
records to define the quality of data that is
generated. Development of accuracy state-
ments is described in Section 8.4.
8.2 Initial precisloa and accuracy—to es-
tablish the ability to generate acceptable
precision and accuracy, the analyst shall
perform the following operations:
8.2.1 Extract, concentrate, and analyze
two sets of four one-liter aliquots (8 aliquots
total) of the precision and recovery standard
(Section 6.14) according to the procedure in
Section 10.
8,2.2 Using results of the first set of four
analyses, compute the average recovery (X)
in p.g/mli and the standard deviation of the
recovery (s) in 8g/nL for each compound, by
isotope dilution for pollutants with a labeled
analog, and by internal standard for labeled
compounds and pollutants with no labeled
analog".
8,2.3 For each compound, compare s and X
with the corresponding limits for initial pre-
cision and accuracy in Table 8. If s and X for
all compounds meet the acceptance criteria,
system performance is acceptable and anal-
ysis of blanks and samples may begin. If,
however, any individual s exceeds the preci-
sion limit or any individual X falls outside
the range for accuracy, system performance
is unacceptable for that compound.
NOTE: The large number of compounds in
Table 8 present a substantial probability
that one or more will fail the acceptance cri-
teria when all compounds are analyzed. To
determine if the analytical system is out of
control, or If the failure can be attributed to
probability, proceed as follows:
8.2.4 Using the results of the se_cond set of
four analyses, compute s and X for only
those compounds which failed the test of the
first set of four analyses (Section 8.2.3). If
these compounds now pass, system perform-
ance Is acceptable for all compounds and
analysis of blanks and samples may begin. If,
however, any of the same compoulds fail
again, the analysis system Is not performing
properly for these compounds. In this event,
correct the problem and repeat the entire
test (Section 8.2,1).
8,3 The laboratory shall spike all samples
with labeled compounds to assess method
performance on the sample matrix.
8.3.1 Analyze each sample according to
the method in Section 10.
8.3,2 Compute the percent recovery (P) of
the labeled compounds using the internal
standard methmd (Section 7.5).
8.3.3 Compare the labeled compound re-
covery for each compound with the cor-
responding limits in Table 8. If the recovery
of any compounds falls outside its warning
limit, method performance Is unacceptable
for that compound in that sample, Therefore,
the sample is complex and is to be diluted
and reanalyzed per Section 15.4.
8.4 As part of the QA program for the lab-
oratory, method accuracy for waste water
samples shall be assessed and records shall
be maintained. After the analysis of five
wastewater samples for which the labeled
compounds pass the tests in Section 8.3,
compute the average percent recovery (P)
301
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Pt. 136, App. A, Math, 1625
40 CFR Ch. I (7-1-04 Edition)
and the standard deviation of the percent re-
covery (Sp) for the labeled compounds only.
Express the accuracy assessment as a per-
cent recovery interval from P — 2 ,p to P+2sp.
For example, if P=90% and %=10%, the accu-
racy interval is expressed as 70-100%. Update
the accuracy assessment for each compound
on a regular basis (e.g. after each 5-10 new
accuracy measurements).
8.5 Blanks — reagent water blanks are ana-
lyzed to demonstrate freedom from contami-
nation.
8.5.1 Extract and concentrate a blank
with each sample lot (samples started
through the extraction process on the same
8 hr shift, to a maximum of 20 samples). Ana-
lyze the blank immediately after analysis of
the precision and recovery standard (Section
6.14) to demonstrate freedom from contami-
nation,
8.5,2 If any of the compounds of interest
(Tables 1 and 2) or any potentially inter-
fering compound is found in a blank at great-
er than 10 (tg/L (assuming a response factor
of 1 relative to the internal standard for
compounds not listed in Tables 1 and 2),
analysis of samples is halted until the source
of contamination is eliminated and a blank
shows no evidence of contamination at this
level.
8.6 The specifications contained in this
method can be met if the apparatus used is
calibrated properly, then maintained in a
calibrated state. The standards used for cali-
bration (Section 7), calibration verification
(Section 12.5), and for initial (Section 8.2)
and on-going (Section 12.7) precision and re-
covery should be identical, so that the most
precise results will be obtained. The GO/MS
instrument in particular will provide the
most reproducible results if dedicated to the
settings and conditions required for the anal-
ysis of semi-volatiles by this method.
8.7 Depending on specific program re-
quirements, field replicates may be collected
to determine the precision of the sampling
technique, and spiked samples may be re-
quired to determine the accuracy of the
analysis when internal or external standard
methods are. used.
9.
Sample Collection, Preservation, and
Handling
9.1 Collect samples in glass containers
following conventional sampling practices
(Reference 7). Composite samples are col-
lected in refrigerated glass containers (Sec-
tion 5.1.3) in accordance with the require-
ments of the sampling program.
9.2 Maintain samples at 0-4 °C from the
time collectimn until extraction. If residual
chlorine is present, add 80 mg sodium
thiosulfate per liter of water, EPA Methods
330.4 and 830.5 may be used to measure resid-
ual chlorine (Reference 8).
9.3 Begin sample extraction within seven
days of collection, and analyze all extracts
within 40 days of extraction,
10. Sample Extraction and Concentration (See
Figure 4)
10,1 Labeled compound spiking—measure
1.00 ± 0.01 liter of sample into a glass con-
tainer. For untreated effluents, and samples
which are expected to be difficult to extract
and/or concentrate, measure an additional
10.0 ± 0.1 mL and dilute to a final volume of
1.00 ± 0.01 liter with reagent water in a glass
container.
10.1.1 For each sample or sample lot (to a
maximum of 20) to be extracted at the same
time, place three 1.00 ± 0,10 liter aliquots of
reagent water in glass containers.
10.1.2 Spike 0.5 mL of the labeled com-
pound spiking solution (Section 6.8) into all
samples and one reagant water aliquot.
10.1.3 Spike 1.0 mL of the precision and
recovery standard (Section 6.14) into the two
remaining reagent water aliquots.
10,1,4 Stir and equilibrate all solutions for
1-2 hr.
10.2 Base/neutral extraction—place 100-150
mL methylene chloride in each continuous
extractor and 200-300 in each distilling flask,
10.2.1 Pour the sample(s), blank, and
standard aliquots into the extractors. Rinse
the glass containers with 50-100 mL meth-
ylene chloride and add to the respective ex-
tractor,
10.2.2 Adjust the pH of the waters in the
extractors to 12-13 with 6N NaOH while mon-
itoring with a pH meter. Begin the extrac-
tion by heating the flask until the meth-
ylene chloride is boiling. When properly ad-
justed, 1-2 drops of methylene chloride per
second will fall from the condenser tip into
the water. After 1-2 hours of extraction, test
the pH and readjust to 12-13 if required. Ex-
tract for 18-24 hours.
10,2.3 Remove the distilling flask, esti-
mate and record the volume of extract (to
the nearest 100 mL), and pour the contents
through a drying column containing 7 to 10
cm anhydrous sodium sulfate. Rinse the dis-
tilling flask with 30-50 mL of methylene
chloride and pour through the drying col-
umn. Collect the solution in a 500 mL K-D
evaporator flask equipped with a 10 mL con-
centrator tube. Seal, label as the base/neu-
tral fraction, and concentrate per Sections
10.4 to 10.5.
10.3 Acid extraction—adjust the pH of the
waters in the extractors to 2 or less using 6N
sulfuric acid. Charge clean distilling flasks
with 300-400 mL of methylene chloride. Test
and adjust the pH of the waters after the
first 1-2 hr of extraction. Extract for 18-24
hours.
10.3,1 Repeat Section 10.2.3, except label
as the acid fraction.
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Environmental Protection Agency
Pt. 136,App. A, Meth. 1625
10.4 Concentration—concentrate the ex-
tracts in separate 500 mL K-D flasks
equipped with 10 mL concentrator tubes.
10.4.1 Add 1 to 2 clean boiling chips to the
flask and attach a three-ball macro Snyder
column. Prewet the column by adding ap-
proximately one mL of methylene chloride
through the top. Place the K-D apparatus in
a hot water bath so that the entire lower
rounded surface of the flask is bathed with
steam. Adjust the vertical position of the ap-
paratus and the water temperature as re-
quired to complete the concentration in 15 to
20 minutes. At the proper rate of distillation,
the balls of the column will actively chatter
but the chambers will not flood. When the
liquid has reached an apparent volume of 1
mL, remove the K-D apparatus from the
bath and allow the solvent to drain and cool
for at least 10 minutes. Remove the Snyder
column and rinse the flask and its lower
joint into the concentrator tube with 1-2 mL
of methylene chloride. A 5-mL syringe is rec-
ommended for this operation.
10.4.2 For performance standards (Sec-
tions 8.2 and 12.7} and for blanks (Section
8.5), combine the acid and base/neutral ex-
tracts for each at this point. Do not combine
the acid and base/neutral extracts for sam-
ples.
10,5 Add a clean boiling chip and attach a
two ball micro Snyder column to the concen-
trator tube. Prewet the column by adding
approx 0.5 mL methylene chloride through
the top. Place the apparatus in the hot water
bath. Adjust the vertical position and the
water temperature as required to complete
the concentration in 5-10 minutes. At the
proper rate of distillation, the balls of the
column will actively chatter but the cham-
bers will not flood. When the liquid reaches
an apparent volume of approx 0.5 mL, re-
move the apparatus from the water bath and
allow to drain and cool for at least 10 min-
utes. Remove the micro Snyder column and
rinse its lower joint into the concentrator
tube with approx 0.2 mL of methylene chlo-
ride. Adjust the final volume to 1.0 mL.
10.6 Transfer the concentrated extract to
a clean screw-cap vial. Seal the vial with a
Teflon-lined lid, and mark the level on the
vial. Label with the sample number and frac-
tion, and store In the dark at — 20 to —10 "0
until ready for analysis.
11. GC/MS Analysis
11.1 Establish the operating- conditions
given in Table 3 or 4 for analysis of the base/
neutral or acid extracts, respectively. For
analysis of combined extracts (Section
10.4.2), use the operating conditions In Table
3.
11.2 Bring the concentrated extract (Sec-
tion 10.6) or standard (Sections 6,13 through
6.14) to room temperature and verify that
any precipitate has redissolved. Verify the
level on the extract (Sections 6.6 and 10.6)
and bring to the mark with solvent if re-
quired.
11,3 Add the internal standard solution
(Section 6.10) to the extract (use 1.0 uL of so-
lution per 0.1 mL of extract) immediately
prior to injection to minimize the possibility
of loss by evaporation, adsorption, or reac-
tion. Mix thoroughly.
11.4 Inject a volume of the standard solu-
tion or extract such that 100 ng of the inter-
nal standard will be injected, using on-col-
umn or splitless injection. For 1 mL ex-
tracts, this volume will be 1.0 uL. Start the
GO column Initial isothermal hold upon in-
jection. Start MS data collection after the
solvent peak elutes. Stop data collection
after the benzo (ghi) perylene or
pentachlorophenol peak elutes for the base/
neutral or acid fraction, respectively, Beturn
the column to the initial temperature for
analysis of the next sample.
12, System and Laboratory Performance
12.1 At the beginning of each 8 hr shift
during which analyses are performed, Q-O/MS
system performance and calibration are
verified for all pollutants and labeled com-
pounds. For these tests, analysis of the 100
Hg'/mL calibration standard (Section 6.13)
shall be used to verify all performance cri-
teria. Adjustment and/or recalibration (per
Section 7) shall be performed until all per-
formance criteria are met. Only after all per-
formance criteria are met may samples,
blanks, and precision and recovery standards
be analyzed,
12.2 DFTPP spectrum validity—inject 1
UL of the DFTPP solution (Section 6.11) ei-
ther separately or within a few seconds of in-
jection of the standard (Section 12.1) ana-
lyzed at the beginning of each shift. The cri-
teria in Table 5 shall be met.
12,3 Retention times—the absolute reten-
tion time of 2,2'-difluorobiphenyl shall be
within the range of 1078 to 1248 seconds and
the relative retention times of all pollutants
and labeled compounds shall fall within the
limits given in Tables 3 and 4.
12.4 GC resolution—the valley height be-
tween anthracene and phenanthrene at m/z
178 (or the analogs at m/z 188) shall not ex-
ceed 10 percent of the taller of the two peaks,
12.5 Calibration verification—compute
the concentration of each pollutant (Tables 1
and 2) by isotope dilution (Section 7,4) for
those compounds which have labeled
analogs. Compute the concentration of each
pollutant which has no labeled analog by the
internal standard method (Section 7.5). Com-
pute the concentration of the labeled com-
pounds by the internal standard method.
These concentrations are computed based on
the calibration data determined in Section 7.
12.5.1 For each pollutant and labeled com-
pound being tested, compare the concentra-
tion with the calibration verification limit
303
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Pt. 136, App. A, Metti. 1625
40 CFR Ch. I (7-1-04 Idition)
in Table 8. If all compounds meet the accept-
ance criteria, calibration has been verified
and analysis of Wanks, samples, and preci-
sion and recovery standards may proceed. If,
however, any compound falls, the measure-
ment system is not performing properly for
that compound. In this event, prepare a fresh
calibration standard or correct the problem
causing the failure and repeat the test (Sec-
tion 12.1), or recalibrate (Section 7).
12.6 Multiple peaks—each compound in-
jected shall give a single, distinct GO peak.
12.7 On-going precision and accuracy.
12.7.1 Analyze the extract of one of the
pair of precision and recovery standards
(Section 10.1.3) prior to analysis of samples
from the same lot.
12.7.2 Compute the concentration of each
pollutant (Tables 1 and 2) by isotope dilution
(Section 7.4) for those compounds which have
labeled analogs. Compute the concentration
of each pollutant which has no labeled ana-
log by the internal standard method (Section
7.5). Compute the concentration of the la-
beled compounds by the internal standard
method.
12.7.3 For each pollutant and labeled com-
pound, compare the concentration with the
limits for on-going accuracy in Table 8. K all
compounds meet the acceptance criteria,
system performance is acceptable and anal-
ysis of blanks and samples may proceed. If,
however, any individual concentration falls
outside of the range given, system perform-
ance Is unacceptable for that compound.
NOTE: The large number of compounds in
Table 8 present a substantial probability
that one or more will fail when all com-
pounds are analyzed. To determine if the ex-
traction/concentration system is out of con-
trol or if the failure is caused by probability,
proceed as follows:
12.7.3.1 Analyze the second aliquot of the
pair of precision and recovery standard (Sec-
tion 10.1.3).
12.7.3.2 Compute the concentration of
only those pollutants or labeled compounds
that failed the previous test (Section 12.7.3).
If these compounds now pass, the extraction/
concentration processes are in control and
analysis of blanks and samples may proceed.
If, however, any of the same compounds fail
again, the extraction/concentration proc-
esses are not being performed properly for
these compounds. In this event, correct the
problem, re-extract the sample lot (Section
10) and repeat the on-going precision and re-
covery test (Section 12.7).
12.7.4 Add results which pass the speci-
fications in Section 12,7.2 to Initial and pre-
vious on-going data. Update QC charts to
perform a graphic representation of contin-
ued laboratory performance (Figure 5). De-
velop a statement of laboratory accuracy for
each pollutant and labeled compound by cal-
culating the average percent recovery (R)
and the standard deviation of percent recov-
ery (ST). Express the accuracy as a recovery
interval from R-2s, to E+2s,. For example, if
R=95% and s,=5%, the accuracy is 86-105%.
13, Qualitative Determination
13.1 Quantitative determination is ac-
complished by comparison of data from anal-
ysis of a sample or blank with data from
analysis of the shift standard (Section 12.1)
and with data stored in the spectral libraries
(Section 7.2.4). Identification is confirmed
wnen spectra and retention times agree per
the criteria below.
13.2 Labeled compounds and pollutants
having no labeled analog:
13.2.1 The signals for all characteristic
masses stored in the spectral library (Sec-
tion 7.2.4) shall be present and shall maxi-
mize within the same two consecutive scans.
13.2.2 Either (1) the background corrected
EICP areas, or (2) the corrected relative in-
tensities of the mass spectral peaks at the
GC peak maximum shall agree within a fac-
tor of two (0.5 to 2 times) for all masses
stored in the library.
13.2.3 The retention time relative to the
nearest eluted internal standard shall be
within ±15 scans or ±15 seconds, whichever is
greater of this difference in the shift stand-
ard (Section 12.1).
13.3 Pollutants having a labled analog:
13.3.1 The signals for all characteristic
masses stored in the spectral library (Sec-
tion 7.2.4) shall be present and shall maxi-
mize within the same two consecutive scans.
13.3.2. Either (1) the background corrected
EICP areas, or (2) the corrected relative in-
tensities of the mass spectral peaks at the
GC peak maximum shall agree within a fac-
tor of two for all masses stored In the spec-
tral library.
13.3,3. The retention time difference be-
tween the pollutant and its labeled analog
shall agree within ± 6 scans or ± 6 seconds
(whichever is greater) of this difference in
the shift standard (Section 12.1).
13.4 Masses present in the experimental
mass spectrum that are not present in the
reference mass spectrum shall be accounted
for by contaminant or background ions. If
the experimental mass spectrum is contami-
nated, an experienced spectrometrist (Sec-
tion 1.4) is to-determine the presence or ab-
sence of the cmmpound.
14. Quantitative Determination
14.1 Isotope dilution—by adding a known
amount of a labeled compound to every sam-
ple prior to extraction, correction for recov-
ery of the pollutant can be made because the
pollutant and its labeled analog exhibit the
same effects upon extraction, concentration,
and gas chromatography. Relative response
(RB) values for mixtures are used in conjunc-
tion with calibration curses described in
304
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Environmental Protection Agency
Pt. 136, App. A, Meth. 1625
Section 7.4 to determine concentrations di-
rectly, so long as labeled compound spiking
levels are constant. For the phenml example
given in Figure 1 (Section 7.4,1), BB would be
equal to 1.114. For this RR value, the phenol
calibration curve given in Figure 1 indicates
a concentration of 27 (ig/mL in the sample ex-
tract (C«).
14.2 Internal standard—compute the con-
centration in the extract using the response
factor determined from calibration data
(Section 7.5) and the following equation:
CUQig/mLXA, x C|S/(A,S x RF) where Ce» is the
concentration of the compound in the ex-
tract, and the other terms are as defined in
Section 7.5.1.
14.3 The concentration of the pollutant in
water is computed using the volumes of the
original water sample (Section 10.1) and the
final extract volume (Section 10.5), as fol-
lows: Concentration in water (ng/L)=(C« x
Vex)/Vj where Vex is the extract volume in
mL, and Vs is the sample volume in liters.
14.4 If the EICP area at the quantitiation
mass for any compound exceeds the calibra-
tion range of the system, the extract of the
dilute aliquot (Section 10.1) is analyzed by
Isotope dilution; otherwise, the extract is di-
luted by a factor of 10, 9 gL of internal stand-
ard solution (Section 6.10) are added to a 1.0
mL aliquot, and this diluted extract is ana-
lyzed by the internal standard method (Sec-
tion 14.2). Quantify each compound at the
highest concentration level within the cali-
bration range.
14.5 Report results for all pollutants and
labeled compounds (Tables 1 and 2) found in
all standards, blanks, and samples in ng/L, to
three significant figures. Results for samples
which have been diluted are reported at the
least dilute level at which the area at the
quantitation mass is within the calibration
range (Section 14.4) and the labeled com-
pound recovery is within the normal range
for the method (Section 15.4).
IS. Analysis of Complex Samples
15.1 Untreated effluents and other sam-
ples frequently contain high levels (>1000 \igl
L) of the compounds of interest, interfering
compounds, and/or polymeric materials.
Some samples will not concentrate to one
mL (Section 10.5); others will overload the
QC column and/or mass spectrometer.
15.2 Analyze the dilute aliquot (Section
10,1) when the sample will not concentrate to
1.0 mL. If a dilute aliquot was not extracted,
and the sample holding time (Section 9.3) has
not been exceeded, dilute an aliquot of the
sample with reagent water and re-extract
(Section 10,1); otherwise, dilute the extract
(Section 14.4) and analyze by the internal
standard method (Section 14.2).
15.3 Recovery of internal standard— the
BICP area of the internal standard should be
within a factor of two of the area in the shift
standard (Section 12,1). If the absolute areas
of the labeled compounds are within a factor
of two of the respective areas in the shift
standard, and the internal standard area is
less than one-half of its respective area, then
internal standard loss in the extract has oc-
curred, In this case, use one of the labeled
compounds (perferably a polynuclear aro-
matic hydrocarbon) to compute the con-
centration of a pollutant with no labeled
analog.
15.4 Recovery of labeled compounds— in
most samples, labeled compound recoveries
will be similar to those from reagent water
(Section 12.7). If the labeled compound recov-
ery is outside the limits given in Table 8, the
dilute extract (Section 10,1) is analyzed as in
Section 14.4. If the recoveries of all labeled
compounds and the internal staldard are low
(per the criteria above), then a loss in instru-
ment sensitivity is the most likely cause. In
this case, the 100 ng/mL calibration standard
(Section 12.1) shall be analyzed and calibra-
tion verified (Section 12.5). If a loss in sensi-
tivity has occurred, the instrument shall be
repaired, the performance specifications in
Section 12 shall be met, and the extract re-
analyzed. If a loss in instrument sensitivity
has not occurred, the method does not work
on the sample being analyzed and the result
may not be reported for regulatory compli-
ance purposes.
16. Method Performance
16.1 Interlaboratory performance for this
method is detailed in references 9 and 10.
16.2 A chromatogram of the 100 ng/mL
acid/base/neutral calibration standard (Sec-
tion 6.13) is shown in Figure 6.
REFERENCES
1. "Performance Tests for the Evaluation of
Computerized Gas Chromatography/Mass
Spectrometry Equipment and Laboratories"
USEPA, EMSL/Cmeinnati, OH 45268, EPA-
600/4-80-025 (April 1980).
2. "Working- with Carcinogens," DHEW,
PHS, CDC, NIOSH, Publication 77-206, (Au-
gust 1977).
3, "OSHA Safety and Health Standards,
General Industry" OSHA 2208, 29 CFR part
1910 (January 1976).
4. "Safety in Academic Chemistry Labora-
tories, " ACS Committee on Chemical Safety
(1979).
5. "Reference Compound to Calibrate Ion
Abundance Measurement in Gas Chroma-
tography-Mass Spectrometry Systems," J.W.
Bichelberger. L.B. Harris, and W.L. Budde.
Anal. Chem., 47, 955 (1975).
6. "Handbook of Analytical Quality Control
in Water and Wastewater Laboratories,"
USEPA, EMSL/Cincinuati, OH 45268, EPA-
600/4-79-019 (March 1979).
7. "Standard Practice for Sampling Water,"
ASTM Annual Book of Standards, ASTM,
Philadelphia, PA, 76 (1980),
305
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Pt. 136, App. A, Meth. 1625
40 CFR Ch. I (7-1-04 Edition)
8. "Methods 330.4 and 330.5 for Total Resid-
ual Chlorine," USBPA, EMSL/ Cincinnati, OH
45268, EPA 600/4-70-020 (March 1979).
9. Colby, B.N., Beimer, E.G., Bushneek,
D.E., and Telliard, W.A., "Isotope Dilution
Gas Chromatography-Mass Spectrometry for
the determination of Priority Pollutants in
Industrial Effluents." USEPA, Effluent
Guidelines Division, Washington, DC 20460
(1980).
10. "Inter-laboratory Validation of US En-
vironmental Protection Agency Method
1625," USEPA, Effluent Guidelines Division,,
Washington, DC 20460 (June 15, 1984).
TABLE 1—BASE/NEUTRAL EXTRACTABLE COMPOUNDS
Compound
Bis(2-chlQroethyl) ether
Bis(2-ethy!hexyl) phihalate ...
4-bfomophenyl ptienyi ether
n-C14 (Appendix C)
n-C16 (Appendix C)
n-C18 (Appendix C)
n-C20 (Appendix C)
n-C22 (Appendix C) .. ....
Di-n-octyl phthalate
Diphenyl ether (Appendix G)
B-naphthylamine (Appendix C)
N-nitrosodiphenviamine
STORET
34205
34200
34220
39120
34526
34230
34242
34247
34S21
81513
34273
34278
34283
39100
34636
34292
77427
77588
77691
77757
77804
77830
77859
77886
77901
78116
78117
77571
34581
34641
34320
77356
34556
81302
77639
39110
34536
34566
34571
34631
34336
34606
34341
34611
34626
34598
77579
77587
34346
34376
34381
39700
34391
34396
34386
34403
34408
34696
82553
34447
34438
34428
34433
CAS reg-
istry
83-32-9
208-96-8
120-12-7
92-87-5
56-55-3
205-99-2
207-08-9
50-32-8
191-24-2
92-52-4
111-44-4
111-91-1
108-60-1
117-81-7
101-55-3
85-68-7
124-18-5
112-40-2
629-59-4
544_76-3
593-45-3
112-95-8
629-97-0
646-31-1
630-01-3
630-02—*
638-68-6
86-74-8
91-58-7
7005-72-3
218-01-9
99-87-6
53-70-3
132-64-9
132-65-0
84-74-2
95_50_1
541_73_1
106-46—7
91-94-1
84-66-2
105-67-9
131-11-3
121-14-2
606-20-2
1 1 7-84-0
122-39-4
101-84-8
122-66-7
206-44-0
86-73-7
1 1 8-74-1
87-68-3
67_72-1
77-47-4
193-39-5
78-59-1
91_20-3
91-59-8
98-95-3
62-75-9
621-64-7
86-30-3
EPA-
EGD
001 B
077 B
078 B
005 B
072 B
074 B
075 B
073 B
079 B
512 B
018 B
043 B
042 B
066 B
041 B
067 B
517 B
506B
518 B
519 B
520 B
521 B
522 B
523 B
524 B
525 B
526 B
528 B
020 B
040 B
076 B
513 B
082 B
505 B
504 B
068 B
025 B
026 B
027 B
028 B
070 B
034 A
071 B
035 B
036 B
069 B
507 B
508B
037 B
039 B
080 B
009 B
052 B
012 B
053 B
083 B
054 B
055 B
502 B
056 B
061 B
063 B
062 B
NPDES
001 B
002 B
003 B
004 B
005 B
007 B
009 B
006 B
008 B
011 B
010 B
012 B
013 B
014 B
015 B
016 B
017 B
018 B
019 B
026 B
020 B
021 B
022 B
023 B
024 B
003 A
025 B
027 B
028 B
029 B
030 B
031 B
032 B
033 B
034 B
036 B
035 B
037 B
038 B
039 B
040 B
041 B
042 B
043 B
306
-------
Environmental Protection Agency
Pt, 136, App. A, Meth, 1625
TABLE 1— BASE/NEUTRAL EXTRACTABLE COMPOUNDS—Continued
Compound
STORE!
34481
34694
77088
34469
77128
77493
77613
34551
CAS reg-
istry
85-01-8
108-95-2
109-06-69
129-00-0
100-42-5
98-55-5
87-81-6
120-82-1
EPA-
EGD
081 B
065 A
503 B
084 B
510 B
509 B
529 B
008 B
NPDES
044 B
010 A
045 B
046 B
TABLE 2—ACID EXTRACTABLE COMPOUNDS
Compound
STORET
34452
34586
34601
34616
34657
34591
34646
39032
77688
34621
CAS reg-
istry
59-50-7
95-57-8
120-63-2
51-29-5
534-52-1
88-75-5
100-02-7
87-86-5
93_37_55
95-95-4
88-06-2
EPA-
EGD
022 A
024 A
031 A
059 A
060 A
057 A
058 A
064 A
530 A
531 A
021 A
NPDES
008 A
001 A
002 A
005 A
004 A
006 A
007 A
009 A
011 A
TABLE 3—GAS CHROMATOQRAPHY OF BASE/NEUTRAL EXTRACTABLE COMPOUNDS
EGD
No.1
164
061
603
703
610
710
613
713
265
365
218
318
617
717
226
326
227
327
225
325
242
342
212
312
063
256
356
254
354
234
334
043
208
308
255
355
609
Compound
2)2i-difluorobiphenyl (int std)
bis(2-chloroethyl) ether-d8 -
1 ,3-dichtorobenzene .
1 ,4-dichiorobenzene
bis{2-chloroisopropyl) ether-d12
2,4-ditnethyl phenol-d3
1 ,2,4-trichlorobenzene
atoha-teroineol-ciS
Retention time
Mean
(sec)
1163
385
417
426
546
549
742
755
696
700
696
704
698
720
722
724
737
740
758
760
788
799
819
823
830
845
849
881
889
921
924
939
955
958
963
967
973
EGD
Ref
164
164
164
603
164
610
164
613
164
265
164
218
164
617
164
226
164
227
164
225
164
242
164
212
164
164
256
164
254
164
234
164
164
208
164
255
164
Relative
1.000-1.000
ns
0.326-0.393
1.006-1.028
0.450-0.488
1.002-1.009
0.624-0.652
1.008-1.023
0.584-0.613
0.995-1.010
0.584-0.607
1.007-1.016
0,585-0,615
1.022-1.038
0.605-0.636
0.998-1 .008
0.601-0.666
0.997-1 .009
0.632-0.667
0.995-1.008
0.664-0.691
1.010-1.016
0.690-0.717
0.999-1 ,001
ns
0.706-0.727
1.002-1.007
0.747-0.767
0.999-1.017
0.781-0.803
0999-1.003
ns
0.813-0.830
1 .000-1 .005
0.819-0.836
1.001-1.006
0.829-0.844
Detec-
tion
limit2
(H8/L)
10
50
50
50
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
20
10
10
10
10
10
10
10
10
10
10
10
10
307
-------
Pt. 136, App. A, Metti. 1625
CFR Ch. I (7-1-04 Edition)
TABLE 3—GAS CHRQMATOGRAPHY OF BASE/NEUTRAL EXTRACTABLE COMPOUNDS—Continued
E6D
No.1
709
606
706
529
252
352
253
353
220
320
518
612
712
608
708
277
377
271
371
236
336
201
301
605
705
602
702
280
380
240
340
270
370
619
719
23S
335
237
337
607
707
262
362
041
209
309
281
520
381
278
378
604
704
528
621
721
268
368
239
339
284
384
205
305
522
623
723
067
276
376
Compound
n-dodecane-
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1625
TABLE 3—GAS CHROMATOGRAPHY OF BASE/NEUTRAL EXTRACTABLE COMPOUNDS—Continued
EGD
Retention time
Detec-
tion
No-1
272
372
228
328
266
366
524
269
369
525
274
354
275
375
273
373
626
726
083
082
279
379
8is(2-etnylhexyl) phthalate-d4
Bis(2-ethylhexyl) phthalate
Benzo(b)fluoranthene-d12
BenzofahrtDeryiene
Mean
(sec)
2082
2090
2088
2086
2123
2124
2147
2239
2240
2272
2281
2293
2287
2293
2351
2350
2384
2429
2650
2660
2741
2750
EGD
Ref
164
272
164
228
164
266
164
164
269
164
164
274
164
275
164
273
164
626
164
164
164
279
Relative
1.735-1 846
0.999-1 007
1 .744-1 .848
1 000-1 001
1 771 1 880
1 000-1 002
1.867-1.982
1 000-1 002
1.902-2.025
1.000-1 005
1.906-2.033
1 000-1 005
1 .954-2 088
1 000-1 004
1.972-2 127
1.011-1.028
2 187-2 524
1.001-1.006
limit2
(«/L)
10
10
50
50
10
10
10
10
10
10
10
10
10
10
10
10
10
10
20
20
20
20
' Reference numbers beginning with 0, 1 or 5 indicate a pollutant quantified by the interna! standard method; reference num-
bers beginning with 2 or 6 indicate a labeled compound quantified by the Internal standard method; reference numbers beginning
with 3 or 7 indicate a pollutant quantified by isotope dilution.
2 This is a minimum level at which the entire GC/MS system must give recognizable mass spectra {background corrected) and
acceptable calibration points.
'Detected as aiobenzene.
4 Detected as diphenyiamine,
ns = specification not available at time of release of method.
Column: 30 ±2 m x 0.25 ±0.02 mm i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase fused silica capillary.
Temperature program; 5 min at 30 °C; 30 - 280 °C at 8 "C per min; Isothermal at 280 <"C until benzo(ghi)perylene elutes.
Gas velocity: 30 ±5 cm/sec.
TABLE 4—GAS CHROMATOGRAPHY OF ACID EXTRACTABLE COMPOUNDS
EGD
No. '
164
224
324
257
357
231
331
222
322
221
321
531
530
259
359
258
358
260
360
264
364
Compound
2,2'-difluorobiphenyl (int std)
2,4,6-triehlorophenoI
2,3,6-trichlorophenol
2-methyl-4,6-dinitrophenol
Pentachlorophenol"13C6
Pentachloroohenol ,
Retention time
Mean
(see)
1163
701
705
898
900
944
947
1086
1091
1162
1165
1170
1195
1323
1325
1349
1354
1433
1435
1559
1561
EGD
Ref
164
164
224
164
257
164
231
164
222
164
221
164
164
164
259
164
258
164
260
164
264
Relative
1.000-1.000
0.587-0.618
0.997-1.010
0.761-0.783
0.994-1.009
0.802-0.822
0.997-1 ,006
0.930-0.943
0.998-1 .003
0.994-1.005
0.998-1.004
ns
ns
1.127-1.149
1.000-1,005
1.147-1.175
0.997-1.006
1,216-1.249
1.000-1.002
1.320-1.363
0.998-1.002
Detec-
tion limit
= «P
10
10
10
20
20
10
10
10
10
10
10
10
10
50
50
50
50
20
20
50
50
! Reference numbers beginning with 0, 1 or 5 indicate a pollutant quantified by the internal standard method; reference num-
bers beginning with 2 or 8 indicate a labeled compound quantified by the infernal standard method; reference numbers beginning
with 3 or 7 indicate a pollutant quantified by isotope dilution.
3 This is a minimum level at which the entire GC/MS system must give recognizable mass spectra (background corrected) and
acceptable calibration points,
ns=specification not available at time of release of method.
Column: 30 ±2mx0.25 ±0,02mm i.d, 94% methyl. 4% phenyl, 1% vinyl bonded phase fused silica capillary.
Temperature program: 5 min at 30 °C; 8 °C/min, to 250°C or until pentachlorophenol elutes.
Gas velocity: 3Q± 5 cm/sec.
309
-------
Ph 136, App. A, Mefh. 1625
40 CFR Ch, I (7-1-04 Edition)
TABLE 5—DFTPP MASS INTENSITY
SPECIFICATIONS
TABLE 6—BASE/NEUTRAL EXTRACTABLE COM-
POUND CHARACTERISTIC MASSES—Continued
Mass Intensity required
51
68
70
127
197
199
276
365
441
442
443
30-60 percent of mass 198.
Less than 2 percent ot mass 69.
Less than 2 percent of mass 69.
40-60 percent of mass 198,
Less than 1 percent of mass 198.
5-8 percent of mass 198.
10-30 percent of mass 198.
greater than 1 percent of mass 198
present and less than mass 443
40-100 percent of mass 198.
17-23 percent of mass 442.
TABLE 6—BASE/NEUTRAL EXTRACTABLE
COMPOUND CHARACTERISTIC MASSES
Compound
Benzo(a)anthracene
Benzo(k)fluoranthene
Benzo(ghi)perylene
Bis{2-chloroethyi) ether ,
Bis(2-ethyinexyt) phthalate
n-ClO
n-C12
n-C14
n-C16
n-C18
n-C20
n-C22
n-C24
n-C26
n-C28
D-C30
4-chlorophenyl phenyl ether
Dibenzothlophene
1 ,2-dichlorobenzene
1 ,3-dichlorobenzene
Labeled
analog
d10
d8
d10
d8
d12
d12
d12
d12
d12
d10
d8
d12
d4
d22
d26
d34
d42
d50
d62
d8
d7
dS
e!12
d14
d8
dS
d4
d4
d4
Primary m/
z
154/164
152/160
178/188
184/192
228/240
252/264
252/264
252/264
276/288
154/164
93/101
93
121/131
149/153
248
149
55/66
55/66
55
65/66
55
55/66
55
55/66
55
55
55/66
167/175
162/169
204/209
228/240
114/130
278
168/176
184/192
149/153
146/152
146/152
Compound
1 N4-dichlorobenzene
3,3'-dichiorobenzidine
Diethyl phthalate
2,4-dimethylphenol , ,
Dimethyl phthalate
2,4-dinitrotoluene
2,6-dinitrotoluene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachloroeyctopentadiene
ldeno(1 ,2,3-cd)pyfene
B-naphthylamine
Nitrobenzene , ..
N-nitrosodimethylamine .
N-nrtrosodi-n-propylamine
N-nttrosodiphenylamile2
Phenanthrene
Phenol ,.
a-picoline
Pyrene
Styrene
a-terpineol
1 ,2,3-triehlorobenzene
1,2,4-trichlorobenzene
Labeled
analog
d4
d6
d4
d3
d4
d3
d3
d4
d10
d10
d10
d10
d10
13C6
13C4
13C
13C4
d8
d8
d?
d5
d6
d10
d5
d7
d10
d5
d3
d3
d3
Primary ml
z
146/152
252/ZS8
149/153
122/125
163/167
164/168
165/167
149/153
169/179
170/180
77/82
202/212
166/176
284/292
225/231
201/204
237/241
276
82/88
128/136
143/150
123/128
74
70
169/175
178/188
94/71
93/100
202/212
104/109
59/62
180/183
180/183
1 Defected as azobenzene,
2 Detected as diphenylamine.
TABLE 77—ACID EXTRACTABLE COMPOUND
CHARACTERISTIC MASSES
Compound
4-chioro-3-methylphenol
2-methyi-4,6-dinitrophenol
2 3 6-tricntoropbenol
2 4 , 5-tf ichtorophenol
Labeled
analog
d2
d4
d3
d3
d2
d4
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1625
TABLE 8—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS—Continued
E6D
No,1
378
278
305
205
372
272
374
274
375
275
373
273
379
279
712
612
318
218
043
342
242
366
266
041
067
717
617
706
606
518
719
619
520
721
621
522
723
623
524
525
726
626
528
320
220
322
222
324
224
340
240
376
276
713
613
082
705
605
704
604
368
268
325
225
326
226
327
Compound
Anthracene
Benzo(a)anthracene-d12
Benzo(k)ftuoranthene , ,
Benzo(ghi)peryiene
Biphenyl-d12
8is(2-ehloroethyl) ether
Bis(2-ehloroethyl) ether-d8
Bis(2"Ch!oroethoxy)methane*
Bis(2-ehloroisopropyl) ether
Bis(2"Chloroisopropyi)ether-d12
Bis(2-ethylhexyl) phthalate-d4
4-bromophenyl phenyl ether* ,,.,.,.,. ,
n-C10-d22
n-C12 (Appendix C) . .
n-C12-d26
n-C14 (Appendix C)*
n-C16 (Appendix C}
n-C16-d34
n-C1 8 (Appendix C)" . ,.
n-C20 {Appendix C)
n-C20-d42
n-C22 (Appendix C}*
n-C24 (Appendix C) ..., ,
n-C24-d50
n-C26 (Appendix C)*
n-C28 (Appendix C)*
n-C30 (Appendix C)
n-C3G-d62
2-chloronaphthalene ,
4-chloro-3-methylphenol-d2
2-chiorophenol-d4 ..,.,....
4-chlorophenyl phenyl ether
Chrysene ,
Chrysene-dl2
p-cymene (Appendix C)
Dibenzothiophene-dS
Di-n-butyl phthalafe-d4 ,.
1 ^-dichlorobenzene^
1 ,3-diehlorobenzene
1 ,3-dicMorobenzene~d4
1 ,4-dichtorobenzene ,
Acceptance criteria
Initial precision and ac-
curacy section 8,2.3
(M9/U
5 X
41
49
119
269
20
41
183
168
26
114
26
24
21
45
41
43
34
33
27
17
27
31
29
44
31
51
70
74
53
109
33
46
39
59
34
31
11
28
35
35
32
41
38
100
41
37
111
13
24
42
52
51
69
18
67
55
20
31
31
31
15
23
17
35
43
48
42
58-174
31-194
16-518
ns-ns
65-168
25-298
32-545
11-577
59-143
15-514
62-195
35-181
72-160
29-268
75-148
28-165
55-196
29-196
43-153
81-138
35-149
69-220
32-205
44-140
19-233
24-195
ns-298
35-369
ns-331
ns-985
80-162
37-162
42-131
53-263
34-172
45-152
80-139
27-21 1
35-193
35-193
61-200
27-242
36-165
46-357
30-168
76-131
30-174
79-135
36-162
75-166
40-161
59-186
33-219
76-140
ns-359
23-299
85-136
47-136
79-150
48-130
76-165
23-195
73-146
14-212
63-201
13-203
61-194
Labeled com-
pound recov-
ery sec. 8.3
and 14.2 P
(percent)
14-419
ns-ns
12-605
ns-ns
ns-ns
21-290
14-529
ns-ns
15-372
20-260
18-364
ns-ns
ns-ns
18-308
19-306
15-376
13-479
15-324
ns-613
23-255
19-325
13-512
ns-ns
28-220
29-215
13-346
ns-494
ns-550
Calibration
verification
sec. 12.5
(ng/rnL)
60-168
58-171
34-296
ns-ns
70-142
28-357
61-164
14-ns
13-ns
13-ns
78-129
12-ns
69-145
13-ns
58-171
52-192
61-164
52-194
44-228
67-148
44-229
76-131
43-232
52-193
22-450
42-235
44-227
60-166
41-242
37-268
72-138
54-186
40-249
54-184
62-162
40-249
65-154
50-199
26-392
26-392
66-152
24-423
44-227
58-171
72-139
85-115
68-147
78-129
55-180
71-142
57-175
70-142
24-411
79-127
66-152
13-761
73-136
66-150
72-140
69-145
71-142
52-192
74-135
61-164
65-154
52-192
62-161
On-going
accuracy
sec. 11.6 R
(H3/L)
50-199
23-242
11-672
ns-ns
62-176
22-329
20-ns
ns-ns
53-155
ns-685
59-206
32-194
58-168
25-303
62-176
17-267
5O-213
25-222
39-166
77-145
30-169
64-232
28-224
35-172
35-170
19-237
ns-504
29-424
ns-408
ns-ns
71-181
28-202
35-167
46-301
29-198
39-195
78-142
25-229
31-212
31-212
56-215
23-274
31-188
35-442
24-204
62-159
14-314
76-138
33-176
63-194
29-212
48-221
23-290
72-147
ns-468
19-340
79-146
39-160
70-168
40-156
74-169
22-209
70-152
11-247
55-225
ns-260
53-219
311
203-160 D-11
-------
Pt. 136, App. A, Meth. 1625
40 CFR Ch. I (7-1-04 Edition)
TABLE 8—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS—Continued
EGD
No-1
227
328
228
331
231
370
270
334
234
371
271
359
259
335
235
336
236
369
269
707
607
708
608
337
237
339
239
380
280
309
209
352
252
312
212
353
253
083
354
254
360
260
355
255
702
602
356
256
357
257
358
258
061
063
362
262
364
264
381
281
365
265
703
603
384
284
710
Compound
1 ,4-dichlorobenzene-d4
3,3'-dichlorobenzidine -
3,3'-dichlorotoenzidine-d6
2,4-dichiorophenol-d3
Disthyl phthaiate . ,
Diethyl phthalale-d4
2.4-dimethylphenol-d3
Dimethyl phthaiate
Dimethyl phthalate-d4
2s4-dinitrophenol-d3
2,4-dinitroioluene-d3
2,6-dinrtrotolu@ne-d3
Di-n-octyt prrthalate-d4
Diphenylamine-d1Q
Diphenyl ethet-d1Q
hexachlorocyelopentadiene
2-methyl-4,6-dinitrophenol-d2
naphthalene
2-nitrophenol-d4
phenol >
stvrene (Appendix C)
Acceptance criteria
Initial precision and ac-
curacy section 8.2.3
(M/U
s
48
26
80
12
28
44
78
13
22
36
108
18
66
18
37
30
59
16
46
45
42
19
37
73
35
33
35
29
43
16
81
56
63
227
77
15
60
55
25
23
19
64
20
39
49
33
25
28
15
23
42
188
198
198
45
37
21
49
13
40
36
161
38
138
19
29
42
X
15-193
68-174
ns-562
85-131
38-164
75-196
ns-260
62-153
15-228
74-188
ns-640
72-134
22-308
75-158
22-245
80-141
44-184
77-161
12-383
58-205
27-206
82-136
36-155
49-308
31-173
71-177
36-161
81-132
51-131
90-124
36-228
51-251
ns-316
21-ns
ns-^100
69-144
ns-ns
23-299
76-156
49-133
77-133
36-247
80-139
28-157
10-ns
ns-ns
69-161
18-265
78-140
41-145
62-146
14-398
21-^172
21^72
65-142
54-126
76-140
37-212
93-119
45-130
77-127
21-210
59-149
11-380
76-152
32-176
53-221
Labeled com-
pound recov-
ery sec. 8.3
and 14.2 P
(percent)
ns-474
ns-ns
24-260
ns-fis
ns-449
ns-fis
ns-ns
10-514
17-442
ns-ns
11-488
19-281
17-316
20-278
27-238
13-595
ns-ns
ns-ns
ns-ns
33-193
16-527
14-305
ns-ns
ns-ns
27-217
ns-ns
26-256
18-412
24-241
ns-ns
ns-ns
18-303
Calibration
verification
sec. 12.5
Jug/ml)
65-153
77-130
18-558
67-149
64-157
74-13S
47-21 1
67-150
58-172
73-137
50-201
75-133
39-256
79-127
53-187
55-183
36-278
71-140
21-467
57-176
59-169
83-120
77-129
75-134
58-174
67-149
47-215
74-135
61-164
78-128
38-265
74-135
68-148
71-141
47-212
77-129
47-21 1
13-761
70-142
52-194
69-145
56-177
73-137
71-141
39-256
44-230
85-115
46-219
77-129
61-163
55-183
35-287
40-249
40-249
68-148
59-170
77-130
42-237
75-133
67-149
65-155
48-208
60-165
31-324
78-132
48-210
65-153
On-going
accuracy
sec. 11.6 R
(H9/L)
11-245
64-185
ns-ns
83-135
34-182
65-222
ns— ns
60-156
14-242
67-207
ns-ns
68-141
17-378
72-164
19-275
70-159
31-250
74-166
10-433
51-231
21-249
77-144
29-186
40-360
26-200
64-194
30-187
70-151
38-172
85-132
23-321
43-287
ns-413
13-ns
ns-563
67-148
ns-ns
19-340
70-168
44-147
72-142
28-307
75-149
22-192
ns-ns
ns-ns
65-169
15-314
75-145
37-158
51-175
ns-ns
12-807
12-807
53-173
40-166
71-150
29-254
87-126
34-168
62-154
ns-ns
50-174
ns-608
72-159
28-196
48-244
312
-------
Environmental Protection Agency Pt. 136, App. A, Mefh. 1625
TABLE 8—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS—Continued
EGD
No.1
610
709
609
529
308
208
530
531
321
221
Compound
a-terpineol (Appendix C)
1 ,2,3-trichiorobenzene (4c)*
2,3,6-trichloropheno! (4c}*
2,4,5-trichlorophenol (4c)*
2,4.6~trichlorophenol
2.4.6-trichloroDhenol-d2
Acceptance criteria
Initial precision and ac-
curacy section 8.2.3
s ! X
49
44
48
69
19
57
30
30
57
47
ns-281
42-234
22-292
15-229
82-136
15-212
58-137
58-137
59-205
43-183
Labeled com-
pound recov-
ery S8C. 8.3
and 14.2 P
(percent)
ns-ns
ns-672
ns-592
21-363
Calibration
verification
sec. 12.5
(ng/mL)
44-228
54-186
20-502
60-167
78-128
61-163
56-180
56-180
81-123
69-144
On-going
accuracy
sec. 11. 6 R
(tig/L)
ns-348
38-258
18-339
11-297
77-144
10-282
51-153
51-153
48-244
34-226
1 Reference numbers beginning with 0, 1 or 5 indicate a pollutant quantified by the internal standard method; reference num-
bers beginning with 2 or 6 indicate a labeled compound quantified by the internal standard method; reference numbers beginning
with 3 or 7 indicate a pollutant quantified by isotope dilution.
"Measured by internal standard; specification derived from related compound.
ns=no specification; limit is outside the range that can be measured reliably.
313
-------
Pt. 136, App, A, Meth. 1625
40 CFR Ch. I (7-1-04 Edition)
> 1.0-
3
2 10 20 50 100 200
CONCENTRATION {MS^M
AREA* 48300
FIGURE 1 Relative Response Calibration Curve
tor Phenol. The Dotted Lines Enclose a ±10
Percent Error Window.
FIGURE 3 Extracted Ion Current Profiles for (3A)
Unlabelsd Compound, (3B) Labeled Compound,
and (3C) Equal Mixture of Uniabeled and Labeled
Compounds,
FIGURE 2 Extracted Ion Current Profiles for
Chromataarapnically Resolved Labeled (m^z) and
Unlabeled (m,/z) Pairs.
314
-------
Environmental Protection Agency
Ft. 136, App. A, Meth, 1625
STANDARD
BLANK
SAMPLE
110.1.1
[10.1.21
[10.1.31
[10.1.4J
(10.21
[10.31
[10.4.21
(10.4,10.5!
[11.3]
[11.4J
s
ORG*
^ f
1 L REAGENT
WATER
X
SPIKE 500 pi
Of 200 jigrtnL
ISOTOPES
X
SPIKE 1.0 mL
OF STANDARDS
X
STIR AND
EQUILIBRATE
1 L REAGENT
WATER
1 L ALIQUOT
X X
SPIKE 500 (jL
OF 200 jjgtoL
ISOTOPES
^
SPIKE 500 ML
OF 200 ns/mL
ISOTOPES
t \
STIR AND
EQUILIBRATE
FANDARD Oft BLANK
EXTRACT BASE/
NEUTRAL
kNIC
CONCENTRATE
TO 2-4 n>L
1 AQUEOUS
4,
EXTRACT ACID
X
CONCENTRATE
TO 2-4 mL
I
4-
CONCENTRATE
TO 1.0 mL
X
ADD INTERNAL
STANDARD
X
INJECT
one
*
t
STIR AND
EQUILIBRATE
X
EXTRACT BASE;
NEUTRAL
ANIC AQUEOUS
t
CONCENTRATE
TOlOmL
4,
EXTRACT ACID
s f
CONCENTRATE
TO 1.0 mL
1 1
ADD INTERNAL
STANDARD
ADD INTERNAL
STANDARD
1 X
INJECT
INJECT
FIGURE 4 Flow Chart lor Extraction/Concentration ol Precision and Recovery Standard, Blank,
and Sample by Method 1625. Numbers in Brackets [ 1 Refer to Section Numbers in the Method,
315
-------
Pt. 136, App. A, Meth. 1625
40 CFR Ch. I (7-1-04 Edition)
/w\ _J
1 1 j 1 1 1 1 1 1
ANTHRACENE-D^
, .
. -
123456789 10
ANALYSIS NUMBER
til Ul 1,10 •
Z <
tu £p
> z
*«• UJ
58
I 1 3 I I II I I
ANTHRACENE
_.^
• I 0-90 -| 1 , , , 1 , , 1 r
< 8/1 6/1 6/1 Sn 6/2 6/2 6/3 6/3 6/4 6/5
5 DATE ANALYZED
FIGURE 5 Quality Control Charts Showing Area (top graph) and
Relative Response of Anthracene to Anthracene-d10 (lower graph)
Plotted as a Function of Time or Analysis Number.
R3C
83/13^84 3:24:80 CSU: i
&WIE: <*. G,UER. 80180, ee,C.Ntt:»tt.NaS
COWfi,: 16/» 3»,8..t«r '*» 3(^28
-------
Environmental Protection Agency
Pt. 136, App. A, Meth. 1625
ATTACHMENT 1 TO METHOD 1625
INTRODUCTION
To support measurement of several
semivolatile pollutants, EPA lias developed
this attachment to EPA Method 1625B.1 The
modifications listed in this attachment are
approved only for monitoring wastestreams
from the Centralized Waste Treatment Point
Source Category (40 CPR Part 437) and the
Landfills Point Source Category (40 CPE
Part 445). EPA Method 1625B (the Method)
employs sample extraction with methylene
chloride followed by analysis of the extract
using- capillary column gas chromatography-
mass spectrometry (GC/MS). This attach-
ment addresses the addition of the
semivolatile pollutants listed in Tables 1 and
2 to all applicable standard, stock, and spik-
ing solutions utilized for the determination
of semivolatile organic compounds by EPA
Method 1625B.
1.0
EPA METHOD 1625 REVISION B
MODIFICATION SUMMARY
The additional semivolatile organic com-
pounds listed in Tables 1 and 2 are added to
all applicable calibration, spiking, and other
solutions utilized in the determination of
semivolatile compounds by EPA Method
1625. The instrument is to be calibrated with
these compounds, and all procedures and
quality control tests described in the Method
must be performed,
2.0 SECTION MODIFICATIONS
NOTE: All section and figure numbers in
this Attachment reference section and figure
numbers in EPA Method 1626 Revision B un-
less noted otherwise. Sections not listed here
remain unchanged.
Section 6.7 The stock standard solutions de-
scribed in this section are modified such
that the analytes in Tables 1 and 2 of this
attachment are required in addition to
those specified in the Method.
Section 6.8 The labeled compound spiking:
solution in this section is modified to in-
clude the labeled compounds listed in Ta-
bles 5 and 6 of this attachment.
Section 6.9 The secondary standard is modi-
fied to include the additional analytes
'EPA Method 1625 Revision B,
Semivolatile Org-anic Compounds by Isotope
Dilution GC/MS, 40 CFR Part 136, Appendix
A.
listed in Tables 1 and 2 of this attach-
ment.
Section 6.12 The solutions for obtaining au-
thentic mass spectra are to include all
additional analytes listed in Tables 1 and
2 of this attachment.
Section 6.13 The calibration solutions are
modified to include the analytes listed in
Tables 1 and 2 and the labeled compounds
listed in Tables 5 and 6 of this attach-
ment.
Section 6.14 The precision and recovery
standard is modified to include the
analytes listed in Tables 1 and 2 and the
labeled compounds listed in Tables 5 and
6 of this attachment.
Section 6.15 The solutions containing the
additional analyt.es listed in Tables 1 and
2 of this attachment are to be analyzed
for stability.
Section 7.2.1 This section is modified to in-
clude the analytes listed in Tables 1 and
2 and the labeled compounds listed in Ta-
bles 5 and 6 of this attachment.
Section 7.4.5 This section is modified to in-
clude the analytes listed in Tables 1 and
2 and the labeled compounds listed in Ta-
bles 5 and 8 in the calibration.
Section 8.2 The initial precision and recov-
ery (IPR) requirements are modified to
include the analytes listed in Tables 1
and 2 and the labeled compounds listed in
Tables 5 and 6 of this attachment. Addi-
tional IPE performance criteria are sup-
plied in Table 7 of this attachment.
Section 8.3 The labeled compounds listed in
Tables 3 and 4 of this attachment are to
be included in the method performance
tests. Additional method performance
criteria are supplied in Table 7 of this at-
tachment.
Section 8.5.2 The acceptance criteria for
blanks includes the analytes listed in Ta-
bles 1 and 2 of this attachment.
Section 10.1.2 The labeled compound solu-
tion must include the labeled compounds
listed in Tables 5 and 6 of this attach-
ment.
Section 10.1,3 The precision and recovery
standard must include the analytes list-
ed in Tables 1 and 2 and the labeled com-
pounds listed in Tables 5 and 6 of this at-
tachment.
Section 12.5 Additional QC requirements for
calibration verification are supplied in
Table 7 of this attachment.
Section 12.7 Additional QC requirements for
ongoing precision and recovery are sup-
plied in Table 7 of this attachment.
317
-------
Pt. 136, App. A, Meth. 1625 40 CFR Ch. I (7-1-04 Edition)
TABLE 1—BASE/NEUTRAL EXTRACTABLE COMPOUNDS
Pollutant
Compound
acetophenone'
aniline2
-2,3-dichloroaniline'
-o-cresol'
pyridine3 ,
CAS
Registry
98-86-2
62-53-3
608-27-5
95-J»-7
110-86-1
EPA-EGD
758
757
578
771
1330
CAS ^ Chemical Abstracts Registry.
EGD - Effluent Guidelines Division,
' Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
2 Analysis of this poilutanl is approved only for the Centralized Waste Treatment and Landfills industries,
TABLE 2—ACID EXTRACTABLE COMPOUNDS
Compound
o-creso! ! .
Pollutant
CAS
Registry
106-^(4-5
EPA-EGD
1744
CAS = Chemical Abstracts Registry.
EGD = Effluent Guidelines Division.
1 Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.
TABLE 3—GAS CHROMATOGRAPHY ' OF BASE/NEUTRAL EXTRACTABLE COMPOUNDS
EGD No.
758
757 . .
578
771
1330
Compound
ovridine5
Mean
(sec)
818
694
1160
814
378
Retention time 2
EGD Ref
658
657
164
871
1230
Relative
1 003-1 005
0.994-1 ,023
1 003-1 007
1 .005-1 .009
1.00S-1.011
Minimum
level '
Sug/L)
10
10
10
10
10
EGD = Effluent Guidelines Division.
1 The data presented in this table were obtained under the chromatographic conditions given in the footnote to Table 3 of EPA
Method 1625B.
2 Retention times are approximate and are intended to be consistent with the retention times for the analytes in EPA Method
162SB.
3 See the definition in footnote 2 to Table 3 of EPA Method 1625B.
4 Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
* Analysts of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries,
TABLE 4—GAS CHROMATOGRAPHY > OF ACID EXTRACTABLE COMPOUNDS
EGD No.
1744
Compound
p~cresol4 , ,
Mean
(sec)
834
Retention time2
EGD Ref
1644
Relative j
1.004-1.008 I
Minimum
level
(u/L)-'
20
EGO = Effluent Guidelines Division.
'The data presented in this table were obtained under the chromatographic conditions given in the footnote to Table 4 of EPA
Method 1625B.
2 Retention times are approximate and are intended to be consistent with the retention times for the analytes in EPA Method
1625B.
3 See the definition in footnote 2 to Table 4 of EPA Method 1625B.
4 Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.
TABLE 5—BASE/NEUTRAL EXTRACTABLE COMPOUND CHARACTERISTIC M/Z'S
Compound
pyridine3 ,.,.,.,.,.,....,...,.,.,.,..,.„,. ,.,.,.,.,.,.,.....„.,...,.,.,.,„.,.,.......
m/2 = mass to charge ratio.
i Labeled Ana- j
log
u
d- i
• n/a 1
Primary
mlz l
105/110
93/1 00
108/116
181
79/84
318
-------
Environmental Protection Agency
Pt, 136, App. B
' Native/labeled.
2 Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
:J5 Analysis of this pollutant is approved on!y for the Centralized Waste Treatment and Landfills industries.
TABLE 6—ACID EXTRACTABLE COMPOUND CHARACTERISTIC M/Z'S
p-creso!- ...-..«.,,.....„-,..,.-
Compound
1 Labeled Ana-
I log
.„..., .,...,...,.,., ' d,
Primary
m/z '
108/116
m/z - mass to charge ratio.
1 Native/labeled.
2 Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.
TABLE 7—ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS
EGO No,
758
658
757
857
771
671
1744
1644
578
1330
1230
Compound
acetophenone-d s '
aniline2
aniline-*
o-creso
p-creso
p-creso
2,3-did-
pyridine
Dvridine
r
-d-,'
2
-d,2
-d,J
Acceptance criteria
Initial precision and accu-
racy section 8.2
(M/L)
tak)
34
51
32
71
40
23
59
22
13
28
ns
X
44-167
23-254
30-171
15-278
31-226
30-146
54-140
11-618
40-160
10-421
7-392
Labeled
compound
recovery
sec. S.3 and
14.2 P
(percent)
45-162
33-154
35-196
37-203
19-238
Calibration
verification
sec. 12.5
^ig/'mL)
85-115
85-115
85-115
85-115
85-115
85-115
85-115
85-115
85-115
83-117
85-115
On -going
accuracy
sec, 12.7 R
(M9/M
45-162
22-264
33-154
12-344
35-196
31-142
37-203
16-415
44-144
18-238
4-621
s = Standard deviation of four recovery measurements.
X = Average recovery for four recovery measurements.
EGD = Effluent Guidelines Division.
ns = no specification; limit is outside the range that can be measured reliably.
1 Analysis of this pollutant is approved only for the Cenlralized Waste Treatment industry.
~ Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.
[49 FR 43261, Oct. 26, 1984; 50 FR 692, 695, Jan. 4, 1985, as amended at 51 FR 23702, June 30, 1986;
62 FR 48405, Sept. 15, 1997; 65 PR 3044, Jan. 19, 2000; 65 FR 81295, 81298, Dec. 22, 2000]
APPENDIX B TO PART 136—DEFINITION
AND PROCEDURE FOR THE DETER-
MINATION OF THE METHOD DETEC-
TION LIMIT—REVISION 1.11
Definition
The method detection limit (MDL) is de-
fined as the minimum concentration of a
substance that can be measured and reported
with 99% confidence that the analyte con-
centration is greater than zero and is deter-
mined from analysis of a sample in a given
matrix containing the analyte,
Scope and Application
This procedure is designed for applicability
to a wide variety of sample types ranging
from reagent (blank) water containing'
analyte to wastewater containing analyte.
The MDL for an analytical procedure may
vary as a function of sample type. The proce-
dure requires a complete, specific, and well
defined analytical method. It is essential
that all sample processing- steps of the ana-
lytical method be included in the determina-
tion of the method detection limit.
The MDL obtained by this procedure is
used to judge the significance of a single
measurement of a future sample.
The MDL procedure was designed for appli-
cability to a broad variety of physical and
chemical methods. To accomplish this, the
procedure was made deyice- or instrument-
independent,
Procedure
1. Make an estimate of the detection limit
using one of the following:
(a) The concentration value that cor-
responds to an instrument signal/noise in the
range of 2.5 to 5.
(b) The concentration equivalent of three
times the standard deviation of replicate in-
strumental measurements of the analyte in
reagent water.
(c) That region of the standard curve where
there is a significant change in sensitivity.
i.e., a break in the slope of the standard
curve.
319
-------
Pt. 136, App, B
40 CFR Ch. I (7-1-04 Edition)
(d) Instrumental limitations.
It is recognized that the experience of the
analyst is important to this process. How-
ever, the analyst must include the above
considerations in the initial estimate of the
detection limit,
2. Prepare reagent (blank) water that Is as
free of analyte as possible. Reagent or inter-
ference free water is defined as a water sam-
ple in which analyte and interferent con-
centrations are not detected at the method
detection limit of each analyte of interest.
Interferences are defined as systematic er-
rors in the measured analytical signal of an
established procedure caused by the presence
of interfering species (interferent). The
interferent concentration is presupposed to
be normally distributed in representative
samples of a given matrix.
3. (a) If the MDL is to be determined in re-
agent (blank) water, prepare a laboratory
standard (analyte in reagent water) at a con-
centration which is at least equal to or in
the same concentration rangre as the esti-
mated method detection limit, (Recommend
between 1 and 5 times the estimated method
detection limit.) Proceed to Step 4,
(b) If the MDL is to be determined in an-
other sample matrix, analyze the sample. If
the measured level of the analyte is in the
recommended range of one to five times the
estimated detection limit, proceed to Step 4.
If the measured level of analyte is less
than the estimated detection limit, add a
known amount of analyte to bring the level
of analyte between one and five times the es-
timated detection limit.
If the measured level of analyte is greater
than five times the estimated detection
limit, there are two options.
(1) Obtain another sample with a lower
level of analyte in the same matrix if pos-
sible.
(2) The sample may be used as is for deter-
mining the method detection limit if the
analyte level does not exceed 10 times the
MDL of the analyte in reagent water. The
variance of the analytical method changes as
the analyte concentration increases from the
MDL, hence the MDL determined under
these circumstances may not truly reflect
method variance at lower analyte concentra-
tions.
4. (a) Take a minimum of seven aliquots of
the sample to be used to calculate the meth-
od detection limit and process each through
the entire analytical method. Make all com-
putations according to the defined method
with final results in the method reporting
units. If a blank measurement is required to
calculate the measured level of analyte, ob-
tain a separate blank measurement for each
sample aliquot analyzed. The average blank
measurement is subtracted from the respec-
tive sample measurements.
(b) It may be economically and technically
desirable to evaluate the estimated method
detection limit before proceeding with 4a.
This will: (1) Prevent repeating this entire
procedure when the costs of analyses are
high and (2) insure that the procedure is
being conducted at the correct concentra-
tion. It is quite possible that an inflated
MDL will be calculated from data obtained
at many times the real MDL even though the
level of analyte is less than five times the
calculated method detection limit. To insure
that the estimate of the method detection
limit is a good estimate, it is necessary to
determine that a lower concentration of
analyte will not result in a significantly
lower method detection limit. Take two
aliquots of the sample to be used to calculate
the method detection limit and process each
through the entire method, including blank
measurements as described above in 4a.
Evaluate these data;
(1) If these measurements indicate the
sample is in desirable range for determina-
tion of the MDL, take five additional
aliquots and proceed. Use all seven measure-
ments for calculation of the MDL.
(2) If these measurements indicate the
sample is not in correct range, reestimate
the MDL, obtain new sample as in 3 and re-
peat either 4a or 4b.
5. Calculate the variance (S2) and standard
deviation (S) of the replicate measurements,
as follows;
I*?
where:
Xi; 1=1 to n, are the analytical results in the
final method reporting units obtained from
320
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Environmental Protection Agency
Pt. 136, App. B
the n sample aliquots and I refers to the
sum of the X values from 1=1 to n.
6. (a) Compute the MDL as follows:
MDL = IVM-a-O^l (S)
where:
MDL = the method detection limit
ttn-i.i-oK.99> = the students' t value appropriate
for a 99% confidence level and a standard
deviation estimate with n-1 degrees of free-
dom. See Table.
S = standard deviation of the replicate anal-
yses.
(b) The 96% confidence interval estimates
for the MDL derived in 6a are computed ac-
cording- to the following equations derived
from percentiles of the chi square over de-
grees of freedom distribution (x2/df).
LCL = 0.64 MDL
UCL = 2.20 MDL
where: LCL and UCL are the lower and upper
95% confidence limits respectively based
on seven aliquots.
7. Optional iterative procedure to verify
the reasonableness of the estimate of the
MDL and subsequent MDL determinations.
(a) If this is the initial attempt to compute
MDL based on the estimate of MDL formu-
lated in Step 1, take the MDL as calculated
in Step 6, spike the matrix at this calculated
MDL and proceed through the procedure
starting with Step 4.
(b) If this is the second or later iteration of
the MDL calculation, use S2 from the cur-
rent MDL calculation and S2 from the pre-
vious MDL calculation to compute the F-
ratio. The P-ratio is calculated by sub-
stituting the larger S2 into the numerator
S2A and the other into the denominator S2a.
The computed F-ratio is then compared with
the F-ratio found in the table whicli is 3.05 as
follows: if S2A(S2B<3.05, then compute the
pooled standard deviation by the following
equation:
'pooled
6SJ+6S*?
12
if S2A/S2B>3.05, respike at the most recent
calculated MDL and process the samples
through the procedure starting- with Step
4. If the most recent calculated MDL
does not permit qualitative identifica-
tion when samples are spiked at that
level, report the MDL as a concentration
between the current and previous MDL
whicli permits qualitative identification.
(c) Use the Sptx)|Cd as calculated in 7b to
compute The final MDL according to the fol-
lowing equation:
MDL=2.681 (Spooled)
where 2.681 is equal to t(i2,i-<«=.9o).
(d) The 95% confidence limits for MDL de-
rived in 7c are computed according to the
following equations derived from precentiles
of the chi squared over degrees of freedom
distribution.
LCL=0.72 MDL
UCL=1,6S MDL
where LCL and UCL are the lower and upper
95% confidence limits respectively based on
14 aliquots.
TABLES OF STUDENTS' T VALUES AT THE 99
PERCENT CONFIDENCE LEVEL
TABLES OF STUDENTS' T VALUES AT THE 99
PERCENT CONFIDENCE LEVEL—Continued
Number of replicates
8
9
11
16
21
31
61
00
Degrees
of free-
dom (n-1)
7
8
9
10
15
20
25
30
60
00
Wi..»)
2.998
2896
2821
2764
2.602
2.528
2.485
2.457
2.390
2.326
3.143
Reporting
The analytical method used must be spe-
cifically identified by number or title aid the
MDL for each analyte expressed in the ap-
propriate method reporting units. If the ana-
lytical method permits options which affect
the method detection limit, these conditions
must be specified with the MDL value. The
sample matrix used to determine the MDL
mast also be identified with MDL value. Re-
port the mean analyte level with the MDL
and indicate if the MDL procedure was
iterated. If a laboratory standard or a sam-
ple that contained a known amount analyte
was used for this determination, also report
the mean recovery.
321
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Pt. 136, App. C
40 CFR Ch, I (7-1-04 Edition)
If the level of analyte in the sample was
below the determined MDL or exceeds 10
times the MDL of tlie analyte in reagent
water, do not report a value for the MDL.
[49 FR 43430, Oct. 26, 1984; 50 FR 694, 696, Jan.
4, 1985, as amended at 51 FR 23703, June 30,
1986]
APPENDIX C TO PART 136—INDUCTIVELY
COUPLED PLASMA—ATOMIC EMISSION
SPECTEOMETRIC METHOD FOR TRACE
ELEMENT ANALYSIS OF WATER AND
WASTES METHOD 200.7
1. Scope and Application
1.1 This method may be used for the de-
termination of dissolved, suspended, or total
elements In drinking water, surface water,
and domestic and industrial wastewaters.
1.2 Dissolved elements are determined in
filtered and acidified samples. Appropriate
steps must be taken in all analyses to ensure
that potential interferences are taken into
account. This is especially true when dis-
solved solids exceed 1500 mg/L. (See Section
5.)
1.3 Total elements are determined after
appropriate digestion procedures are per-
formed. Since digestion techniques increase
the dissolved solids content of the samples,
appropriate steps must be taken to correct
for potential interference effects. (See Sec-
tion 5.)
1.4 Table 1 lists elements for which this
method applies along with recommended
wavelengths and typical estimated Instru-
mental detection limits using conventional
pneumatic nebulization. Actual working- de-
tection limits are sample dependent and as
the sample matrix varies, these concentra-
tions may also vary. In time, other elements
may be added as more information becomes
available and as required.
1.5 Because of the differences between
various makes and models of satisfactory in-
struments, no detailed Instrumental oper-
ating instructions can be provided. Instead,
the analyst is referred to the instruction
provided by the manufacturer of the par-
ticular Instrument.
2. Summary of Method
2.1 The method describes a technique for
the simultaneous or sequential multielement
determination of trace elements In solution.
The basis of the method is the measurement
of atomic emission by an optical
spectroscopic technique. Samples are
nebulized and the aerosol that is produced is
transported to the plasma torch where exci-
tation occurs. Characteristic atomic-line
emission spectra are produced by a radio-fre-
quency inductively coupled plasma (IOP).
The spectra are dispersed by a grating spec-
trometer and the intensities of the lines are
monitored by photomultipller tubes. The
photocurrents from the photomultlplier
tubes are processed and controlled by a com-
puter system. A background correction tech-
nique is required to compensate for variable
background contribution to the determina-
tion of trace elements. Background must be
measured adjacent to analyte lines on sam-
ples during analysis. The position selected
for the background intensity measurement,
on either or both sides of the analytical line,
will be determined by the complexity of the
spectrum adjacent to the analyte line. The
position used must be free of spectral inter-
ference and reflect the same change in back-
ground intensity as occurs at the analyte
wavelength measured. Background correc-
tion is not required in cases of line broad-
ening where a background correction
measurement would actually degrade the
analytical result. The possibility of addi-
tional interferences named in 5.1 (and tests
for their presence as described la 5.2) should
also be recognized and appropriate correc-
tions made.
3. Definitions
3.1 Dissolved—Those elements which will
pass through a 0.45 p.m membrane filter.
3.2 Suspended—Those elements which are
retained by a 0.45 nm membrane filter.
3.3 Total—The concentration determined
on an unfiltered sample following vigorous
digestion (Section 9.3), or the sum of the dis-
solved plus suspended concentrations. (Sec-
tion 9.1 plus 9.2).
3.4 Total recoverable—The concentration
determined on an unaltered sample fol-
lowing treatment with hot, dilute mineral
acid (Section 9.4).
3.5 Instrumental detection limit—The con-
centration equivalent to a signal, due to the
analyte, which is equal to three times the
standard deviation of a series of ten replicate
measurements of a reagent blank signal at
the same wavelength.
3.6 Sensitivity—The slope of the analytical
curve, I.e. functional relationship between
emission intensity and concentration.
3.7 Instrument check standard—A multiele-
ment standard of known concentrations pre-
pared by the analyst to monitor and verify
instrument performance on a daily basis.
(See 7.6.1)
3.8 Interference check sample—A solution
containing both interfering and analyte
elemelts of known concentration that can be
used to verify background and interelement
correction factors. (See 7.6.2.)
3.9 Quality control sample—A solution ob-
tained from an outside source having known,
concentration values to be used to verify the
calibration standards. (See 7.6.3)
3.10 Calibration standards—A series of
known standard solutions used by the ana-
lyst for calibration of the instrument (i.e.,
preparation of the analytical curve). (See 7.4)
322
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Environmental Protection Agency
R. 136, App. C
3.11 Linear dynamic range—The concentra-
tion range over which the analytical curve
remains linear.
3.12 Reagent blank—A volume of deionized,
distilled water containing the same acid ma-
trix as the calibration standards carried
through the entire analytical scheme. (See
7.5.2)
3.13 Calibration blank—A volume of deion-
ized, distilled water acidified with HNO3 and
HC1. (See 7.5.1)
3.14 Methmd of standard addition— The
standard addition technique involves the use
of the unknown and the unknown plus a
known amount of standard. (See 10.6.1.)
4. Safety
4,1 The toxicity of carcinogenicity of each
reagent used in this method has not been
precisely defined; however, each chemical
compound should be treated as a potential
health hazard. From this viewpoint, expo-
sure to these chemicals must be reduced to
the lowest possible level by whatever means
available. The laboratory is repsonsible for
maintaining a current awareness file of
OSHA regulations regarding the safe han-
dling of the chemicals specified in this meth-
od. A reference file of material data handling
sheets should also be made available to all
personnel involved in the chemical analysis.
Additional references to laboratory safety
are available and have been identified
d47.i4.8,«di4,9) f0r the information of the ana-
lyst.
5. Interferences
5.1 Several types of interference effects
may contribute to inaccuracies in the deter-
mination of trace elements. They can be
summarized as follows:
5.1.1 Spectral interferences can be cat-
egorized as (1) overlap of a spectral line from
another element; (2) unresolved overlap of
molecular band spectra; (3) background con-
tribution from continuous or recombination
phenomena; and (4) background contribution
from stray light from the line emission of
high concentration elements. The first of
these effects can be compensated by utilizing
a computer correction of the raw data, re-
quiring the monitoring and measurement of
the interfering element. The second effect
may require selection of an alternate wave-
length. The third and fourth effects can usu-
ally be compensated by a background correc-
tion adjacent to the analyte line. In addi-
tion, users of simultaneous multi-element
instrumentation must assume the responsi-
bility of verifying the absence of spectral in-
terference from an element that could occur
in a sample but for which there is no channel
in the instrument array. Listed in Table 2
are some interference effects for the rec-
ommended wavelengths given in Table 1. The
data in Table 2 are intended for use only as
a rudimentary guide for the indication of po-
tential spectral interferences. For this pur-
pose, linear relations between concentration
and intensity for the analytes and the
interferente can be assumed. The Inter-
ference information, which was collected at
the Ames Laboratory,1 is expressed as
analyte concentration equivalents (i.e. false
analyte concentrations) arising from 100 mg/
L of the interferent element. The suggested
use of this information is as follows: Assume
that arsenic (at 193.696 nm) is to be deter-
mined in a sample containing approximately
10 mg/L of aluminum. According to Table 2,
100 mg/L of aluminum would yield a false sig-
nal for arsenic equivalent to approximately
1.3 mg/L. Therefore, 10 mg/L of aluminum
would result in a false signal for arsenic
equivalent to approximately 0.13 mg/L, The
reader is cautioned that other analytical
systems may exhibit somewhat different lev-
els of interference than those shown in Table
2, and that the interference effects must be
evaluated for each individual system.
Only those interferents listed were inves-
tigated and the blank spaces in Table 2 indi-
cate that measurable interferences were not
observed for the interferent concentrations
listed in Table 3. Generally, interferences
were discernible if they produced peaks or
background shifts corresponding to 2-5% of
the peaks generated by the analyte con-
centrations also listed in Table 3.
At present, information on the listed silver
and potassium wavelengths are not available
but it has been reported that second order
energy from the magnesium 383.231 nm wave-
length interferes with the listed potassium
line at 766.491 nm.
5.1.2 Physical interferences are generally
considered to be effects associated with the
sample nebulization and transport processes.
Such properties as change in viscosity and
surface tension can cause significant inac-
curacies especially in samples which may
contain high dissolved solids and'or acid con-
centrations. The use of a peristaltic pump
may lessen these interferences. If these types
of interferences are operative, they must be
reduced by dilution of the sample and/or uti-
lization of standard addition techniques. An-
other problem which can occur from high
dissolved solids is salt buildup at the tip of
the nebulizer. This affects aersol flow rate
causing instrumental drift. Wetting the
argon prior to nebulization, the use of a tip
washer, or sample dilution have been used to
control this problem. Also, it has been re-
ported that better control of the argon flow
rate improves instrument performance. This
is accomplished with the use of mass flow
controllers.
'Ames Laboratory, USDOB, Iowa State
University, Ames Iowa 50011.
323
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R. 136, App. C
40 CFR Ch. I (7-1-04 Edition)
5.1.3 Chemical Interferences are character-
ized by molecular compound formation, lon-
ization effects and solute vaporization ef-
fects. Normally these effects are not pro-
nounced with the ICP technique, however, if
observed they can be minimized by careful
selection of operating conditions (that is, in-
cident power, observation position, and so
forth), by buffering of the sample, by matrix
matching, and by standard addition proce-
dures. These types of interferences can be
highly dependent on matrix type and the
specific analyte element.
5.2 It is recommended that whenever a
new or unusual sample matrix is encoun-
tered, a series of tests be performed prior to
reporting concentration data for analyte ele-
ments. These tests, as outlined in 5,2.1
through 5.2.4, will ensure the analyst that
neither positive nor negative interference ef-
fects are operative on any of the analyte ele-
ments thereby distorting the accuracy of the
reported values.
5,2.1 Serial dilution. If the analyte con-
centration is sufficiently high (minimally a
factor of 10 above the instrumental detection
limit after dilution), an analysis of a dilu-
tion should agree within 5 percent of the
original determination (or within some ac-
ceptable control limit (14.3) that has been es-
tablished for that matrix.). If not, a chemical
or physical interference effect should be sus-
pected,
5.2.2 Spike addition. The recovery of a
spike addition added at a minimum level of
10X the instrumental detection limit (max-
imum 100X) to the original determination
should be recovered to within 90 to 110 per-
cent or within the established control limit
for that matrix. If not, a matrix effect
should be suspected. The use of a standard
addition analysis procedure can usually com-
pensate for this effect.
Caution: The standard addition technique
does not detect coincident spectral overlap,
If suspected, use of computerized compensa-
tion, an alternate wavelength, or comparison
with an alternate method is recommended
(See 5.2.3).
5.2.3 Comparison with alternate method of
analysis. When investigating a new sample
matrix, comparison tests may be performed
with other analytical techniques such as
atomic absorption spectrometry, or other ap-
proved methodology.
5.2.4 Wavelength scanning of analyte line re-
gion. If the appropriate equipment is avail-
able, wavelength scanning can be performed
to detect potential spectral interferences.
S. Apparatus
6.1 Inductively Coupled Plasma-Atomic
Emission Spectrometer.
6.1.1 Computer controlled atomic emis-
sion spectrometer with background correc-
tion.
6.1.2 Radiofrequency generator.
6.1.3 Argon gas supply, welding grade or
better.
6.2 Operating conditions—Because of the
differences between various makes and mod-
els of satisfactory instruments, no detailed
operating instructions can be provided. In-
stead, the analyst should follow the instruc-
tions provided by the manufacturer of the
particular instrument. Sensitivity, instru-
mental detection limit, precision, linear dy-
namic range, and interference effects must
be investigated and established for each indi-
vidual analyte line on that particular instru-
ment. It is the responsibility of the analyst
to verify that the instrument configuration
and operating conditions used satisfy the an-
alytical requirements and to maintain qual-
ity control data confirming instrument per-
formance and analytical results.
7. Reagents and Standards
7.1 Acids used in the preparation of stand-
ards and for sample processing must be
ultra-high purity grade or equivalent. Redis-
tilled acids are acceptable.
7.1.1 Acetic acid, cone, (sp gr 1.06).
7.1.2 Hydrochloric acid, cone, (sp gr 1.19).
7.1.3 Hydrochloric acid, (1+1): Add 500 mL
cone. HC1 (sp gr 1.19) to 400 mL deionized,
distilled water and dilute to 1 liter.
7.1,4 Nitric acid, cone, (sp grr 1.41).
7.1.5 Nitric acid, (1+1): Add 500 mL cone.
HNO3 (sp gr 1.41) to 400 mL deionized, dis-
tilled water and dilute to 1 liter.
7,2 Deionieed, distilled water: Prepare by
passing distilled water through a mixed bed
of cation and anion exchange resins. Use de-
ionized, distilled water for the preparation of
all reagents, calibration standards and as di-
lution water. The purity of this water must
be equivalent to ASTM Type II reagent
water of Specification D 1193 (14.6).
7.3 Standard stock solutions may be pur-
chased or prepared from ultra high purity
grade chemicals or metals. All salts must be
dried for 1 h at 105 °C unless otherwise speci-
fied.
(CAUTION: Many metal salts are ex-
tremely toxic and may be fatal if swallowed.
Wash hands thoroughly after handling.)
Typical stock solution preparation proce-
dures follow:
7.3.1 Aluminum solution, stock, 1 mL=100ng
Al: Dissolve 0.100 g of aluminum metal in an
acid mixture of 4 mL of (1+1) HC1 and 1 mL
of cone. HNOj in a beaker. Warm gently to
effect solution. When solution is complete,
transfer quantitatively to a liter flask add
an additional 10 mL of (1+1) HC1 and dilute
to 1,000 mL with deionized, distilled water.
7.3,2 Antimony solution stock, 1 mL=100 m?
Sb: Dissolve 0.2669 g K(SbO)C4H4O6 in deion-
ized distilled water, add 10 mL (1+1) HC1 and
dilute to 1,000 mL with deionized, distilled
water.
324
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Environmental Protection Agency
Pt. 136, App. C
7.3.3 Arsenic solution, stock, 1 mL=100 \ig
As: Dissolve 0.1320 g of As2O.i in 100 mL of de-
ionized, distilled water containing 0.4 g
NaOH. Acidify the solution with 2 mL cone.
HNO3 and dilute to 1,000 mL with deionized,
distilled water.
7.3.4 Barium solution, stock, 1 mL=100 n§
Ba: Dissolve 0.1516 g BaCl2 (dried at 250°C for
2 hrs) in 10 mL deionized, distilled water
with 1 mL (1+1) HC1. Add 10.0 mL (1+1) HC1
and dilute to 1,000 with mL deionized, dis-
tilled water.
7.3.5 Beryllium solution, stock, 1 mL=100 |ig
Be: Do not dry. Dissolve 1.966 g BeSCV-JHaO,
in deionized, distilled water, add 10.0 mL
oono. HNO3 and dilute to 1,000 mL with de-
ionized, distilled water.
7.3.6 Boron solution, stock, 1 mL=100(ig B:
Do not dry. Dissolve 0.5716 g anhydrous H3BO3
in deionized, distilled water and dilute to
1,000 mL. Use a reagent meeting ACS speci-
fications, keep the bottle tightly stoppered
and store in a desiccator to prevent the en-
trance of atmospheric moisture.
7.3.7 Cadmium solution, stock, 1 mL=100 pg
Cd: Dissolve 0.1142 g CdO in a minimum
amount of (1+1) HNO3, Heat to increase rate
of dissolution. Add 10.0 mL cone. HNO3 and
dilute to 1,000 mL with deionized, distilled
water.
7.3.8 Calcium solution, stock, 1 mL=100 ng
Oa: Suspend 0.2498 g CaCOj dried at 180 °C for
1 h "before weighing in deionized, distilled
water and dissolve cautiously with a min-
imum amount of (1+1) HNO3. Add 10.0 mL
cone. HNO3 and dilute to 1,000 mL with de-
ionized, distilled water.
7.3.9 Chromium solution, stock, 1 mL=100 \ig
Cr: Dissolve 0.1923 g of CrOj in deionized, dis-
tilled water. When solution is complete,
acidify with 10 mL cone. HNO3 and dilute to
1,000 mL with deionized, distilled water.
7.3.10 Cobalt solution, stock, 1 niL=100 jig-
Co: Dissolve 0.1000 g of cobalt metal in a
minimum amount of (1+1) HNO3. Add 10.0 mL
(1+1) HC1 and dilute to 1,000 mL with deion-
ized, distilled water.
7.3.11 Copper solution, stock, 1 mL=100 UK
Cu: Dissolve 0.1252 g CuO in a minimum
amount of (1+1) HNO3. Add 10.0 mL cone.
HNO3 and dilute to 1,000 mL with deionized,
distilled water.
7.3.12 Iron solution, stock, 1 mL=100 ng Pe:
Dissolve 0.1430 g Fe2O3 in a warm mixture of
20 mL (1+1) HC1 and 2 mL of cone. HNO3.
Cool, add an additional 5 mL of cone. HNO3
and dilute to 1,000 mL with deionized, dis-
tilled water.
7.3.13 Lead solution, stock, 1 mL=100 (ig Pb:
Dissolve 0.1599 g Pb(NO.i)j in a minimum
amount of (1+1) HNO3. Add 10.0 mL cone.
HNO3 and dilute to 1,000 mL with deionized,
distilled water.
7.3.14 Magnesium solution, stock, 1 mL=100
Hg Mg: Dissolve 0.1658 g MgO in a minimum
amount of (1+1) HNOj. Add 10.0 mL cone.
HNO3 and dilute to 1,000 mL with deionized,
distilled water.
7.3.15 Manganese solution, stock, 1 mL=100
ug Mn: Dissolve 0.1000 g of manganese metal
in the acid mixture 10 mL cone. HC1 and 1
mL eonc. HNO3. and dilute to 1,000 mL with
deionized, distilled water.
7.3.16 Molybdenum solution, stock, 1 mL=100
Hg Mo: Dissolve 0.2043 g (NHO; Mod, in deion-
ized, distilled water and dilute to 1,000 mL.
7.3.17 Nickel solution, stock, 1 mL=100 \ig
Ml: Dissolve 0.1000 g of nickel metal in 10 mL
hot cone. HNO3i cool and dilute to 1,000 mL
with deionized, distilled water.
7.3.18 Potassium solution, stock, 1 mL=100
MS K: Dissolve 0.1907 g KC1, dried at 110 °C, in
deionized, distilled water and dilute to 1,000
mL.
7.3.19 Selenium solution, stock, 1 mL=100 ng
Se: Do not dry. Dissolve 0.1727 g H2SeO3 (ac-
tual assay 94.6%) in deionized, distilled water
and dilute to 1,000 mL.
7.3.20 Silica solution, stock, 1 mL=100 us
SiO2s Do not dry. Dissolve 0.4730 g
Na2SiO3-9H2O in deionized, distilled water.
Add 10.0 mL cone. HNO3 and dilute to 1,000
mL with deionized, distilled water,
7.3.21 Silver solution, stock, 1 mL=100 jig
Ag: Dissolve 0.1575 g AgNOj in 100 mL of de-
ionized, distilled water and 10 mL cone.
HNO3. Dilute to 1,000 mL with deionized, dis-
tilled water.
7.3.22 Sodium solution, stock, 1 mL=100 ug
Na: Dissolve 0.2542 g NaCl in deionized, dis-
tilled water. Add 10.0 mL cone. HNO3 and di-
lute to 1,000 mL with deionized, distilled
water.
7.3.23 Thallium solution, stock, 1 mL=100 \ig
Tl; Dissolve 0.1303 g T1NO3 in deionized, dis-
tilled water. Add 10.0 mL cone. HNO3 and di-
lute to 1,000 mL with deionized, distilled
water.
7.3.24 Vanadium solution, stock, 1 mL=100
ug V: Dissolve 0.2297 NHj VO3 in a minimum
amount of cone. HNO3. Heat to increase rate
of dissolution. Add 10.0 mL cone. HNO3 and
dilute to 1,000 mL with deionized, distilled
water.
7.3.25 Zinc solution, stock, 1 mL=100 jig Zn:
Dissolve 0,1245 g ZnO in a minimum amount
of dilute HNO3. Add 10.0 mL cone. HNO3 and
dilute to 1,000 mL deionized, distilled water.
7.4 Mixed calibration standard solutions—
Prepare mixed calibration standard solu-
tions by combining appropriate volumes of
the stock solutions in volumetric flasks.
(See 7.4.1 thru 7.4.5) Add 2 mL of (1+1) HNO3
and 10 mL of (1+1) HC1 and dilute to 100 mL
with deionized, distilled water. (See Notes 1
and 6.) Prior to preparing the mixed stand-
ards, each stock solution should be analyzed
separately to determine possible spectral in-
terference or the presence of impurities.
Care should be taken when preparing the
325
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Pt. 136, App. C
40 CFR Ch. I (7-1-04 Edition)
mixed standards that the elemelts are com-
patible and stable. Transfer the mixed stand-
ard solutions to a PEP fluorooarbon or un-
used polyethylene bottle for storage. Fresh
mixed standards should be prepared as need-
ed with the realization that concentration
can change on aging. Calibration standards
must be initially verified using a quality
control sample and monitored weekly for
stability (See 7.6.3). Although not specifi-
cally required, some typical calibration
standard combinations follow when using
those specific wavelengths listed in Table 1.
7.4.1 Mixed standard solution /—Man-
ganese, beryllium, cadmium, lead, and zinc.
7.4.2 Mixed standard solution II—Barium,
copper, iron, vanadium, and cobalt.
7.4.3 Mixed standard solution III—Molyb-
denum, silica, arsenic, and selenium.
7.4.4 Mixed standard solution IV—Calcium,
sodium, potassium, aluminum, chromium
and nickel.
7.4.5 Mixed standard solution V— Anti-
mony, boron, magnesium, silver, and thal-
lium.
NOTE: 1. If the addition of silver to the rec-
ommended acid combination results in an
Initial precipitation, add 15 mL of deionized
distilled water and warm the flask until the
solution clears. Cool and dilute to 100 mL
with deionized, distilled water. For this acid
combination the silver concentration should
be limited to 2 mg/L. Silver under these con-
ditions is stable in a tap water matrix for 30
days. Higher concentrations of silver require
additional HC1.
7.5 Two types of blanks are required for
the analysis. The calibration blank (3.13) is
used In establishing the analytical curve
while the reagent blank (3.12) IB used to cor-
rect for possible contamination resulting
from varying amounts of the acids used in
the sample processing.
7,5.1 The calibration blank is prepared by
diluting 2 mL of (1+1) HNO3 and 10 mL of
(1+1) HC1 to 100 mL with deionized, distilled
water. (See Note 6.) Prepare a sufficient
quantity to be used to flush the system be-
tween standards and samples.
7.5.2 The reagent blank must contain all
the reagents and in the same volumes as
used in the processing of the samples. The
reagent blank must be carried through the
complete procedure and contain the same
acid concentration In the final solution as
the sample solution used for analysis.
7.6 In addition to the calibration stand-
ards, an instrument check standard (3.7), an
interference check sample (3.8) and a quality
control sample (3.9) are also required for the
analyses.
7.6.1 The instrument check standard is pre-
pared by the analyst by combining compat-
ible elements at a concentration equivalent
to the midpoint of their respective calibra-
tion curves. (See 12.1.1.)
7.6.2 The interference check sample is pre-
pared by the analyst In the following man-
ner. Select a representative sample which
contains minimal concentrations of the
analytes of interest but known concentra-
tion of interfering elements that will provide
an adequate test of the correction factors.
Spike the sample with the elements of Inter-
est at the approximate concentration of ei-
ther 100 ug/L or 5 times the estimated detec-
tion limits given in Table 1. (For effluent
samples of expected high concentrations,
spike at an appropriate level.) If the type of
samples analyzed are varied, a synthetically
prepared sample may be used if the above
criteria and intent are met.
7.6.3 The Quality control sample should be
prepared in the same acid matrix as the cali-
bration standards at a concentration near 1
mg/L and in accordance with the instruc-
tions provided by the supplier. The Quality
Assurance Branch of EMSL-Cincinnati will
either supply a quality control sample or in-
formation where one of equal quality can be
procured. (See 12.1.3.)
8. Sample Handling and Preservation
8,1 For the determination of trace ele-
ments, contamination and loss are of prime
concern. Dust in the laboratory environ-
ment, impurities in reagents and impurities
on laboratory apparatus which the sample
contacts are all sources of potential con-
tamination. Sample containers can intro-
duce either positive or negative errors in the
measurement of trace elements by (a) con-
tributing contaminants through leaching or
surface desorption and (b) by depleting con-
centrations through adsorption. Thus the
collection and treatment of the sample prior
to analysis requires particular attention.
Laboratory glassware including the sample
bottle (whether polyethylene, polyproplyene
or FBP-fluorocarbon) should be thoroughly
washed with detergent and tap water; rinsed
with (1+1) nitric acid, tap water, (1+1) hydro-
chloric acid, tap and finally deionized, dis-
tilled water in that order (See Notes 2 and 3),
NOTE: 2. Chromic acid may be useful to re-
move organic deposits from glassware; how-
ever, the analyst should be cautioned that
the glassware must be thoroughly rinsed
with water to remove the last traces of chro-
mium. This is especially important if
chromium Is to be included in the analytical
scheme. A commercial product,
NOCHBOMIX, available from Godax Labora-
tories, 6 Varick St., New York, NY 10013,
may be used in place of chromic acid. Chro-
mic acid should not be used with plastic bot-
tles.
NOTE: 3. If it can be documented through
an active analytical quality control program
using spiked samples and reagent blanks,
that certain steps in the cleaning procedure
are not required for routine samples, those
steps may be eliminated from the procedure.
326
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Environmental Protection Agency
Pt. 136, App. C
8.2 Before collection of the sample a deci-
sion must be made as to the type of data de-
sired, tliat is dissolved, suspended or total,
so that the appropriate preservation and
pretreatment steps may be accomplished.
Filtration, acid preservation, etc., are to be
performed at the time the sample is col-
lected or as soon as possible thereafter.
8.2.1 For the determination of dissolved
elements the sample must be filtered
through a 0,45-jim membrane filter as soon as
practical after collection. (Glass or plastic
filtering apparatus are recommended to
avoid possible contamination.) Use the first
50-100 mL to rinse the filter flask. Discard
this portion and collect the required volume
of filtrate. Acidify the filtrate with (1+1)
HNO.i to a pH of 2 or less. Normally, 3 mL of
(1+1) acid per liter should be sufficient to
preserve the sample.
8.2.2 For the determination of suspended
elements a measured volume of unpreserved
sample must be filtered through a 0.45-nm
membrane filter as soon as practical after
collection. The filter plus suspended mate-
rial should be transferred to a suitable con-
tainer for storage and/or shipment. No pre-
servative is required.
8.2.3 For the determination of total or
total recoverable elements, the sample is
acidified with (1+1) HNO3 to pH 2 or less as
soon as possible, preferably at the time of
collection. The sample is not filtered before
processing.
9. Sample Preparation
9.1 For the determinations of dissolved
elements, the filtered, preserved sample may
often be analyzed as received. The acid ma-
trix and concentration of the samples and
calibration standards must be the same, (See
Note 6.) If a precipitate formed upon acidifi-
cation of the sample or during transit or
storage, it must be redissolved before the
analysis by adding additional acid and/or by
heat as described in 9.3.
9.2 For the determination of suspended
elements, transfer the membrane filter con-
taining the insoluble material to a 150-mL
G-riffin beater and add 4 mL cone. HNO.i.
Cover the beaker with a watch glass and
heat gently. The warm acid will soon dis-
solve the membrane. Increase the tempera-
ture of the hot plate and digest the material.
When the acid has nearly evaporated, cool
the beaker and watch glass and add another
3 mL of cone. HNO.i. Cover and continue
heating until the digestion is complete, gen-
erally indicated by a light colored digestate.
Evaporate to near dryness (2 mL), cool, and
10 mL HC1 (1+1) and 15 mL deionized, dis-
tilled water per 100 mL dilution and warm
the beaker gently for 15 min. to dissolve any
precipitated or residue material. Allow to
cool, wash down the watch glass and beater
walls with deionized distilled water and fil-
ter the sample to remove insoluble material
that could clog the nebulizer. (See Note 4.)
Adjust the volume based on the expected
concentrations of elements present. This vol-
ume will vary depending on the elements to
be determined (See Note 6). The sample is
now ready for analysis. Concentrations so
determined shall be reported as "suspended."
NOTE: 4. In place of filtering, the sample
after diluting and mixing may be centrifuged
or allowed to settle by gravity overnight to
remove insoluble material. .
9.3 For the determination of total ele-
ments, choose a measured volume of the well
mixed acid preserved sample appropriate for
the expected level of elements and transfer
to a Griffin beaker. (See Note 5.) Add 3 mL
of cone. HNOj. Place the beaker on a hot
plate and evaporate to near dryness cau-
tiously, making certain that the sample does
not boil and that no area of the bottom of
the beaker is allowed to go dry. Cool the
beaker and add another 5 mL portion of
cone. HNOj. Cover the beaker with a watch
glass and return to the hot plate. Increase
the temperature of the hot plate so that a
gently reflux action occurs. Continue heat-
ing, adding additional acid as necessary,
until the digestion is complete (generally in-
dicated when the digestate is light in color
or does not change in appearance with con-
tinued refluxing.) Again, evaporate to near
dryness and cool the beaker. Add 10 mL of
1+1 HC1 and 15 mL of deionized, distilled
water per 100 mL of final solution and warm
the beaker gently for 15 min. to dissolve any
precipitate or residue resulting from evapo-
ration. Allow to cool, wash down the beaker
walls and watch glass with deionized dis-
tilled water and filter the sample to remove
insoluble material that could clog the
nebulizer. (See Note 4.) Adjust the sample to
a predetermined volume based on the ex-
pected concentrations of elements present.
The sample is now ready for analysis (See
Note 6). Concentrations so determined shall
be reported as "total."
NOTE: 5. If low determinations of boron are
critical, quartz glassware should be used,
NOTE: 6. If the sample analysis solution has
a different acid concentration from that
given in 9.4, but does not introduce a phys-
ical interference or affect the analytical re-
sult, the same calibration standards may be
used.
9.4 For the determination of total recov-
erable elements, choose a measured volume
of a well mixed, acid preserved sample appro-
priate for the expected level of elements and
transfer to a Griffin beaker. (See Note 5.)
Add 2 mL of (1+1) HNO3 and 10 mL of (1+1)
HC1 to the sample and heat on a steam bath
or hot plate until the volume has been re-
duced to near 25 mL making certain the sam-
ple does not boil. After this treatment, cool
the sample and filter to remove insoluble
material that could clog the nebulizer. (See
Note 4.) Adjust the volume to 100 mL and
327
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Pf. 136, App. C
40 CFR Ch.! (7-1-04 Edition)
mix. The sample is now ready for analysis.
Concentrations so determined shall be re-
ported as "total."
10. Procedure
10.1 Set up instrument with proper oper-
ating1 parameters established in Section 6.2.
The instrument must be allowed to become
thermally stable before beginning. This usu-
ally requires at least 30 min. of operation
prior to calibration.
10.2 Initiate appropriate operating con-
figuration of computer.
10.3 Profile and calibrate Instrument ac-
cording to instrument manufacturer's rec-
ommended procedures, using the typical
mixed calibration standard solutions de-
scribed in Section 7.4. Flush the system with
the calibration blank (7.5.1) between each
standard. (See Note 7.) (The use of the aver-
age Intensity of multiple exposures for both
standardization and sample analysis has
been found to reduce random error.)
NOTE: 7. For boron concentrations greater
than 500 jtg/L extended flash times of 1 to 2
minutes may be required.
10.4 Before beginning the sample run, re-
analyze the highest mixed calibration stand-
ard as if it were a sample. Concentration val-
ues obtained should not deviate from the ac-
tual values by more than ±5 percent (or the
established control limits whichever is
lower). If they do, follow the recommenda-
tions of the instrument manufacturer to cor-
rect for this condition.
10.5 Begin the sample run flushing the
system with the calibration blank solution
(7.5.1) between each sample. (See Note 7.)
Analyze the instrument check standard
(7.6.1) and the calibration blank (7.5.1) each
10 samples.
10.6 If It has been found that methods of
standard addition are required, the following
procedure Is recommended,
10,6.1 The standard addition technique
(14.2) involves preparing new standards in
the sample matrix by adding known amounts
of standard to one or more aliquots of the
processed sample solution. This technique
compensates for a sample constitutent that
enhances or depresses the analyte signal
thus producing a different slope from that of
the calibration standards. It will not correct
for additive interference which causes a
baseline shift. The simplest version of this
technique is the single-addition method. The
procedure is as follows. Two identical
aliquots of the sample solution, each of vol-
ume Vx, are taken. To the first (labeled A) is
added a small volume V, of a standard
analyte solution of concentration c,. To the
second (labeled B) is added the same volume
V, of the solvent. The analytical signals of A
and B are measured and corrected for
nonanalyte signals. The unknown sample
concentration ex is calculated:
SBV8cs
where SA and SB are the analytical signals
(corrected for the blank) of solutions A and
B, respectively. Vs and c, should be chosen so
that SA Is roughly twice SB on the average.
It is best If Vs is made much less than Vx,
and thus c« is much greater than cx, to avoid
excess dilution of the sample matrix. If a
separation or concentration step is used, the
additions are best made first and carried
through the entire procedure. For the results
from this technique to be valid, the following
limitations must be taken Into consider-
ation:
1, The analytical curve must be linear.
2. The chemical form of the analyte added
must respond the same as the analyte in the
sample.
3, The interference effect must be constant
over the working range of concern.
4, The signal must be corrected for any ad-
ditive Interference.
11. Calculation
11.1 Reagent blanks (7.5.2) should be sub-
tracted from all samples. This is particularly
important for digested samples requiring
large quantities of acids to complete the di-
gestion.
11.2 If dilutions were performed, the ap-
propriate factor must be applied to sample
values.
11.3 Data should be rounded to the thou-
sandth place and all results should be re-
ported in mg/L up to three significant fig-
ures.
12. Quality Control (Instrumental)
12.1 Check the instrument standardiza-
tion by analyzing appropriate quality con-
trol check standards as follow:
12.1.1 Analyze and appropriate instrument
check standard (7.6.1) containing the ele-
ments of interest at a frequency of 10%. This
check standard is used to determine instru-
ment drift. If agreement is not within ±5% of
the expected values or within the established
control limits, whichever is lower, the anal-
ysis is out of control. The analysis should be
terminated, the problem corrected, and the
instrument recalibrated.
Analyze the calibration blank (7.5,1) at a
frequency of 10%. The result should be with-
in the established control limits of 2 stand-
ard deviations of the meal value. If not, re-
peat the analysis two more times and aver-
age the three results. If the average is not
wihin the control limit, terminate the anal-
ysis, correct the problem and recalibrate the
instrument.
12.1.2 To verify interelement and back-
ground correction factors analyze the inter-
ference check sample (7.6.2) at the beginning,
328
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Environmental Protection Agency
Pt. 136, App. C
end, and at periodic intervals throughout the
sample run. Results should fall within the
established control limits of 1.5 times tie
standard deviation of the mean value. If not,
terminate the analysis, correct the problem
and recalibrate the instrument,
12.1.3 A quality control sample (7.6.3) ob-
tained from an outside source must first be
used for the initial verification of the cali-
bration standards. A fresh dilution of this
sample shall be analyzed every week there-
after to monitor their stability. If the re-
sults are not within ±5% of the true value
listed for the control sample, prepare a new
calibration standard and recalibrate the in-
strument. If this does not correct the prob-
lem, prepare a new stock standard and a new
calibration standard and repeat the calibra-
tion.
13. Precision and Accuracy
13.1 An interlaboratory study of metal
analyses by this method was conducted by
the Quality Assurance Branch (QAB) of the
Environmental Monitoring Systems Labora-
tory—Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of the
twenty-five elements listed in Table 4 were
added to reagent water, surface water, drink-
ing water and three effluents. These samples
were digested by both the total digestion
procedure (9.3) and the total recoverable pro-
cedure (9.4). Results for both digestions for
the twenty-five elements in reagent water
are given in Table 4; results for the other
matrices can be found in Reference 14.10,
14. References
14.1 Winge, R.K., V.J. Peterson, and V.A.
Passel, "Inductively Coupled Plasma-Atomic
Emission Spectroscopy: Prominent Lines,
EPA-600/4-79-017.
14.2 Winefordner, J.D., "Trace Analysis:
Speotroscopic Methods for Elements," Chem-
ical Analysis, Vol. 46, pp. 41-42.
14.3 Handbook for Analytical Quality
Control in Water and Wastewater Labora-
tories, EPA-600/4-79-019.
14.4 Garbarino, J.R. and Taylor, H.E., "An
Inductively-Coupled Plasma Atomic Emis-
sion Spectrometric Method for Routine
Water Quality Testing," Applied Spectros-
copy 33, No. 3 (1979).
14.5 "Methods for Chemical Analysis of
Water and Wastes," EFA-600/4-79-020.
14.6 Annual Book of ASTM Standards,
Part 31.
14.7 "Carcinogens—Working With Carcino-
gens," Department of Health, Education, and
Welfare, Public Health Service, Center for
Disease Control, National Institute for Occu-
pational Safety and Health, Publication No.
77-206, August 1977.
14,8 "OSHA Safety and Health Standards,
General Industry," (29 CPE Part 1910), Occu-
pational Safety and Health Administration,
OSHA 2206, (Revised, January 1976).
14.9 "Safety in Academic Chemistry Lab-
oratories, American Chemical Society Publi-
cation, Committee on Chemical Safety, 3rd
Edition, 1979.
14.10 Maxfield R. and Minak B., "EPA
Method Study 27, Method 200.7 Trace Metals
by ICP," National Technical Information
Service, Order No, PB 85-248-656, November
1983.
TABLE 1—RECOMMENDED WAVELENGTHS 1 AND
ESTIMATED INSTRUMENTAL DETECTION LIMITS
Element
Aluminum
Sarium
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Iron
Lead
Magnesium
Manganese
Molybdenum
Potassium
Silica (SiCM
Silver
Thallium
Zinc
Wave-
length,
nm
308.215
193696
206 833
455.403
313.042
249.773
226.502
317.933
267.716
228.616
324 754
259.940
220.353
279.079
257.610
202.030
231 604
766.491
196026
288 1 58
328.068
588 995
'190.864
292 402
213.856
Estimated
detection
limit, iigIL2
45
53
32
2
0.3
5
4
10
7
7
6
7
42
30
15
75
58
7
29
40
2
1The wavelengths listed are recommended because of their
sensitivity and overall acceptance. Other wavelengths may be
substituted if they can provide the needed sensitivity and are
treated with the same corrective techniques for spectral inter-
ference. (See 5,1.1).
2The estimated instrumental detection limits as shown are
taken from "inductively Coupled Plasma-Atomic Emission
SpecifQscopy-Prominent Lines," EPA-^6QQ/4-79~-017. They
are given as a guide for an instrumental limit. The actual
method detection limits are sample dependent and may vary
as the sample matrix varies.
3Highly dependent on operating conditions and plasma
position.
TABLE 1—ANALYTE CONCENTRATION EQUIVALENTS (MG/L) ARISING FROM INTERFERENTS AT THE 100
MG/L LEVEL
Analyte
Wave-
nm
308.214
Interfe
A1 Ca Cr , Cu : Fe
} I
ent—
Mg
Mn
0.21
Nl I Ti I V
I 1.4
329
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Pt. 136,App. C
40 CFR Ch. i (7-1-04 Edition)
TABLE 1-
-ANALYTE CONCENTRATION EQUIVALENTS (MG/L.) ARISING FROM INTERFERENTS AT THE 100
MG/L LEVEL—Continued
Calcium ,... ,
Cobalt
Nickel
Zinc ......,...,.,.,..... .....,...,
Wave-
nm
206833
193696
455403
313042
249 773
226 502
317,933
267716
228616
324 754
259940
220 353
279079
257610
202030
231 604
196 026
288 158
588995
190864
292.402
213.856
A1
0.47
1 3
004
0.17
0.005
0.05
0.23
0.30
Ca
0.02
Cr
2.9
044
0.08
003
011
0.01
007
0.05
Cu
0.14
tmerfa
Fe
0.08
032
0.03
0.01
0.003
0005
0003
013
0.002
003
0.09
0.005
ent—
Mg
0.01
0.002
Mn
0.04
0.04
0 12
025
Ni
002
003
0.29
Tl
0.25
004
0.03
015
005
007
008
0.02
V
045
1 1
DOS
0.03
0.04
0.02
0 12
001
TABLE 3—INTERFERENT AND ANALYTE ELEMENTAL CONCENTRATIONS USED FOR INTERFERENCE
MEASUREMENTS IN TABLE 2
Analyles
Al
AS
B
Ba
Be
Ca
Cd
Co . .
Cr
Cu
Mn
Mo
Na
Ni
Pb
Sb
Se
Si .
Tt
y
Zn
(mg/L)
10
10
10
1
1
1
10
1
1
1
1
1
1
10
10
10
10
10
10
1
10
1
10
tntefferents
Al
Ca
Cr
Cu
Fe
Mg . . .
Mn
Ni
Ti . ,.
V
(tng/L)
1 000
1,000
200
200
1,000
1 000
200
200
200
200
TABLE 4—ICP PRECISION AND RECOVERY DATA
Analyte
Barium .
Concentration
P9/L
69-4792
77-1406
69-1887
9-377
Total digestion (9.3)
WL
"
X=0 9273(C}+3 6
S=0.0559(X)+18.6
SR=0.0507(X)-t-3.5
X=07940jC)-170
S=0.1556(X)-0.6
SR=0.1081(X)+3.9
X=1 0437(C)-122
8=0.1 239(X)+2.4
SH=0.0874SX)+6.4
X=0.7683(C)+0.47
Recoverable digestion
(9.4) (ig/L
X=0 9380(CJ+22 1
S=Q-0873(X)+31.7
SR=0.0481(X)+18.8
X=0 8908(C)+0 9
S=0.0982(X)+8.3
SR=0.0682(X)+2.5
X-1 0175(C)+3 9
S=0.1288(X)+6.1
Sn=O.G643(Xj+10.3
X=0.8380(C)+1.68
330
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Environmental Protection Agency
Pt. 136, App. C
TABLE 4—ICP PRECISION AND RECOVERY DATA—Continued
Analyte
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium .,,,,
Selenium
Silicon
Silver
Sodium
Thallium
Vanadium
Zinc
Concentration
H9/L
3-1906
19-5189
9-1943
17-47170
13-1406
17-2340
8-1887
13-9359
42-4717
34-13868
4-1887
17-1830
17^*7170
347-14151
69-1415
189-9434
8-189
35-47170
79-1434
13-4698
7-7076
Total digestion (9,3)
S=0.1819(X)4-2.78
SR=0,1285(X)+2.55
X=Q.9629(CS+O.Q5
8=0.0136JXJ+G.95
SR=Q.Q203(X)-0.07
X=0.8807(C)+9.Q
S=0,1150(X)+14_1
SR=0.0742(X)+23.2
X=0.9874(C)-0.18
S=0.557(X)+2.02
SR=0.0300(X)+0.94
X=Q.9182(C)-2.6
S=0.1228(X)+10.1
SR=0.0189(X)+3.7
X=0.9S44(C)4-3.1
S=O.Q499(X}+4.4
SH=0.0009(X)+7.9
X=0.9209(C)-4.5
S=0.0436(X)+3.8
SR=0.0428{X)+0.5
X=Q.9297{C)-0.30
S=0.0442(X)+2.85
SH=0.0128(X)+2.53
X=0.8829(C)+7.0
S=0.0683(X)+11.5
SR=O.Q046(X)+10.0
X=0.9699(C)-2.2
S=0.0558{X)+7.0
SR=0,0353(X)+3.6
X=0.9881(C)-1.1
S=0.0607(C)+11,6
SH=0.0298(X)+0.6
X=0.9417(C)+0.13
S=0,0324(X)+0.88
SR=0.0153(X)+0.91
X=0.9682(C)+0.1
3=0.0618(X)+1.6
SR=0,0371(X)+2.2
X=0,9508(C)+0.4
S=0.0604(X)*4.4
SR=0,0425(X)+3.8
X=0.8669(C)-36i4
S=0,0934(X)+77,8
SR=0,0099(X)+144.2
X=0.9363(C)-2-5
S=0-0855(X)+17.8
SR=0,0284(X)+9.3
X=0.5742(C)-35.6
S=0,4160(X)t37.8
SR=0.1987(X)+8-4
X=0.4466(C!+5-07
S=0.5055(X)-3-05
SR=0.2086(X) -1.74
X=0.9581(C)+39.6
S=0,2097(X)+33.0
SR=0.0280(X)+105.8
X=0-9020(C)-7.3
S=0.1004(X)t18.3
SR=0.0364(X)<-11.5
X=0.9615(C)-2.0
8=0.0618(X)+1.7
SR=0.0220(Xj+0.7
X=0.9356(C)-0.30
S=0.0914(X)+3.75
SR=0.0130(X)*10.7
Recoverable digestion
(9.4! ug/L
S=0.2540(X)+0.30
SR=0.0826(X)+3.54
X=1.0177(0)-0.55
S=0.0359(XJ+0.90
SR=0.0445(X)-0.10
X=0.9676(C)+18.7
S=0.1320(X)+16.0
SR=0.0743(X)4-21.1
X=1.0137(0)-0.65
S=0.0585(X)+1.15
SR=0.332(X)*0.90
X=0.9658
-------
Pt. 136, App. D
40 CFR Ch. I (7-1-04 Edition)
APPENDIX D TO PART 136—PRECISION
AND RECOVERY STATEMENTS FOR
METHODS FOR MEASURING METALS
Twenty-eight selected methods from
"Methods for Chemical Analysis of Water and
Wastes," EPA-600/4-79-020 (1979) have been
subjected to interlaboratory method valida-
tion studies. The following precision and re-
covery statements are presented in this ap-
pendix and incorporated into part 136:
Method 202.1
For Aluminum, Method 202.1 (Atomic Ab-
sorption, Direct Aspiration) replace the Pre-
cision and Accuracy Section with the fol-
lowing':
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the
Environmental Monitoring Systems Labora-
tory—Cincinnati (EMSL-CI). Synthetic
concentrates containing various levels of
this element were added to reagent water
and a natural water or effluent of the ana-
lyst's choice. The digestion procedure was
not specified. Results for the reagent water
are given below. Results for other water
types and study details are found in "USEPA
Method Study 7, Analyses for Trace Methods
in water by Atomic Absorption Speotroscopy
(Direction Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. FB86-208708/AS, Winter, J.A. and
Brlttoir, P.W., June, 1986.
For a concentration range of 500-1200
X=Q,979(C)+6.16
S=0.066(X)+125
SR=0.086(X)+40.5
where:
C=True Value for the Concentration,
X=Mean Recovery, jtg/L
S=Multi-laboratory Standard Deviation, us/
L
SR= Single-analyst Standard Deviation, ug/L
Method 206.4
For Arsenic, Method 206.4
(Spectrophotometrie-SDBC) add the fol-
lowing to the Precision and Accuracy Sec-
tion:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the
Environmental Monitoring Systems Labora-
tory—Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Spectroscopy
(Direct Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-2Q8709/AS, Winter, J.A. and
Britton, P.W., June, 1986.
For a concentration range of 20-292 p,g/L
X=0.850(C)-0.25
S=0.198(X)+5.93
SR=0.122(X)+3.10
where:
C=Trne Value for the Concentration, (ig/L
X=Mean Recovery, jig/L
S=Multi-laboratory Standard Deviation, ug/
L
SR=Single-analyst Standard Deviation, p.g/L
Method 213.1
For Cadmium, Method 213.1 (Atomic Ab-
sorption, Direct Aspiration) replace the Pre-
cision and Accuracy Section with the fol-
lowing:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Spectroscopy
(Direct Aspiration) and Oolorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter, J.A. and
Britton, P.W., June, 1986.
For a concentration range of 14-78 jig/L
X=Q.919(C)+2.97
S=0.108(X)+5.08
SR=0.120(X)+0.89
where:
C=Tme Value for the Concentration, \igfL
X=Mean Recovery, ng/L
S=Multi-laboratory Standard Deviation, jig/
L
SR=Sinfle-analyst Standard Deviation, jig/L
Method 218.1
For Chromium, Method 218.1 (Atomic Ab-
sorption, Direct Aspiration) replace the Pre-
cision and Accuracy Section with the fol-
lowing:
332
-------
Environmental Protection Agency
Pt. 136, App. D
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Speetroscopy
(Direct Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter, J.A. and
Britton, P.W., June 1986.
For a concentration range of 74-407 jigv'L
X=Q.976(C)+3,94
S=0.131(X)+4.26
SR=0.052(X)+3.01
where:
C=True Value for the Concentration, (ig/L
X=Mean Recovery, ng/L
S=MultHaboratory Standard Deviation, |ig/
L
SB=Single-analyst Standard Deviation, (ig/L
Method 220.1
For Copper, Method 220.1 (Atomic Absorp-
tion, Direct Aspiration) replace the Preci-
sion and Accuracy Section witli the fol-
lowing:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI), Synthetic con-
centrates containing- yarious levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Speotroscopy
(Direct Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter, J.A. and
Britton, P.W., June, 1986.
For concentration range 60-332 |ig/L
X=0.963(C)+3.49
S=Q,047(X)+12.3
SR=0,042(X)+4.60
where:
C=True Value for the Concentration,
X=Mean Recovery, (ig/L
S=Multi-laboratory Standard Deviation, jig/
L
SR=Singrle-analyst Standard Deviation, ng/L
Method 236.1
For Iron, Method 236.1 (Atomic Absorption,
Direct Aspiration) replace the Precision and
Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI), Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trade Methods in
Water by Atomic Absorption Spectroscopy
(Direct Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter, J.A. and
Britton, P.W., June, 1986.
For concentration range 350-840 jig/L
X=Q.999(C)-2.21
S=0.022(X)+41.0
SR=0,019(X)+21.2
where:
C=True Value for the Concentration, ng/L
X=Mean Recovery, (igv'L
S=Multi-Laboratory Standard Deviation, |ig/
L
SR=Sinirle-analyst Standard Deviation, pg/L
Method 239.1
For Lead, Method 239.1 (Atomic Absorp-
tion, Direct Aspiration) replace Precision
and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice, The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7 Analyses for Trace Methods in
Water by Atomic Absorption Speetroscopy
(Direct Aspiration) and Colorimetry*; Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter. J.A. and
Britton, P.W., June, 1986.
333
-------
Pt. 136, App. D
40 CFR Ch. I (7-1-04 Edition)
For concentration range of 84-367 jig/L
X=0.961(C)+13.8
S=0.028(C)+33.9
SR=0,011(X)+16,1
where:
C=True Value for the Concentration, ng/L
X=Mean Recovery, ug/L
S=Multi-laboratory Standard Deviation, ng/
L
SR=Single-analyst Standard Deviation, ng/L
Method 243.1
For Manganese, Method 243.1 (Atomic Ab-
sorption, Direct Aspiration) replace Preci-
sion and Accuracy Section with the fol-
lowing:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are found in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Spectroscopy
(Direct Aspiration) and Colorlmetry", Na-
tional Technical Information Service, 5285
Port Eoyal Road, Springfield, VA 22161,
Order No. PB86-2Q8709/AS, Winter, J.A. and
Britton, P.W., June, 1986.
Por concentration range 84-^469 |ig/L
X=0.987(C)-1.27
S=0.042(X)+8.95
SR=0.023(X)+4.90
where:
C=Trae Value for tie Concentration, ng/L
X=Mean Recovery, (ig/L
S=Multi-laboratory Standard Deviation, (ig/
L
SR=Single-analyst Standard Deviation, p.g/L
Method 289.1
For Zinc, Method 289.1 (Atomic Absorp-
tion, Direct Aspiration) replace the Preci-
sion and Accuracy Section with the fol-
lowing:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water and a
natural water or effluent of the analyst's
choice. The digestion procedure was not
specified. Results for the reagent water are
given below. Results for other water types
and study details are fonnd in "USEPA Meth-
od Study 7, Analyses for Trace Methods in
Water by Atomic Absorption Spectroscopy
(Direct Aspiration) and Colorimetry", Na-
tional Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB86-208709/AS, Winter, J. A. and
Britton, P. W., June, 1986.
Por concentration range 56-310 ug/L
X=0.999(C)+0.033
S=0.078(X)+10.8
SR=0.049(X)+1.10
where:
C=True Value for the Concentration, ug/L
X=Mean Recovery, ug/L
S=Multi-laboratory Standard Deviation,
SR=Single-analyst Standard Deviation, p.g/
L
Method 202.2
Por Aluminum, Method 202.2 (Atomic Ab-
sorption, Furnace Technique) replace the
Precision and Accuracy Section statement
with the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (BMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques), "National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161, Order No. PB 86-121
704/AS, by Copeland, P.R. and Maney, J.P.,
January 1986.
Por a concentration range of 0.46- 125 (ig/L
X=l. 1579(0-0.121
S=0.4286(X)~ 0.124
SR=0.2908(X)- 0.082
where:
C=True Value for the Concentration, ug/L
X=Mean Recovery, ng/L
S=Multi-laboratory Standard Deviation, [ig/
L
SR=Single-analyst Standard Deviation, (ig/L
Method 204.2
Por Antimony, Method 204.2 (Atomic Ab-
sorption, Furnace Technique) replace the
Precision and Accuracy Section statement
with the following:
334
-------
Environmental Protection Agency
Pt. 136, App, D
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4,1.3 in this manual as
modified by this method. Results for the rea-
gent water are given below. Results for other
water types and study details are found in
"EPA Method Study 31, Trace Metals by
Atomic Absorption (Furnace Techniques)."
National Technical Information Service, 5285
Port Royal Road, Springfield, VA 22161,
Order No. PB 86-121 704/AS, by Copeland, F.R.
and Maney, J.P., January 1986.
For a concentration range of 10.60-240 jig/L
X=0.7219(C)- 0.986
S=0.3732(X)+0.854
SR=0.1874(X)-0.461
where:
C=True Value for the Concentration, jig/L
X=Mean Recovery, ug/L
S=Multi-laboratory standard Deviation, jjg;
L
SR=Single-analyst Standard Deviation, ug/L
Method 206.2
For Arsenic, Method 206,2 (Atomic Absorp-
tion, Furnace Technique) add the following
to tie existing Precision and Accuracy state-
ment:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring- Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
Results for the reagent water are given
below. Results for other water types and
study details are found in "EPA Method
Study 31, Trace Metals by Atomic Absorp-
tion (Furnace Techniques)," National Tech-
nical Information Service, 5285 Port Royal
Road, Springfield, VA 22161, Order No. PB 86-
121 704/AS, by Copeland, F.R. and Maney,
J.P., January 1986.
For a concentration range of 9.78-237 ug/L
X=0.9652(C)+2.112
S=Q.1411(X)+1.873
SR=Q.Q484(X)+2.1B9
where:
C=True Value for the Concentration, ng/L
X=Mean Recovery, M-g/L
S=Multi-laboratory Standard Deviation, \igl
L
SR= Single-analyst Standard Deviation, (ig/L
Method 203.2
For Barium, Method 208.2 (Atomic Absorp-
tion, Furnace Technique) add the following
to the existing Precision and Accuracy infor-
mation:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161, Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 56.50-437 p.g/'L
X=Q.8268(C)+S9.459
S=0.2466(X)+6.436
SB=0.1393(X)-0.428
where:
C=True Value for the Concentration, \igfli
X=Mean Recovery, |ig/L
S=MultHaboratory Standard Deviation, \tgl
L
SR=Single-analyst Standard Deviation, jig/L
Method 210.2
For Beryllium, Method 210.2 (Atomic Ab-
sorption, Furnace Technique) replace the ex-
isting Precision and Accuracy statement
with the following;
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road.
Springfield, VA 22161, Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
335
-------
Pt. 136, App. D
40 CFR Ch. I (7-1-04 Edition)
For a concentration range of 0.45-11.4 jig/L
X=1.0682(O-0.158
S=0.2167(X)+0,090
SR=0.1Q96(X)+0.061
where:
C=True Value for the Concentration, (tg/L
X=Mean Recovery, ug/L
S=Multi-laboratory Standard Deviation, n§/
L
SR=Single-analyst Standard Deviation, ng/L
Method 213,2
For Cadmium, Method 213.2 (Atomic Ab-
sorption, Furnace Technique) add the fol-
lowing to the existing Precision and Accu-
racy information:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring System Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161, Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 0.43-12.5
X=0.9826(C)+0.171
S=0.230Q(X)+O.Q45
SR=0.1031(X)+0.116
where:
C=True Value for the Concentration,
X=Mean Recovery, jig/L
S=Multi-lal)oratory Standard Deviation, ng/
L
SR=Single-analyst Standard Devision, |ig/L
Method 218.2
For Chromium, Method 218.2 (Atomic Ab-
sorption, Furnace Technique) add the fol-
lowing to the existing Precision and Accu-
racy Section:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (BMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161, Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 9.87-246 ng/L
X=0.9120(C)+0.234
S=0.1684(X)+0.852
SR=0,1469(X)+0,315
where:
C=True Value for the Concentration, ng/L
X=Mean Recovery, ftg/L
S=Multi-laboratory Standard Deviation, jig/
L
SR=Single-analyst Standard Devision, jig/L
Method 219.2
For Cobalt, Method 219.2 (Atomic Absorp-
tion, Furnace Technique), replace the Preci-
sion and Accuracy Section statement with
the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
salts for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 704/
AS, by Copeland, F.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 21.10—461 jig/L
X=0.8875(C)+0.859
S=0.24B1(X)-2.541
SR=0.0969(X)+0.134
where:
O=True Value for the Concentration, pg/L
X=Mean Recovery, p.g/L
S=Multi-laboratory Standard Deviation, ng/
L
SR=Single-analyst Standard Deviation, ng/
L
Method 220,2
For Copper, Method 220.2 (Atomic Absorp-
tion, Furnace Technique) replace the Preci-
sion and Accuracy Section statement with
the following:
336
-------
Environmental Protection Agency
Pt. 136, App. D
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI), Synthetic con-
centrates containing various levels of this
element were added to reagrent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4,1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22181 Order No. PB 86-121 704/
AS, by Copeland, P.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 0.30 — 245 ^.g/T-i
X=0,9253(C)+0.01Q
S=0.2735(X)- 0.058
SR=0.2197(X)-0.050
where:
C=True Value for the Concentration. jig/L
X=Mean Recovery, ^g/L
S=Multi-laboratory Standard Deviation, ug/
L
SR=Single-analyst Standard Deviation, m?/
L
Method 236.2
For Iron, Method 236.2 (Atomic Absorption,
Furnace Technique) replace the Precision
and Accuracy Section statement with the
following:
Precision and Accuracy
An iaterlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (BMSL-OI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 70*'
AS, by Copeland, P.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 0.37 — 455 (igv'L
X=1.«94(C)-0.229
S=0.3611(X)- 0.079
SB=0.3715(X)- 0.161
where:
C=True Value for the Concentration, (ig/L
X=Mean Recovery, jtg/L
S=Multi-laboratory Standard Deviation, jig!
L
SR=Single-analyst Standard Deviation, fig/
L
Method 239.2
For Lead, Method 239.2 (Atomic Absorp-
tion, Furnace Technique) add the following
to the existing Precisions and Accuracy Sec-
tion:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 704,'
AS, by Oopeland, F.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 10.40-254 (ig/L
X=0.9430(O-0.504
S=0.2224(X)+0.507
SR=0.1931(X)-0.378
where:
C=True Value for the Concentration, jig/L
X=Mean Recovery, ng/L
S=Multi-laboratory Standard Deviation, ng/
L,
SR=Single-analyst Standard Deviation, UK/
L
Method 243.2
For Manganese, Method 243.2 (Atomic Ab-
sorption, Furnace Technique) replace the
Precision and Accuracy Section statement
with the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL—CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
337
-------
Pt. 136, App. D
40 CFR Ch. I (7-1-04 Idfflon)
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Spring-field, VA 22161. Order No. PB 86-121
7Q4/AS, by Copeland, F.R, and Maney, J.P.,
January 1986.
For a concentration range of 0.42-666 ng/L
X=1.048Q(C)+1.404
S=0.2001(X)+1.042
SR=0.1333(X)-K>.680
where:
C=Trae Value for the Concentration, |ig/L
X=Mean Recovery, ng/L
S=Mnlti-laboratory Standard Deviation, jig/
L
SR=Single-analyst Standard Deviation, |ig/L
Method 249.2
For Nickel, Method 249.2 (Atomic Absorp-
tion, Furnace Technique) replace the Preci-
sion and Accuracy Section statement with
the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL—CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161. Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 26.20-482 iigfL
X=0.8812(C)+2.426
S=0.2475(X)+1.896
SR=0.1935(X)+1.315
where:
C=Trne Value for the Concentration, (ig/L
X=Mean Recovery, \igfli
S=Multi-laboratory Standard Deviation, \igl
L
SR=Single-analyst Standard Deviation, (ig/L
Method 270.2
For Selenium, Method 270.2 (Atomic Ab-
sorption, Furnace Technique) add the fol-
lowing to the existing Precision and Accu-
racy Section:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (EMSL—CI). Synthetic con-
centrates coataining various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
Results for the reagent water are given
below. Results for other water types and
study details are found in "EPA Method
Study 31, Trace Metals by Atomic Absorp-
tion (Furnace Techniques)," National Tech-
nical Information Service, 5285 Port Royal
Road, Springfield, VA 22161. Order No. PB 86-
121 704/AS, by Copeland, F.R. and Maney,
J.P., January 1986.
For a concentration range of 10.00-246 (ig/L
X=0.9564(C)+0.476
S=0.1584(X)+0.878
SR=0,0772(X)+0.547
where:
C=True Value for the Concentration, ttg/L
X=Mean Recovery, (ig/L
S=Multi-laboratory Standard Deviation, \igl
L
SB=Single-analyst Standard Deviation, (ig/L
Method 272.2
For Silver, Method 272.2 (Atomic Absorp-
tion, Furnace Technique) add the following
to the existing Precision and Accuracy Sec-
tion:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory—
Cincinnati (BMSL—CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161. Order No. PB 86-121
704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 0.45-56.5
X=0.9470(C)+0.181
S=0,1805(X)+0,153
SR=0.1417(X)+0.039
where:
C=True Value for the Concentration,
X=Mean Recovery, jig/L
S=Multi-laboratory Standard Deviation, \igi
L
SR=Single-analyst Standard Deviation,
338
-------
Environmental Protection Agency
Pt. 140
Method 279.2
For Thalliu, Method 279,2 (Atomic Absorp-
tion, Furnace Technique) replace the Preci-
sion and Accuracy Section statement with
tie following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-GI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents,
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 704/
AS, by Copeland, F.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 10,00-252 ng/L.
X=0.8781(0)- 0.715
S=0.1112(X)+0.669
SR=0.1005(X)+0.241
where:
C=True Value for the Concentration, |ig/L
X=Meaa Recovery, jig/L
S=Multi-laboratory Standard Deviation, \tgl
L
SR=Single-analyst Standard Deviation, |ig/L
Method 286,2
For Vanadium, Method 286.2 (Atomic Ab-
sorption, Furnace Technique) replace the
Precision and Accuracy Section statement
with the following:
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI), Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 5285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 7Q4/
AS, by Copeland, F.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 1,36-982 jigfL.
X=0.8486(C)+0.252
S=0.3323(X)-0.428
SE=0.1195(X) - 0.121
where:
C=Trae Value for the Concentration, jig/L
X=Mean Recovery, (ig/L
S=Multi-laboratory Standard Deviation, us/
L
SR=Singrle-analyst Standard Deviation, (ig/
L
Method 289.2
For Zinc, Method 289.2 (Atomic Absorp-
tion, Furnace Technique) replace the Preci-
sion and Accuracy Section statement with
the following':
Precision and Accuracy
An interlaboratory study on metal anal-
yses by this method was conducted by the
Quality Assurance Branch (QAB) of the Envi-
ronmental Monitoring Systems Laboratory-
Cincinnati (EMSL-CI). Synthetic con-
centrates containing various levels of this
element were added to reagent water, surface
water, drinking water and three effluents.
These samples were digested by the total di-
gestion procedure, 4.1.3 in this manual. Re-
sults for the reagent water are given below.
Results for other water types and study de-
tails are found in "EPA Method Study 31,
Trace Metals by Atomic Absorption (Fur-
nace Techniques)," National Technical Infor-
mation Service, 8285 Port Royal Road,
Springfield, VA 22161 Order No. PB 86-121 70*'
AS, by Copeland, F.R. and Maney, J.P., Jan-
uary 1986.
For a concentration range of 0.51-189 jig/L.
X=1,8710(C)+1,485
S=0.6740(X)-0.342
SR=0.3895(X)- 0.384
where:
C=True Value for the Concentration, |ig/L
X=Mean Recovery, ng/L
S=Mnlti-laboratory Standard Deviation, jig/
L
SR=Single-analyst Standard Deviation, ng/
L
[55 FR 33442, Aug. 15, 1990]
PART 140—MARINE SANITATION
DEVICE STANDARD
Sec.
140.1 Definitions.
140,2 Scope of standard,
140.3 Standard,
140,4 Complete prohibition.
140.5 Analytical procedures.
AUTHORITY: 33 U.S.C. 1322, as amended.
SOURCE: 41 FR 4453, Jan. 29, 1976, unless
otherwise noted.
339
-------
§140.1
40 CFR Ch. I (7-1-04 Edition)
§ 140.1 Definitions.
For the purpose of these standards
the following definitions shall apply:
(a) Sewage means human body wastes
and the wastes from toilets and other
receptacles intended to receive or re-
tain body wastes;
(b) Discharge includes, but is not lim-
ited to, any spilling, leaking, pumping,
pouring, emitting, emptying, or dump-
ing;
(c) Marine sanitation device includes
any equipment for installation onboard
a vessel and which is designed to re-
ceive, retain, treat, or discharge sew-
age and any process to treat such sew-
age;
(d) Vessel includes every description
of watercraft or other artificial con-
trivance used, or capable of being used,
as a means of transportation on waters
of the United States;
(e) New vessel refers to any vessel on
which construction was initiated on or
after January 30,1975;
(f) Existing vessel refers to any vessel
on which construction was initiated be-
fore January 30, 1975;
(g) Fecal coliform bacteria are those
organisms associated with the intes-
tines of warm-blooded animals that are
commonly used to indicate the pres-
ence of fecal material and the potential
presence of organisms capable of caus-
ing human disease,
§ 140.2 Scope of standard.
The standard adopted herein applies
only to vessels on which a marine sani-
tation device has been installed. The
standard does not require the installa-
tion of a marine sanitation device on
any vessel that is not so equipped. The
standard applies to vessels owned and
operated by the United States unless
the Secretary of Defense finds that
compliance would not be in the inter-
est of national security,
§ 140.3 Standard.
(a) (1) In freshwater lakes, freshwater
reservoirs or other freshwater im-
poundments whose inlets or outlets are
such as to prevent the ingress or egress
by vessel traffic subject to this regula-
tion, or in rivers not capable of naviga-
tion by interstate vessel traffic subject
to this regulation, marine sanitation
devices certified by the U.S. Coast
Guard (see 33 CFR part 159, published
in 40 FB 4622, January 30, 1975), in-
stalled on all vessels shall be designed
and operated to prevent the overboard
discharge of sewage, treated or un-
treated, or of any waste derived from
sewage. This shall not be construed to
prohibit the carriage of Coast Guard-
certified flow-through treatment de-
vices which have been secured so as to
prevent such discharges.
(2) In all other waters, Coast Guard-
certified marine sanitation devices in-
stalled on all vessels shall be designed
and operated to either retain, dispose
of, or discharge sewage. If the device
has a discharge, subject to paragraph
(d) of this section, the effluent shall
not have a fecal coliform bacterial
count of greater than 1,000 per 100 mil-
liliters nor visible floating solids. Wa-
ters where a Coast Guard-certified ma-
rine sanitation device permitting dis-
charge is allowed include coastal wa-
ters and estuaries, the Great Lakes and
inter-connected waterways, fresh-water
lakes and impoundments accessible
through locks, and other flowing wa-
ters that are navigable interstate by
vessels subject to this regulation.
(b) This standard shall become effec-
tive on January 30, 1977 for new vessels
and on January 30, 1980 for existing
vessels (or, In the case of vessels owned
and operated by the Department of De-
fense, two years and five years, for new
and existing vessels, respectively, after
promulgation of implementing regula-
tions by the Secretary of Defense under
section 312(d) of the Act).
(c) Any vessel which is equipped as of
the date of promulgation of this regu-
lation with a Coast Guard-certified
flow-through marine sanitation device
meeting the requirements of paragraph
(a)(2) of this section, shall not be re-
quired to comply with the provisions
designed to prevent the overboard dis-
charge of sewage, treated or untreated,
in paragraph (a)(l) of this section, for
the operable life of that device.
(d) After January 30, 1980, subject to
paragraphs (e) and (f) of this section,
marine sanitation devices on all ves-
sels on waters that are not subject to a
prohibition of the overboard discharge
of sewage, treated or untreated, as
specified in paragraph (a)(l) of this sec-
tion, shall be designed and operated to
340
-------
Environmental Protection Agency
§140.4
either retain, dispose of, or discharge
sewage, and shall be certified by the
U.S. Coast Guard. If the device has a
discharge, the effluent shall not have a
fecal coliform bacterial count of great-
er than 200 per 100 milliliters, nor sus-
pended solids greater than 150 mg/1.
(e) Any existing vessel on waters not
subject to a prohibition of the over-
board discharge of sewage in paragraph
(a)(l) of this section, and which is
equipped with a certified device on or
before January 30, 1978, shall not be re-
quired to comply with paragraph (d) of
this section, for the operable life of
that device.
(f) Any new vessel on waters not sub-
ject to the prohibition of the overboard
discharge of sewage in paragraph (a)(l)
of this section, and on which construc-
tion is initiated before January 31,
1980, which is equipped with a marine
sanitation device before January 31,
1980, certified under paragraph (a)(2) of
this section, shall not be required to
comply with paragraph (d) of this sec-
tion, for the operable life of that de-
vice.
(g) The degrees of treatment de-
scribed in paragraphs (a) and (d) of this
section are "appropriate standards" for
purposes of Coast Guard and Depart-
ment of Defense certification pursuant
to section 312(g)(2) of the Act.
141 FR 4453, Jan. 29, 1976, as amended at 60
PR 33932, June 29, 1995]
§ 140.4 Complete prohibition.
(a) Prohibition pursuant to CWA sec-
tion 312(f)(3): a State may completely
prohibit the discharge from all vessels
of any sewage, whether treated or not,
into some or all of the waters within
such State by making a written appli-
cation to the Administrator, Environ-
mental Protection Agency, and by re-
ceiving the Administrator's affirma-
tive determination pursuant to section
312(0(3) of the Act. Upon receipt of an
application under section 312(f)(3) of
the Act, the Administrator will deter-
mine within 90 days whether adequate
facilities for the safe and sanitary re-
moval and treatment of sewage from
all vessels using such waters are rea-
sonably available. Applications made
by States pursuant to section 312(f)(3)
of the Act shall include:
(1) A certification that the protection
and enhancement of the waters de-
scribed in the petition require greater
environmental protection than the ap-
plicable Federal standard;
(2) A map showing the location of
commercial and recreational pump-out
facilities;
(3) A description of the location of
pump-out facilities within waters des-
ignated for no discharge;
(4) The general schedule of operating
hours of the pump-out facilities;
(5) The draught requirements on ves-
sels that may be excluded because of
insufficient water depth adjacent to
the facility;
(6) Information indicating that treat-
ment of wastes from such pump-out fa-
cilities is in conformance with Federal
law, and
(7) Information on vessel population
and vessel usage of the subject waters.
(b) Prohibition pursuant to CWA sec-
tion 312(f)(4)(A): a State may make a
written application to the Adminis-
trator, Environmental Protection
Agency, under section 312(f)(4)(A) of
the Act, for the issuance of a regula-
tion completely prohibiting discharge
from a vessel of any sewage, whether
treated or not, into particular waters
of the United States or specified por-
tions thereof, which waters are located
within the boundaries of such State.
Such application shall specify with
particularly the waters, or portions
thereof, for which a complete prohibi-
tion is desired. The application shall
include identification of water rec-
reational areas, drinking water in-
takes, aquatic sanctuaries, identifiable
fish-spawning and nursery areas, and
areas of intensive boating activities. If,
on the basis of the State's application
and any other information available to
him, the Administrator is unable to
make a finding that the waters listed
in the application require a complete
prohibition of any discharge in the wa-
ters or portions thereof covered by the
application, he shall state the reasons
why he cannot make such a finding,
and shall deny the application. If the
Administrator makes a finding that
the waters listed in the application re-
quire a complete prohibition of any
discharge in all or any part of the wa-
ters or portions thereof covered by the
341
-------
§140.5
40 CFR Ch.J (7-1-04 Edition)
State's application, he shall publish
notice of such findings together with a
notice of proposed rule making, and
then shall proceed in accordance with 5
U.S.O, 553. If the Administrator's find-
ing is that applicable water quality
standards require a complete prohibi-
tion covering a more restricted or more
expanded area than that applied for by
the State, he shall state the reasons
why his finding differs in scope from
that requested in the State's applica-
tion,
(1) For the following waters the dis-
charge from a vessel of any sewage
(whether treated or not) is completely
prohibited pursuant to OWA section
312(f)(4)(A):
(i) Boundary Waters Canoe Area, for-
merly designated as the Superior, Lit-
tle Indian Sioux, and Caribou Roadless
Areas, in the Superior National Forest,
Minnesota, as described in 16 U.S.C.
577-5T7dl.
(ii) Waters of the State of Florida
within the boundaries of the Florida
Keys National Marine Sanctuary as de-
lineated on a map of the Sanctuary at
http://www.fknms.nos.noaa.gov/.
(c)(l) Prohibition pursuant to CWA sec-
tion 312(1)(4)(B): A State may make
written application to the Adminis-
trator of the Environmental Protection
Agency under section 312(f)(4)(B) of the
Act for the issuance of a regulation es-
tablishing- a drinking water intake no
discharge zone which completely pro-
hibits discharge from a vessel of any
sewage, whether treated or untreated,
into that zone in particular waters, or
portions thereof, within such State.
Such application shall:
(i) Identify and describe exactly and
in detail the location of the drinking
water supply intake(s) and the commu-
nity served by the intake(s), including
average and maximum expected
amounts of inflow;
(ii) Specify and describe exactly and
in detail, the waters, or portions there-
of, for which a complete prohibition is
desired, and where appropriate, aver-
age, maximum and low flows in million
gallons per day (MOD) or the metric
equivalent;
(iii) Include a map, either a USGS
topographic quadrant map or a NOAA
nautical chart, as applicable, clearly
marking by latitude and longitude the
waters or portions thereof to be des-
ignated a drinking water intake zone;
and
(iv) Include a statement of basis jus-
tifying the size of the requested drink-
ing water intake zone, for example,
identifying areas of intensive boating
activities.
(2) If the Administrator finds that a
complete prohibition is appropriate
under this paragraph, he or she shall
publish notice of such finding together
with a notice of proposed rulemaking,
and then shall proceed in accordance
with 5 U.S.C. 553. If the Administra-
tor's finding is that a complete prohibi-
tion covering a more restricted or more
expanded area than that applied for by
the State is appropriate, he or she shall
also include a statement of the reasons
why the finding differs in scope from
that requested in the State's applica-
tion.
(3) If the Administrator finds that a
complete prohibition is inappropriate
under this paragraph, he or she shall
deny the application and state the rea-
sons for such denial.
(4) For the following waters the dis-
charge from a vessel of any sewage,
whether treated or not, is completely
prohibited pursuant to CWA section
312(f)(4)(B):
(i) Two portions of the Hudson River
in New York State, the first is bounded
by an east-west line through the most
northern confluence of the Mohawk
River which will be designated by the
Troy-Waterford Bridge (126th Street
Bridge) on the south and Lock 2 on the
north, and the second of which is
bounded on the north by the southern
end of Houghtaling Island and on the
south by a line between the Village of
Boseton on the western shore and Low
Point on the eastern shore in the vicin-
ity of Chelsea, as described in Items 2
and 3 of 6 NYCRR Part 858.4.
(ii) [Reserved]
[41 FE 4453, Jan. 29, 1976, as amended at 42
FH 43837. Aur. 31, 1977: 60 FB 63945, Deo. 13,
1995; 63 PR 1320, Jan. 8, 1998; 87 FB 35743, May
21, 2002]
§ 140.5 Analytical procedures.
In determining the composition and
quality of effluent discharge from ma-
rine sanitation devices, the procedures
342
-------
Environmental Protection Agency
Pt. 141
contained in 40 CPR part 136, "Guide-
lines Establishing Test Procedures for
the Analysis of Pollutants," or subse-
quent revisions or amendments there-
to, shall be employed.
PART 141—NATIONAL PRIMARY
DRINKING WATER REGULATIONS
Sec.
141.1
141.2
141.3
141.4
141.5
141.6
Subpart A—General
Applicability.
Definitions.
Coverage.
Variances and exemptions.
Siting requirements.
Effective dates.
Subpart B—Maximum Contaminant Levels
141.11 Maximum contaminant levels for In-
organic chemicals.
141.12 Maximum contaminant levels for
total trihalomethanes.
141.13 Maximum contaminant levels for tur-
bidity.
Subpart C—Monitoring and Analytical
Requirements
141.21 Coliform sampling.
141.22 Turbidity sampling and analytical re-
quirements.
141.23 Inorganic chemical sampling and ana-
lytical requirements.
141.24 Organic chemicals, sampling and ana-
lytical requirements.
141.25 Analytical methods for radioactivity.
141.26 Monitoring frequency and compliance
requirements for radionuclldes in com-
munity water systems
141.27 Alternate analytical techniques.
141.28 Certified laboratories,
141.29 Monitoring of consecutive public
water systems.
141.30 Total trihalomethanes sampling, ana-
lytical and other requirements.
Subpart D—Reporting and Recordkeeping
141.31 Reporting requirements.
141.32 Public notification.
141.33 Record maintenance,
141.34 [Reserved]
141.35 Reporting of unregulated contami-
nant monitoring results.
Subpart E—Special Regulations, Including
Monitoring Regulations and Prohibition
on Lead Use
141.40 Monitoring requirements for unregu-
lated contaminants.
141.41 Special monitoring for sodium.
141.42 Special monitoring for corrosivity
characteristics.
141.43 Prohibition on use of lead pipes, sol-
der, and flux.
Subpart F—Maximum Contaminant Level
Goals and Maximum Residual Dis-
infectant Level Goals
141.60 Maximum contaminant level goals
for organic contaminants.
141.51 Maximum contaminant level goals
for inorganic contaminants.
141.52 Maximum contaminant level goals
for microbiological contaminants.
141.63 Maximum contaminant level goals
for disinfection byproducts.
141.54 Maximum residual disinfectant level
goals for disinfectants.
141,65 Maximum contaminant level goals
for radionuclides.
Subpart G—National Primary Drinking
Water Regulations: Maximum Con-
taminant Levels and Maximum Resid-
ual Disinfectant Levels
141,60 Effective dates.
141.61 Maximum contaminant levels for or-
ganic contaminants.
141.62 Maximum contaminant levels for in-
organic contaminants.
141.63 Maximum contaminant levels (MCLs)
for microbiological contaminants,
141.64 Maximum contaminant levels for dis-
infection byproducts.
141.65 Maximum residual disinfectant lev-
els.
141.66 Maximum contaminant levels for
radionuclldes,
Subpart H—Filtration and Disinfection
141.70 General requirements.
141.71 Criteria for avoiding filtration.
141.72 Disinfection.
141.73 Filtration.
141.74 Analytical and monitoring require-
ments.
141.75 Reporting and reeordkeeping require-
ments.
141.76 Recycle provisions.
Subpart I—Control of Lead and Copper
141,80 General requirements.
141.81 Applicability of corrosion control
treatment steps to small, medium-size
and large water systems.
141.82 Description of corrosion control
treatment requirements.
141.83 Source water treatment require-
ments.
141.84 Lead service line replacement re-
quirements,
141.85 Public education and supplemental
monitoring requirements.
343
203-160 D-12
-------
Pt. 141
40 CFR Ch. I (7-1-04 Edition)
141.86 Monitoring requirements for lead and
copper in tap water.
141.87 Monitoring' requirements for water
quality parameters.
141.88 Monitoring requirements for lead and
copper in source water.
141.89 Analytical methods.
141.90 Reporting requirements.
141,91 Reeordkeeping requirements.
Subpart J—Use of Non-Centralized
Treatment Devices
141.100 Criteria and procedures for public
water systems using point-of-entry de-
vices.
141.101 Use of bottled water.
Subpart K—Treatment Techniques
141.110 General requirements.
141.111 Treatment techniques
amide and epiehlorohydrln.
for acryl-
Subpart L—Disinfectant Residuals, Disinfec-
tion Byproducts, and Disinfection By-
product Precursors
141.130 General requirements.
141.131 Analytical requirements.
141.132 Monitoring requirements.
141.133 Compliance requirements.
141.134 Reporting and reeordkeeping re-
quirements,
141.135 Treatment technique for control of
disinfection byproduct (DBF) precursors.
Subparts M-N [Reserved]
Subpart O—Consumer Confidence Reports
141.151 Purpose and applicability of this
subpart.
141.152 Effective dates.
141.153 Content of the reports.
141.154 Required additional health informa-
tion.
141.155 Report delivery and recordkeeping,
APPENDIX A TO SUBPART O OP PAET 141—REG-
ULATED CONTAMINANTS
Subpart P—Enhanced Filtration and Dis-
infection—Systems Serving 10,000 or
More People
141.170 General requirements.
141.171 Criteria for avoiding filtration.
141.172 Disinfection profiling and
benchmarking.
141.173 Filtration.
141.174 Filtration sampling requirements.
141.175 Reporting and recordkeeping' re-
quirements.
Subpart Q—Public Notification of Drinking
Water Violations
141.201 General public notification require-
ments.
141.202 Tier 1 Public Notice—Form, manner,
and frequency of notice.
141.203 Tier 2 Public Notice—Form, manner,
and frequency of notice.
141.204 Tier 3 Public Notice—Form, manner,
and frequency of notice.
141.205 Content of the public notice.
141.206 Notice to new billing units or new
customers.
141,207 Special notice of the availability of
unregulated contaminant monitoring re-
sults.
141.208 Special notice for exceedance of the
SMCL for fluoride.
141.209 Special notice for nitrate
exceedances above MCL by non-commu-
nity water systems (NCWS), where grant-
ed permission by the primacy agency
under §141.11(d).
141.210 Notice by primacy agency on behalf
of the public water system.
APPENDIX A TO SUBPART Q OF PART 141—
NPDWR VIOLATIONS AND SITUATIONS RE-
QUIRING PUBLIC NOTICE
APPENDIX B TO SUBPAET Q OF PABT 141—
STANDARD HEALTH EFFECTS LANGUAGE
FOR PUBLIC NOTIFICATION
APPENDIX C TO SUBPART Q OF PAET 141—LIST
OF ACRONYMS USED IN PUBLIC NOTIFICA-
TION REGULATION
Subparts R-S [Reserved]
Subpart T—Enhanced Filtration and Dis-
infection—Systems Serving Fewer Than
10,000 People
GENERAL REQUIREMENTS
141.500 General requirements.
141.501 Who Is subject to the requirements
of subpart T?
141.502 When must my system comply with.
these requirements?
141.503 What does subpart T require?
FINISHED WATER RESERVOIRS
141.510 Is my system subject to the new fin-
ished water reservoir requirements?
141.511 What is required of new finished
water reservoirs?
ADDITIONAL WATERSHED CONTROL
REQUIREMENTS FOE UNFILTERED SYSTEMS
141.520 Is my system subject to the updated
watershed control requirements?
141.521 What updated watershed control re-
quirements must my nnfiltered system
Implement to continue to avoid filtra-
tion?
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Environmental Protection Agency
§141.2
141.522 How does the State determine
whether my system's watershed control
requirements are adequate?
DISINFECTION PROFILE
141.530 What is a disinfection profile and
who must develop one?
141.531 What criteria must a State use to
determine that a profile is unnecessary?
141.532 How does my system develop a dis-
infection profile and when must it begin?
141.533 What data must my system collect
to calculate a disinfection profile?
141.534 How does my system use this data to
calculate an inaetivation ratio?
141.535 What if my system uses
chloramines, ozone, or chlorine dioxide
for primary disinfection?
141.536 My system has developed an inac-
tivation ratio; what must we do now?
DISINFECTION BENCHMARK
141.540 Who has to develop a disinfection
benchmark?
141.541 What are significant changes to dis-
infection practice?
141.542 What must my system do if we are
considering a significant change to dis-
infection practices?
141.543 How is the disinfection benchmark
calculated?
141.544 What if my system uses
chloramines, ozone, or chlorine dioxide
for primary disinfection?
COMBINED FILTER EFFLUENT REQUIREMENTS
141.550 Is my system required to meet sub-
part T combined filter effluent turbidity
limits?
141.551 What strengthened combined filter
effluent turbidity limits must my system
meet?
141.552 My system consists of "alternative
filtration" and is required to conduct a
demonstration—what is required of my
system and how does the State establish
my turbidity limits?
141.553 My system practices lime soft-
ening—is there any special provision re-
garding my combined filter effluent?
INDIVIDUAL FILTER TURBIDITY REQUIREMENTS
141.560 Is my system subject to individual
filter turbidity requirements?
141.561 What happens if my system's tur-
bidity monitoring equipment fails?
141.562 My system only has two or fewer fil-
ters—is there any special provision re-
garding individual filter turbidity moni-
toring?
141.563 What follow-up action is my system
required to take based on continuous
turbidity monitoring?
141.564 My system practices lime soft-
ening—is there any special provision re-
garding my individual filter turbidity
monitoring?
REPORTING AND BBCORDKEEPING
REQUIBEMBMTS
141.570 What does subpart T require that my
system report to the State?
141.571 What records does subpart T require
my system to keep?
AUTHORITY: 42 U.S.C, 300f, 300g-i, 300g-2,
300g-3, 300g-4, 300g-5, 300g-6, 300J-4, 300J-9,
and 300J-11.
SOURCE: 40 PR 59570, Dec. 24, 1975, unless
otherwise noted.
EDITORIAL NOTE: Nomenclature changes to
part 141 appear at 69 PR 18803, Apr. 9, 2004.
NOTE: For community water systems serv-
ing 75,000 or more persons, monitoring must
begin 1 year following- promulation and the
effective date of the MCL is 2 years following
promulgation. For community water sys-
tems serving 10,000 to 75,000 persons, moni-
toring must begin within 3 years from the
date of promulgation and the effective date
of the MCL is 4 years from the date of pro-
mulgation. Effective immediately, systems
that plan to make significant modifications
to their treatment processes for the purpose
of complying with the TTHM MCL are re-
quired to seek and obtain State approval of
their treatment modification plans. This
note affects §§141.2, 141,6, 141.12, 141.24 and
141.30, For additional information see 44 PR
68641, Nov. 29, 1979.
Subpart A—General
§ 141.1 Applicability.
This part establishes primary drink-
ing water regulations pursuant to sec-
tion 1412 of the Public Health Service
Act, as amended by the Safe Drinking
Water Act (Pub. L. 93-523); and related
regulations applicable to public water
systems.
$ 141.2 Definitions.
As used in this part, the term:
Act means the Public Health Service
Act, as amended by the Safe Drinking
Water Act, Public Law 93-523.
Action level, is the concentration of
lead or copper in water specified in
§141,80(c) which determines, in some
cases, the treatment requirements con-
tained in subpart I of this part that a
water system is required to complete.
Best available technology or BAT
means the best technology, treatment
techniques, or other means which the
Administrator finds, after examination
345
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§141.2
40 CFR Ch. I (7-1-04 Edition)
for efficacy under field conditions and
not solely under laboratory conditions,
are available (taking cost into consid-
eration). For the purposes of setting
MOLs for synthetic organic chemicals,
any BAT must be at least as effective
as granular activated carbon,
Coagulation means a process using co-
agulant chemicals and mixing by which
colloidal and suspended materials are
destabilized and agglomerated into
floes.
Community water system means a pub-
lic water system which serves at least
15 service connections used by year-
round residents or regularly serves at
least 25 year-round residents.
Compliance cycle means the nine-year
calendar year cycle during which pub-
lic water systems must monitor. Bach
compliance cycle consists of three
three-year compliance periods. The
first calendar year cycle begins Janu-
ary 1, 1993 and ends December 31, 2001;
the second begins January 1, 2002 and
ends December 31, 2010; the third begins
January 1, 2011 and ends December 31,
2019.
Compliance period means a three-year
calendar year period within a compli-
ance cycle. Each compliance cycle has
three three-year compliance periods.
Within the first compliance cycle, the
first compliance period runs from Jan-
uary 1, 1993 to December 31, 1995; the
second from January 1, 1996 to Decem-
ber 31, 1998; the third from January 1,
1999 to December 31, 2001.
Comprehensive performance evaluation
(CPE) is a thorough review and anal-
ysis of a treatment plant's perform-
ance-based capabilities and associated
administrative, operation and mainte-
nance practices. It is conducted to
identify factors that may be adversely
impacting a plant's capability to
achieve compliance and emphasizes ap-
proaches that can be implemented
without significant capital improve-
ments. For purpose of compliance with
subparts P and T of this part, the com-
prehensive performance evaluation
must consist of at least the following
components: Assessment of plant per-
formance; evaluation of major unit
processes; identification and
prioritization of performance limiting
factors; assessment of the applicability
of comprehensive technical assistance;
and preparation of a CPE report.
Confluent growth means a continuous
bacterial growth covering the entire
filtration area of a membrane filter, or
a portion thereof, in which bacterial
colonies are not discrete.
Contaminant means any physical,
chemical, biological, or radiological
substance or matter in water.
Conventional filtration treatment
means a series of processes including
coagulation, flocculation, sedimenta-
tion, and filtration resulting in sub-
stantial particulate removal.
Corrosion inhibitor means a substance
capable of reducing the corrosivity of
water toward metal plumbing mate-
rials, especially lead and copper, by
forming a protective film on the inte-
rior surface of those materials.
CT or CTcalc is the product of "resid-
ual disinfectant concentration" (C) in
mg/1 determined before or at the first
customer, and the corresponding "dis-
infectant contact time" (T) in minutes,
i.e., "C" x "T". If a public water system
applies disinfectants at more than one
point prior to the first customer, it
must determine the OT of each dis-
infectant sequence before or at the
first customer to determine the total
percent inactivation or "total inactiva-
tion ratio." In determining the total in-
activation ratio, the public water sys-
tem must determine the residual dis-
infectant concentration of each dis-
infection sequence and corresponding
contact time before any subsequent
disinfection application point(s).
"CTW is the CT value required for 99.9
percent (3-log) inactivation of Giardia
lamblia cysts. CT99.9 for a variety of dis-
infectants and conditions appear in ta-
bles 1.1-1.6, 2.1, and 3.1 of §141.74(b)(3).
CTcalc
CT999
is the inactivation ratio. The sum of
the inactivation ratios, or total inac-
tivation ratio shown as
(CTcalc)
(CT9M)
is calculated by adding together the in-
activation ratio for each disinfection
346
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Environmental Protection Agency
§141.2
sequence. A total inactivation ratio
equal to or greater than 1.0 is assumed
to provide a 3-1 og inactivation of
Giardia lamblia cysts.
Diatomaceous earth filtration means a
process resulting in substantial partic-
ulate removal in which (1) a precoat
cake of diatomaceous earth filter
media is deposited on a support
membrance (septum), and (2) while the
water is filtered by passing through the
cake on the septum, additional filter
media known as body feed is continu-
ously added to the feed water to main-
tain the permeability of the filter
cake.
Direct filtration means a series of
processes including coagulation and fil-
tration but excluding sedimentation
resulting in substantial particulate re-
moval.
Disinfectant means any oxidant, in-
cluding but not limited to chlorine,
chlorine dioxide, chloramines, and
ozone added to water in any part of the
treatment or distribution process, that
is intended to kill or inactivate patho-
genic microorganisms.
Disinfectant contact time ("T" in CT
calculations) means the time in min-
utes that it takes for water to move
from the point of disinfectant applica-
tion or the previous point of disinfect-
ant residual measurement to a point
before or at the point where residual
disinfectant concentration ("C") is
measured. Where only one "C" is meas-
ured, "T" is the time in minutes that it
takes for water to move from the point
of disinfectant application to a point
before or at where residual disinfectant
concentration ("C") is measured. Where
more than one "C" is measured, "T" is
(a) for the first measurement of "C",
the time in minutes that it takes for
water to move from the first or only
point of disinfectant application to a
point before or at the point where the
first "C" is measured and (b) for subse-
quent measurements of "C", the time in
minutes that it takes for water to
move from the previous "C" measure-
ment point to the "C" measurement
point for which the particular "T" is
being calculated. Disinfectant contact
time in pipelines must be calculated
based on "plug flow" by dividing the in-
ternal volume of the pipe by the max-
imum hourly flow rate through that
pipe. Disinfectant contact time within
mixing basins and storage reservoirs
must be determined by tracer studies
or an equivalent demonstration.
Disinfection means a process which
inactivates pathogenic organisms in
water by chemical oxidants or equiva-
lent agents.
Disinfection profile is a summary of
Giardia lamblia inactivation through
the treatment plant. The procedure for
developing a disinfection profile is con-
tained in §141.172 (Disinfection
profiling and benchmarking) in subpart
P and §§141.530-141.536 (Disinfection
profile) in subpart T of this part.
Domestic or other non-distribution sys-
tem plumbing problem means a coliform
contamination problem in a public
water system with more than one serv-
ice connection that is limited to the
specific service connection from which
the coliform-positive sample was
taken.
Dose equivalent means the product of
the absorbed dose from ionizing radi-
ation and such factors as account for
differences in biological effectiveness
due to the type of radiation and its
distribution in the body as specified by
the International Commission on
Radiological Units and Measurements
(ICBU).
Effective corrosion inhibitor residual,
for the purpose of subpart I of this part
only, means a concentration sufficient
to form a passivating film on the inte-
rior walls of a pipe.
Enhanced coagulation means the addi-
tion of sufficient coagulant for im-
proved removal of disinfection byprod-
uct precursors by conventional filtra-
tion treatment.
Enhanced softening means the im-
proved removal of disinfection byprod-
uct precursors by precipitative soft-
ening.
Filter profile is a graphical represen-
tation of individual filter performance,
based on continuous turbidity meas-
urements or total particle counts
versus time for an entire filter run,
from startup to backwash inclusively,
that includes an assessment of filter
performance while another filter is
being backwashed.
Filtration means a process for remov-
ing particulate matter from water by
passage through porous media.
347
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§141.2
40 CFR Ch. I (7-1-04 Edition)
First draw sample means a one-liter
sample of tap water, collected in ac-
cordance with §141.86(b)(2), that has
been standing in plumbing pipes at
least 6 hours and is collected without
flushing the tap.
Flocculation means a process to en-
hance agglomeration or collection of
smaller floe particles into larger, more
easily settleable particles through
gentle stirring by hydraulic or mechan-
ical means.
GAC10 means granular activated car-
bon filter beds with an empty-bed con-
tact time of 10 minutes based on aver-
age daily flow and a carbon reactiva-
tion frequency of every 180 days.
Ground water under the direct influence
of surface water (GWUDI) means any
water beneath the surface of the
ground with significant occurrence of
insects or other macroorganisms,
algae, or large-diameter pathogens
such as Giardia lamblia or
Cryptosporidium, or significant and rel-
atively rapid shifts in water character-
istics such as turbidity, temperature,
conductivity, or pH which closely cor-
relate to climatologieal or surface
water conditions. Direct influence
must be determined for individual
sources in accordance with criteria es-
tablished by the State. The State de-
termination of direct influence may be
based on site-specific measurements of
water quality and/or documentation of
well construction characteristics and
geology with field evaluation.
Gross alpha particle activity means the
total radioactivity due to alpha par-
ticle emission as inferred from meas-
urements on a dry sample.
Gross beta particle activity means the
total radioactivity due to beta particle
emission as inferred from measure-
ments on a dry sample.
Haloacetic acids (five) (HAAS) mean
the sum of the concentrations In milli-
grams per liter of the haloacetic acid
compounds (monochloroacetic acid,
dichloroacetic acid, trichloroacetic
acid, monobromoacetic acid, and dibro-
moacetic acid), rounded to two signifi-
cant figures after addition.
Halogen means one of the chemical
elements chlorine, bromine or iodine.
Initial compliance period means the
first full three-year compliance period
which begins at least 18 months after
promulgation, except for contaminants
listed at §141.61(a) (19)-(21). (c) (19)-(33),
and §141.62(b) (11)-(15), initial compli-
ance period means the first full three-
year compliance period after promulga-
tion for systems with 150 or more serv-
ice connections (January 1993-Decem-
ber 1995), and first full three-year com-
pliance period after the effective date
of the regulation (January 1996-Decem-
ber 1998) for systems having fewer than
150 service connections,
Large water system, for the purpose of
subpart I of this part only, means a
water system that serves more than
50,000 persons.
Lead service line means a service line
made of lead which connects the water
main to the building inlet and any lead
pigtail, gooseneck or other fitting
which is connected to such lead line,
Legionella means a genus of bacteria,
some species of which have caused a
type of pneumonia called Legionnaires
Disease.
Man-made beta particle and photon
emitters means all radionuclides emit-
ting beta particles and/or photons list-
ed in Maximum Permissible Body Bur-
dens and Maximum Permissible Con-
centration of Radionuclides in Air or
Water for Occupational Exposure, NBS
Handbook 69, except the daughter prod-
ucts of thormm-232, uranium-235 and
uranium-238.
Maximum contaminant level means the
maximum permissable level of a con-
taminant in water which is delivered to
any user of a public water system.
Maximum contaminant level goal or
MCLG means the maximum level of a
contaminant in drinking water at
which no known or anticipated adverse
effect on the health of persons would
occur, and which allows an adequate
margin of safety. Maximum contami-
nant level goals are nonenforceable
health goals.
Maximum residual disinfectant level
(MRDL) means a level of a disinfectant
added for water treatment that may
not be exceeded at the consumer's tap
without an unacceptable possibility of
adverse health effects. For chlorine and
chloramines, a PWS is in compliance
with the MRDL when the running an-
nual average of monthly averages of
samples taken in the distribution sys-
tem, computed quarterly, is less than
348
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Environmental Protection Agency
§141.2
or equal to the MRDL. For chlorine di-
oxide, a PWS is in compliance with the
MRDL when daily samples are taken at
the entrance to the distribution system
and no two consecutive daily samples
exceed the MRDL. MRDLs are enforce-
able in the same manner as maximum
contaminant levels under Section 1412
of the Safe Drinking Water Act. There
is convincing evidence that addition of
a disinfectant is necessary for control
of waterborne microbial contaminants.
Notwithstanding the MRDLs listed in
§141.65, operators may increase resid-
ual disinfectant levels of chlorine or
chloramines (but not chlorine dioxide)
in the distribution system to a level
and for a time necessary to protect
public health to address specific micro-
biological contamination problems
caused by circumstances such as dis-
tribution line breaks, storm runoff
events, source water contamination, or
cross-connections.
Maximum residual disinfectant level
goal (MRDLG) means the maximum
level of a disinfectant added for water
treatment at which no known or an-
ticipated adverse effect on the health
of persons would occur, and which al-
lows an adequate margin of safety.
MRDLGs are nonenforceable health
goals and do not reflect the benefit of
the addition of the chemical for con-
trol of waterborne microbial contami-
nants.
Maximum Total Trihalomethane Poten-
tial (MTP) means the maximum con-
centration of total trihalomethanes
produced in a given water containing a
disinfectant residual after 7 days at a
temperature of 25 °C or above.
Medium-size water system, for the pur-
pose of subpart I of this part only,
means a water system that serves
greater than 3,300 and less than or
equal to 50,000 persons.
Near the first service connection means
at one of the 20 percent of all service
connections in the entire system that
are nearest the water supply treatment
facility, as measured by water trans-
port time within the distribution sys-
tem.
Non-community water system means a
public water system that is not a com-
munity water system. A non-commu-
nity water system is either a "transient
non-community water system (TWS)"
or a "non-transient non-community
water system (NTNCWS)."
Non-transient non-community water
system or NTNCWS means a public
water system that is not a community
water system and that regularly serves
at least 25 of the same persons over 6
months per year.
Optimal corrosion control treatment, for
the purpose of subpart I of this part
only, means the corrosion control
treatment that minimizes the lead and
copper concentrations at users* taps
while insuring that the treatment does
not cause the water system to violate
any national primary drinking water
regulations.
Performance evaluation sample means
a reference sample provided to a lab-
oratory for the purpose of dem-
onstrating that the laboratory can suc-
cessfully analyze the sample within
limits of performance specified by the
Agency. The true value of the con-
centration of the reference material is
unknown to the laboratory at the time
of the analysis.
Person means an individual; corpora-
tion; company; association; partner-
ship; municipality; or State, Federal,
or tribal agency.
Picocurie (pd) means the quantity of
radioactive material producing 2.22 nu-
clear transformations per minute.
Point of disinfectant application is the
point where the disinfectant is applied
and water downstream of that point is
not subject to recontamination by sur-
face water runoff.
Point-of-entry treatment device (POE)
is a treatment device applied to the
drinking water entering a house or
building for the purpose of reducing
contaminants in the drinking water
distributed throughout the house or
building.
Point-of-use treatment device (POU) is
a treatment device applied to a single
tap used for the purpose of reducing
contaminants in drinking water at
that one tap.
Public water system means a system
for the provision to the public of water
for human consumption through pipes
or, after August 5, 1998, other con-
structed conveyances, if such system
has at least fifteen service connections
or regularly serves an average of at
least twenty-five individuals daily at
349
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§141.2
40 CFR Ch. I (7-1-04 Edition)
least 60 days out of the year. Such term
includes: any collection, treatment,
storage, and distribution facilities
under control of the operator of such
system and used primarily in connec-
tion with such system; and any collec-
tion or pretreatment storage facilities
not under such control which are used
primarily in connection with such sys-
tem. Such term does not include any
"special irrigation district." A public
water system is either a "community
water system" or a "noncommunlty
water system."
Rem means the unit of dose equiva-
lent from ionizing radiation to the
total body or any internal organ or
organ system. A "millirem (mrem)" is I/
1000 of a rem.
Repeat compliance period means any
subsequent compliance period after the
initial compliance period.
Residual disinfectant concentration ("C"
in CT calculations) means the con-
centration of disinfectant measured in
mg/1 in a representative sample of
water.
Sanitary survey means an onsite re-
view of the water source, facilities,
equipment, operation and maintenance
of a public water system for the pur-
pose of evaluating the adequacy of such
source, facilities, equipment, operation
and maintenance for producing and dis-
tributing safe drinking water.
Sedimentation means a process for re-
moval of solids before filtration by
gravity or separation.
Service connection, as used in the defi-
nition of public water system, does not
include a connection to a system that
delivers water by a constructed con-
veyance other than a pipe if:
(1) The water is used exclusively for
purposes other than residential uses
(consisting of drinking, bathing, and
cooking, or other similar uses);
(2) The State determines that alter-
native water to achieve the equivalent
level of public health protection pro-
vided by the applicable national pri-
mary drinking water regulation is pro-
vided for residential or similar uses for
drinking and cooking; or
(3) The State determines that the
water provided for residential or simi-
lar uses for drinking, cooking, and
bathing is centrally treated or treated
at the point of entry by the provider, a
pass-through entity, or the user to
achieve the equivalent level of protec-
tion provided by the applicable na-
tional primary drinking water regula-
tions.
Service line sample means a one-liter
sample of water collected in accord-
ance with |141.86(b)(3), that has been
standing for at least 6 hours in a serv-
ice line.
Single family structure, for the purpose
of subpart I of this part only, means a
building constructed as a single-family
residence that is currently used as ei-
ther a residence or a place of business.
Slow sand filtration means a process
involving passage of raw water through
a bed of sand at low velocity (generally
less than 0.4 m/h) resulting in substan-
tial particulate removal by physical
and biological mechanisms.
Small water system, for the purpose of
subpart I of this part only, means a
water system that serves 3,300 persons
or fewer.
Special irrigation district means an ir-
rigation district in existence prior to
May 18, 1994 that provides primarily
agricultural service through a piped
water system with only incidental resi-
dential or similar use where the system
or the residential or similar users of
the system comply with the exclusion
provisions in section 1401(4)(B)(i)(II) or
(III).
Standard sample means the aliquot of
finished drinking water that is exam-
ined for the presence of coliform bac-
teria.
State means the agency of the State
or Tribal government which has juris-
diction over public water systems. Dur-
ing any period when a State or Tribal
government does not have primary en-
forcement responsibility pursuant to
section 1413 of the Act, the term
"State" means the Regional Adminis-
trator, U.S. Environmental Protection
Agency.
Subpart H systems means public water
systems using surface water or ground
water under the direct influence of sur-
face water as a source that are subject
to the requirements of subpart H of
this part.
Supplier of water means any person
who owns or operates a public water
system.
350
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Environmental Protection Agency
§141,4
Surface water means all water which
is open to the atmosphere and subject
to surface runoff.
SUVA means Specific Ultraviolet Ab-
sorption at 254 nanometers (nm), an in-
dicator of the humic content of water.
It is a calculated parameter obtained
by dividing a sample's ultraviolet ab-
sorption at a wavelength of 254 nm
(UV254> (in m=1) by its concentration of
dissolved organic carbon (DOC) (in mg/
L).
System with a single service connection
means a system which supplies drink-
ing water to consumers via a single
service line.
Too numerous to count means that the
total number of bacterial colonies ex-
ceeds 200 on a 47-mm diameter mem-
brane filter used for coliform detec-
tion.
Total Organic Carbon (TOC) means
total organic carbon in mg/L measured
using heat, oxygen, ultraviolet irradia-
tion, chemical oxidants, or combina-
tions of these oxidants that convert or-
ganic carbon to carbon dioxide, round-
ed to two significant figures.
Total trihalomethan.es (TTHM) means
the sum of the concentration in
milligrams per liter of the trihalo-
methane compounds (trichloromethane
[chloroform], dibromochloromethane,
bromodichloromethane and
tribromometliane [bromoformj), round-
ed to two significant figures.
Transient non-community water system
or TWS means a non-community water
system that does not regularly serve at
least 25 of the same persons over six
months per year.
Trihalomethane (THM) means one of
the family of organic compounds,
named as derivatives of methane,
wherein three of the four hydrogen
atoms in methane are each substituted
by a halogen atom in the molecular
structure.
Uncovered finished water storage facil-
ity is a tank, reservoir, or other facility
used to store water that will undergo
no further treatment except residual
disinfection and is open to the atmos-
phere.
Virus means a virus of fecal origin
which is infectious to humans by wa-
terborne transmission.
Waterborne disease outbreak means the
significant occurrence of acute infec-
tious illness, epidemiologically associ-
ated with the ingestion of water from a
public water system which is deficient
in treatment, as determined by the ap-
propriate local or State agency.
[40 PR 59570, Dec. 24, 1975, as amended at 41
PE 28403, July 9, 1976; 44 FR 68641, Nov. 29,
1979; 51 FR 11410, Apr. 2, 1986; 52 FR 20674,
June 2, 1987; 52 FR 25712, July 8, 1987; 53 FB
37410, Sept. 26, 1988; 54 FR 27526, 27562, June
29, 1989; 56 FR 3578, Jan. 30, 1991; 56 FR 26547,
June 7, 1991: 57 PR 31838, July 17, 1992; 59 FR
34322, July 1, 1994; 61 FR 24368, May 14, 1996;
63 FR 23366, Apr. 28, 1998; 63 FR 69463, 69515,
Dec. 16, 1998; 66 FE 7061, Jan. 22, 2001; 67 FR
1835, Jan. 14, 2002]
§ 141,3 Coverage.
This part shall apply to each public
water system, unless the public water
system meets all of the following con-
ditions:
(a) Consists only of distribution and
storage facilities (and does not have
any collection and treatment facili-
ties);
(b) Obtains all of its water from, but
is not owned or operated by, a public
water system to which such regula-
tions apply:
(c) Does not sell water to any person;
and
(d) Is not a carrier which conveys
passengers in interstate commerce.
§ 141.4 Variances and exemptions.
(a) Variances or exemptions from
certain provisions of these regulations
may be granted pursuant to sections
1415 and 1416 of the Act and subpart K
of part 142 of this chapter (for small
system variances) by the entity with
primary enforcement responsibility,
except that variances or exemptions
from the MCL for total coliforms and
variances from any of the treatment
technique requirements of subpart H of
this part may not be granted.
(b) EPA has stayed the effective date
of this section relating to the total
coliform MCL of §141.63(a) for systems
that demonstrate to the State that the
violation of the total coliform MCL is
due to a persistent growth of total coli-
forms in the distribution system rather
than fecal or pathogenic contamina-
tion, a treatment lapse or deficiency,
351
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§141.5
40 CFR Ch. I (7-1-04 Edition)
or a problem in the operation or main-
tenance of the distribution system.
[54 FE 27562, June 29, 1989, as amended at 56
FE 1557, Jan. 15, 1991; 63 FE 43846, Aug. 14,
1998]
§ 141.5 Siting requirements.
Before a person may enter into a fi-
nancial commitment for or initiate
construction of a new public water sys-
tem or increase the capacity of an ex-
isting public water system, he shall no-
tify the State and, to the extent prac-
ticable, avoid locating part or all of the
new or expanded facility at a site
which:
(a) Is subject to a significant risk
from earthquakes, floods, fires or other
disasters which could cause a break-
down of the public water system or a
portion thereof; or
(b) Except for intake structures, is
within the floodplain of a 100-year
flood or is lower than any recorded
high tide where appropriate records
exist. The U.S. Environmental Protec-
tion Agency will not seek to override
land use decisions affecting public
water systems siting which are made
at the State or local government lev-
els.
§ 141.6 Effective dates.
(a) Except as provided in paragraphs
(b) through (k) of this section, and in
§141.80(a)(2), the regulations set forth
in this part shall take effect on June
24, 1977.
(b) The regulations for total trihalo-
methanes set forth in §141.12(c) shall
take effect 2 years after the date of
promulgation of these regulations for
community water systems serving
75,000 or more individuals, and 4 years
after the date of promulgation for com-
munities serving 10,000 to 74,§99 indi-
viduals.
(c) The regulations set forth in
§§ 141.11(d); 141.21(a), (c) and (i); 141.22(a)
and (e); 141.23(a)(3) and (a)(4); 141.23(f);
141.24(e) and (f); 141.25(e); 141.27(a);
141.28(a) and (b); 141.31(a), (d) and (e);
141.32(b)(3); and 141.32(d) shall take ef-
fect immediately upon promulgation.
(d) The regulations set forth in
§141.41 shall take effect 18 months from
the date of promulgation. Suppliers
must complete the first round of sam-
pling and reporting within 12 months
following the effective date.
(e) The regulations set forth in
§141.42 shall take effect 18 months from
the date of promulgation. All require-
ments in §141.42 must be completed
within 12 months following the effec-
tive date,
(f) The regulations set forth in
§141.11(c) and §141.23(g) are effective
May 2, 1986. Section 141.23(g)(4) is effec-
tive October 2, 1987.
(g) The regulations contained in
§141.6, paragraph (c) of the table in
141.12, and 141.62(b)(l) are effective July
1, 1991. The regulations contained in
§§ 141.11(b), 141.23, 141.24, 142.57(b),
143.4(b)(12) and (b)(13), are effective
July 30,1992. The regulations contained
in the revisions to §§141.32(e) (16), (25)
through (27) and (46); 141.61(c)(16); and
141.62(b)(3) are effective January 1,1993.
The effective date of regulations con-
tained in §141.61(c) (2), (3), and (4) is
postponed.
(h) Regulations for the analytic
methods listed at §141.23(k)(4) for
measuring antimony, beryllium, cya-
nide, nickel, and thallium are effective
August 17, 1992. Regulations for the
analytic methods listed at §141.24(f)(16)
for dichloromethane, 1,2,4-trtchloro-
benzene, and 1,1,2-trichloroethane are
effective August 17, 1992. Regulations
for the analytic methods listed at
§141.24(h)(12) for measuring dalapon,
dinoseb, diquat, endothall, endrin,
glyphosate, oxamyl, picloram,
simazine, benzo(a)pyrene, di(2-
ethylhexyDadipate, di(2-
ethylhexyDphthalate, hexachloroben-
zene, hexachlorocyclopentadiene, and
2,3,7,8-TCDD are effective August 17,
1992. The revision to §141.12(a) promul-
gated on July 17, 1992 is effective on
August 17, 1992.
(i) [Reserved]
(j) The arsenic maximum contami-
nant levels (MCL) listed in §141.62 is ef-
fective for the purpose of compliance
on January 23, 2006. Requirements re-
lating to arsenic set forth in
§§141.23(0(4), 141.23(k)(3) introductory
text, 141.23(k)(3)(ii), 141.51(b), 141.62(b),
141.62(b)(16), 141.62(c), 141.62(d), and
142,62(b) revisions in Appendix A of sub-
part O for the consumer confidence
rule, and Appendices A and B of sub-
part Q for the public notification rule
352
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Environmental Protection Agency
§141.13
are effective for the purpose of compli-
ance on January 23, 2006, However, the
consumer confidence rule reporting re-
quirements relating to arsenic listed in
§141.154(b) and (f) are effective for the
purpose of compliance on February 22.
2002.
(k) Regulations set forth in
§§141.23(1)(1), 141.23(i)(2), 141.24(f)(15),
141.24(f)(22). 141.24(h)(ll), 141.24(h)(20),
142.16(e), 142.16(j), and 142.16(k) are ef-
fective for the purpose of compliance
on January 22, 2004.
[44 PR 68641, Nov. 29, 1979, as amended at 45
FR 57342, Aug. 27, 1980: 47 FR 10998, Mar, 12,
1982; 51 PR 11410, Apr. 2, 1986; 56 FR 30274,
July 1, 1991; 57 FR 22178, May 27, 1992; 57 FR
31838, July 17, 1992; 59 FR 34322, July 1, 1994;
61 FR 24368, May 14, 1996; 86 FR 7061, Jan. 22,
2001; 66 FE 28350, May 22, 2001]
Subpart B—Maximum
Contaminant Levels
§141.11 Maximum contaminant levels
for inorganic chemicals.
(a) The maximum contaminant level
for arsenic applies only to community
water systems. The analyses and deter-
mination of compliance with the 0.05
milligrams per liter maximum con-
taminant level for arsenic use the re-
quirements of §141.23.
(b) The maximum contaminant level
for arsenic is 0.05 milligrams per liter
for community water systems until
January 23, 2006.
(c) [Reserved]
(d) At the discretion of the State, ni-
trate levels not to exceed 20 mg/1 may
be allowed in a non-community water
system if the supplier of water dem-
onstrates to the satisfaction of the
State that:
(1) Such water will not be available
to children under 6 months of age; and
(2) The non-community water system
is meeting the public notification re-
quirements under §141.209, including
continuous posting of the fact that ni-
trate levels exceed 10 mg/1 and the po-
tential health effects of exposure; and
(3) Local and State public health au-
thorities will be notified annually of
nitrate levels that exceed 10 mg/1; and
(4) No adverse health effects shall re-
sult.
[40 FR 59570, Deo. 24, 1975, as amended at 45
FR 57342, Aug. 27. 1980; 47 FR 10998, Mar. 12,
1982; 51 FR 11410, Apr. 2, 1986; 56 FR 3578, Jan.
30, 1991; 56 FR 26548, June 7, 1991; 56 FR 30274,
July 1, 1991; 56 FR 32113, July 15, 1991; 60 FR
33932, June 29, 1995; 65 FR 26022, May 4, 2000;
66 FR 7061, Jan. 22, 2001]
§ 141.12 Maximum contaminant levels
for total trihalomethanes.
The maximum contaminant level of
0.10 mg/L for total trihalomethanes
(the sum of the concentrations of
bromodichloromethane,
dibromochloromethane,
tribromome thane (bromoform), and
trichloromethane (chloroform)) applies
to subpart H community water systems
which serve a population of 10,000 peo-
ple or more until December 31, 2001.
This level applies to community water
systems that use only ground water
not under the direct influence of sur-
face water and serve a population of
10,000 people or more until December
31, 2003. Compliance with the maximum
contaminant level for total
trihalomethanes is calculated pursuant
to §141.30. After December 31, 2003, this
section is no longer applicable.
[63 FR 69463, Dec. 16, 1998, as amended at 66
FR 3776, Jan. 16, 2001]
§ 141.13 Maximum contaminant levels
for turbidity.
The maximum contaminant levels
for turbidity are applicable to both
community water systems and non-
community water systems using sur-
face water sources in whole or in part.
The maximum contaminant levels for
turbidity in drinking water, measured
at a representative entry point(s) to
the distribution system, are:
EDITORIAL NOTE: At 54 FR 27527, June 29,
1989, §141.13 was amended by adding intro-
ductory text, effective December 31, 1990.
However, introductory text already exists.
The added text follows.
The requirements in this section
apply to unfiltered systems until De-
cember 30, 1991, unless the State has
determined prior to that date, in writ-
ing pursuant to § 1412(b)(7)(C)(iiO, that
filtration is required. The requirements
353
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§141.21
40 CFR Ch. I (7-1-04 Edition)
in this section apply to filtered sys-
tems until June 29, 1993. The require-
ments in this section apply to
unfiltered systems that the State has
determined, in writing pursuant to
§1412(b)(7)(C)(iii), must install filtra-
tion, until June 29, 1993, or until filtra-
tion is installed, whichever is later.
(a) One turbidity unit (TU), as deter-
mined by a monthly average pursuant
to § 141.22, except that five or fewer tur-
bidity units may be allowed if the sup-
plier of water can demonstrate to the
State that the higher turbidity does
not do any of the following:
(1) Interfere with disinfection;
(2) Prevent maintenance of an effec-
tive disinfectant agent throughout the
distribution system; or
(3) Interfere with microbiological de-
terminations.
(b) Five turbidity units based on an
average for two consecutive days pur-
suant to §141.22.
[40 FR 59570, Deo. 24, 1975]
Subpart C—Monitoring and
Analytical Requirements
§ 141.21 Coliform sampling.
(a) Routine monitoring, (1) Public
water systems must collect total coli-
form samples at sites which are rep-
resentative of water throughout the
distribution system according to a
written sample siting plan. These plans
are subject to State review and revi-
sion.
(2) The monitoring frequency for
total coliforms for community water
systems is based on the population
served by the system, as follows;
TOTAL COLIFORM MONITORING FREQUENCY FOR
COMMUNITY WATER SYSTEMS
TOTAL COLIFORM MONITORING FREQUENCY FOR
COMMUNITY WATER SYSTEMS—Continued
Population served
25 to 1,000'
1,001 to 2,500
2,501 to 3,300
3.301 to 4,100
4 101 to 4 900 ., .
4,901 to 5,800
5,801 to 6,700
6 701 to 7 600
7601to8,500
3,501 to 12,900
12,901 to 17.200
Minimum
number
of sam-
ples per
month
1
2
3
4
5
6
7
8
9
10
15
Population served
17,201 to 21 ,500
21 501 to 25 000
25,001 to 33,000
33,001 to 41,000
41,001to50,000
50 001 to 59 000 , . ,
59,001 to 70,000
70,001 to 83,000
830011096,000
96,001 to 130,000
130,001 to 220,000
220 001 to 320 000
320,001 to 450,000
45000110600,000
600,001 10780,000
780,001 to 970,000
970 001 to 1 ,230 000
1,230,001 to 1,520,000
1 520001 to 1 850000
1,850,001 to 2,270,000
2 270 001 to 3 020 000
3,020,001 to 3,960,000
3,960 001 or more
Minimum
number
of sam-
ples per
month
20
25
30
40
50
60
70
80
90
100
120
150
180
210
240
270
300
330
360
390
420
450
480
11ncludes public water systems which have at least 15
service connections, but serve fewer than 25 persons.
If a community water system serving
25 to 1,000 persons has no history of
total coliform contamination in its
current configuration and a sanitary
survey conducted in the past five years
shows that the system is supplied sole-
ly by a protected groundwater source
and is free of sanitary defects, the
State may reduce the monitoring fre-
quency specified above, except that in
no case may the State reduce the mon-
itoring frequency to less than one sam-
ple per quarter. The State must ap-
prove the reduced monitoring fre-
quency in writing.
(3) The monitoring frequency for
total coliforms for non-community
water systems is as follows:
(i) A non-community water system
using only ground water (except
ground water under the direct influ-
ence of surface water, as defined in
§141.2) and serving 1,000 persons or
fewer must monitor each calendar
quarter that the system provides water
to the public, except that the State
may reduce this monitoring frequency,
in writing, if a sanitary survey shows
that the system is free of sanitary de-
fects. Beginning June 29, 1994, the
State cannot reduce the monitoring
frequency for a non-community water
354
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Environmental Protection Agency
§141.21
system using only ground water (ex-
cept ground water under the direct In-
fluence of surface water, as defined in
§141.2) and serving 1,000 persons or
fewer to less than once/year.
(ii) A non-community water system
using only ground water (except
ground water under the direct influ-
ence of surface water, as defined in
§ 141.2) and serving more than 1,000 per-
sons during any month must monitor
at the same frequency as a like-sized
community water system, as specified
in paragraph (a)(2) of this section, ex-
cept the State may reduce this moni-
toring frequency, in writing, for any
month the system serves 1,000 persons
or fewer. The State cannot reduce the
monitoring frequency to less than
once/year. For systems using ground
water under the direct influence of sur-
face water, paragraph (a)(3)(iv) of this
section applies.
(ill) A non-community water system
using surface water, in total or in part,
must monitor at the same frequency as
a like-sized community water system,
as specified in paragraph (a)(2) of this
section, regardless of the number of
persons it serves.
(iv) A non-community water system
using ground water under the direct
influence of surface water, as defined
in §141.2, must monitor at the same
frequency as a like-sized community
water system, as specified in paragraph
(a)(2) of this section. The system must
begin monitoring at this frequency be-
ginning six months after the State de-
termines that the ground water is
under the direct influence of surface
water.
(4) The public water system must col-
lect samples at regular time intervals
throughout the month, except that a
system which uses only ground water
(except ground water under the direct
influence of surface water, as defined
in §141.2), and serves 4,900 persons or
fewer, may collect all required samples
on a single day if they are taken from
different sites.
(5) A public water system that uses
surface water or ground water under
the direct influence of surface water, as
defined in §141.2, and does not practice
filtration in compliance with Subpart
H must collect at least one sample near
the first service connection each day
the turbidity level of the source water,
measured as specified in §141.74(b)(2),
exceeds 1 NTU, This sample must be
analyzed for the presence of total coli-
forms. When one or more turbidity
measurements in any day exceed 1
NTU, the system must collect this coli-
form sample within 24 hours of the first
exceedance, unless the State deter-
mines that the system, for logistical
reasons outside the system's control,
cannot have the sample analyzed with-
in 30 hours of collection. Sample re-
sults from this coliform monitoring
must be included in determining com-
pliance with the MCL for total coli-
forms in §141.63.
(6) Special purpose samples, such as
those taken to determine whether dis-
infection practices are sufficient fol-
lowing pipe placement, replacement, or
repair, shall not be used to determine
compliance with the MCL for total
coliforms in §141.63. Repeat samples
taken pursuant to paragraph (b) of this
section are not considered special pur-
pose samples, and must be used to de-
termine compliance with the MCL for
total coliforms in § 141.63.
(b) Repeat monitoring. (1) If a routine
sample is total coliform-positive, the
public water system must collect a set
of repeat samples within 24 hours of
being notified of the positive result. A
system which collects more than one
routine sample/month must collect no
fewer than three repeat samples for
each total coliform-positive sample
found. A system which collects one
routine sample/month or fewer must
collect no fewer than four repeat sam-
ples for each total coliform-positive
sample found. The State may extend
the 24-hour limit on a case-by-case
basis if the system has a logistical
problem in collecting the repeat sam-
ples within 24 hours that is beyond its
control. In the case of an extension,
the State must specify how much time
the system has to collect the repeat
samples.
(2) The system must collect at least
one repeat sample from the sampling
tap where the original total coliform-
positive sample was taken, and at least
one repeat sample at a tap within five
service connections upstream and at
least one repeat sample at a tap within
five service connections downstream of
355
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§141.21
40 CFR Ch. I (7-1-04 Edition)
the original sampling site. If a total
coliform-positive sample is at the end
of the distribution system, or one away
from the end of the distribution sys-
tem, the State may waive the require-
ment to collect at least one repeat
sample upstream or downstream of the
original sampling site.
(3) The system must collect all re-
peat samples on the same day, except
that the State may allow a system
with a single service connection to col-
lect the required set of repeat samples
over a four-day period or to collect a
larger volume repeat sample(s) in one
or more sample containers of any size,
as long as the total volume collected is
at least 400 ml (300 ml for systems
which collect more than one routine
sample/month).
(4) If one or more repeat samples in
the set is total coliform-positive, the
public water system must collect an
additional set of repeat samples in the
manner specified in paragraphs (b) (1>-
(3) of this section. The additional sam-
ples must be collected within 24 hours
of being notified of the positive result,
unless the State extends the limit as
provided in paragraph (b)(l) of this sec-
tion. The system must repeat this
process until either total coliforms are
not detected in one complete set of re-
peat samples or the system determines
that the MCL for total coliforms in
§141.63 has been exceeded and notifies
the State.
(5) If a system collecting fewer than
five routine samples/month has one or
more total coliform-positive samples
and the State does not invalidate the
sample(s) under paragraph (c) of this
section, it must collect at least five
routine samples during the next month
the system provides water to the pub-
lic, except that the State may waive
this requirement if the conditions of
paragraph (b)(5) (i) or (ii) of this sec-
tion are met. The State cannot waive
the requirement for a system to collect
repeat samples in paragraphs (b) (l)-(4)
of this section.
(i) The State may waive the require-
ment to collect five routine samples
the next month the system provides
water to the public if the State, or an
agent approved by the State, performs
a site visit before the end of the next
month the system provides water to
the public. Although a sanitary survey
need not be performed, the site visit
must be sufficiently detailed to allow
the State to determine whether addi-
tional monitoring- and/or any correc-
tive action is needed. The State cannot
approve an employee of the system to
perform this site visit, even if the em-
ployee is an agent approved by the
State to perform sanitary surveys.
(ii) The State may waive the require-
ment to collect five routine samples
the next month the system provides
water to the public if the State has de-
termined why the sample was total
coliform-positive and establishes that
the system has corrected the problem
or will correct the problem before the
end of the next month the system
serves water to the public. In this case,
the State must document this decision
to waive the following month's addi-
tional monitoring requirement in writ-
ing, have it approved and signed by the
supervisor of the State official who
recommends such a decision, and make
this document available to the EPA
and public. The written documentation
must describe the specific cause of the
total coliform-positive sample and
what action the system has taken and/
or will take to correct this problem.
The State cannot waive the require-
ment to collect five routine samples
the next month the system provides
water to the public solely on the
grounds that all repeat samples are
total coliform-negative. Under this
paragraph, a system must still take at
least one routine sample before the end
of the next month it serves water to
the public and use it to determine com-
pliance with the MCL for total coli-
forms in §141.63, unless the State has
determined that the system has cor-
rected the contamination problem be-
fore the system took the set of repeat
samples required in paragraphs (b) (1)-
(4) of this section, and all repeat sam-
ples were total coliform-negative.
(6) After a system collects a routine
sample and before it learns the results
of the analysis of that sample, if it col-
lects another routine sample(s) from
within five adjacent service connec-
tions of the initial sample, and the ini-
tial sample, after analysis, is found to
356
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Environmental Protection Agency
§141.21
contain total coliforms, then the sys-
tem may count the subsequent sam-
ple(s) as a repeat sample instead of as
a routine sample.
(7) Results of all routine and repeat
samples not invalidated by the State
must be included in determining com-
pliance with the MCL for total coli-
forms in § 141.63.
(c) Invalidation of total coliform sam-
ples. A total coliform-positive sample
invalidated under this paragraph (c)
does not count towards meeting the
minimum monitoring requirements of
this section.
(1) The State may invalidate a total
coliform-positive sample only if the
conditions of paragraph (c)(l) (i), (ii),
or (ill) of this section are met.
(i) The laboratory establishes that
improper sample analysis caused the
total coliform-positive result.
(ii) The State, on the basis of the re-
sults of repeat samples collected as re-
quired by paragraphs (b) (1) through (4)
of this section, determines that the
total coliform-positive sample resulted
from a domestic or other non-distribu-
tion system plumbing problem. The
State cannot invalidate a sample on
the basis of repeat sample results un-
less all repeat sample(s) collected at
the same tap as the original total coli-
form-positive sample are also total
coliform-positive, and all repeat sam-
ples collected within five service con-
nections of the original tap are total
coliform-negative (e.g., a State cannot
invalidate a total coliform-positive
sample on the basis of repeat samples if
all the repeat samples are total coli-
form-negative, or if the public water
system has only one service connec-
tion).
(iii) The State has substantial
grounds to believe that a total coli-
form-positive result is due to a cir-
cumstance or condition which does not
reflect water quality in the distribu-
tion system. In this case, the system
must still collect all repeat samples re-
quired under paragraphs (b) (l}-(4) of
this section, and use them to deter-
mine compliance with the MCL for
total coliforms in §141.63. To invalidate
a total coliform-positive sample under
this paragraph, the decision with the
rationale for the decision must be doc-
umented in writing, and approved and
signed by the supervisor of the State
official who recommended the decision.
The State must make this document
available to EPA and the public. The
written documentation must state the
specific cause of the total coliform-
positive sample, and what action the
system has taken, or will take, to cor-
rect this problem. The State may not
invalidate a total coliform-positive
sample solely on the grounds that all
repeat samples are total coliform-nega-
tive.
(2) A laboratory must invalidate a
total coliform sample (unless total
coliforms are detected) if the sample
produces a turbid culture in the ab-
sence of gas production using an ana-
lytical method where gas formation is
examined (e.g., the Multiple-Tube Fer-
mentation Technique), produces a
turbid culture in the absence of an acid
reaction in the Presence-Absence (P-A)
Coliform Test, or exhibits confluent
growth or produces colonies too numer-
ous to count with an analytical method
using a membrane filter (e.g., Mem-
brane Filter Technique). If a labora-
tory invalidates a sample because of
such interference, the system must col-
lect another sample from the same lo-
cation as the original sample within 24
hours of being notified of the inter-
ference problem, and have it analyzed
for the presence of total coliforms. The
system must continue to re-sample
within 24 hours and have the samples
analyzed until it obtains a valid result.
The State may waive the 24-hour time
limit on a case-by-case basis.
(d) Sanitary surveys. (l)(i) Public
water systems which do not collect five
or more routine samples/month must
undergo an initial sanitary survey by
June 29, 1994, for community public
water systems and June 29, 1999, for
non-community water systems. There-
after, systems must undergo another
sanitary survey every five years, ex-
cept that non-community water sys-
tems using only protected and dis-
infected ground water, as defined by
the State, must undergo subsequent
sanitary surveys at least every ten
years after the initial sanitary survey.
The State must review the results of
each sanitary survey to determine
whether the existing monitoring fre-
quency is adequate and what additional
357
-------
§141.21
40 CFR Ch, I (7-1-04 Edition)
measures, if any, the system needs to
undertake to Improve drinking water
quality.
(ii) In conducting a sanitary survey
of a system using ground water in a
State having an EPA-approved well-
head protection program under section
1428 of the Safe Drinking Water Act,
information on sources of contamina-
tion within the delineated wellhead
protection area that was collected in
the course of developing and imple-
menting the program should be consid-
ered instead of collecting new informa-
tion, if the information was collected
since the last time the system was sub-
ject to a sanitary survey.
(2) Sanitary surveys must be per-
formed by the State or an agent ap-
proved by the State. The system is re-
sponsible for ensuring the survey takes
place.
(e) Fecal coliforms/Escherichia coli (E.
coli) testing, (1) If any routine or repeat
sample is total coliform-positive, the
system must analyze that total coli-
form-positive culture medium to deter-
mine if fecal coliforms are present, ex-
cept that the system may test for E.
coli in lieu of fecal coliforms. If fecal
coliforms or E. coli are present, the sys-
tem must notify the State by the end
of the day when the system is notified
of the test result, unless the system is
notified of the result after the State of-
fice is closed, in which case the system
must notify the State before the end of
the next business day.
(2) The State has the discretion to
allow a public water system, on a case-
by-case basis, to forgo fecal coliform or
E. coli testing on a total coliform-posi-
tive sample if that system assumes
that the total coliform-positive sample
is fecal coliform-positive or E. coH-posi-
tive. Accordingly, the system must no-
tify the State as specified in paragraph
(e)(l) of this section and the provisions
of § 141.63(b) apply,
(f) Analytical methodology. (1) The
standard sample volume required for
total coliform analysis, regardless of
analytical method used, is 100 ml.
(2) Public water systems need only
determine the presence or absence of
total coliforms; a determination of
total coliform density is not required.
(3) Public water systems must con-
duct total coliform analyses in accord-
ance with one of the analytical meth-
ods in the following table.
Organism
Total Coliforms2 ....
Methodology12
Total Coliform Fermentation Technique 3'4'fl
Total Coliform Membrane Filter Technique6 , ....
Presence-Absence (P-A) Coiiform Test-"1-7
ONPG-MUG Test"
Colisure Test9.
E'Colite«Test1t>.
m-ColiBlue24® Test11.
Readyculta Coliforms 100 Presence/Absence Test13.
Membrane Filter Technique using Chromocult* Coliform Agar1'
CoiitagdiTesl1'.
Citation1
9221A, B.
9222A, B, C.
9221D.
I 9223.
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following
documents listed in footnotes 1, 6, 8, 9, 10 , 11, 13, 14 and 15 was approved by the Director of the Federal Register in accord-
ance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed below. Infor-
mation regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800—426-4791. Docu-
ments may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., EPA West, Room B102,
Washington DC 20460 (Telephone: 202-586-2426); or at the National Archives and Records Administration (NARA). For infor-
mation on the availability of this material at NARA, cail 2G2-741-6Q3G, or go to: http://www.archtves.gov/fedeml register/
code of federal regu/aiions/ibr_ locations.html
1 Standard Mettmds for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995). or 20th edition
(1998). American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in
any of these three editions may be used.
^The time from sample coliection to initiation of analysis may not exceed 30 hours. Systems are encouraged but not required
to hold samples below 10 deg, C during transit
3 Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system conducts at least 25 par-
allel tests between this medium and laury! tryptose broth using the water normaily tested, and this comparison demonstrates that
the false-positive rate and false-negative rate for total coliform, using lactose broth, is less than 10 percent,
4 If inverted tubes are used to detect gas production, the media should cover these tubes at least one-half to two-thirds after
the sample is added.
5 No requirement exists to run the completed phase on 10 percent of all total coliform-positive confirmed lubes.
6 Ml agar also may be used. Preparation and use of Ml agar is set forth in the article, "New medium for the simultaneous de-
tection of total coliform and Escherichia coli in water" by Brenner, K.P., at. at, 1996, Appl. Environ. Microbiol. 59:3534-3544.
Also available from the Office of Water Resource Center (HC-4100T), 1200 Pennsylvania Avenue, NW., Washington, DC 20460,
EPA/600/J-99/225. Verification of colonies is not required,
7 Six-times formulation strength may be used if the medium is filter-sterilized rather than autoclaved.
8 The ONPG-MUG Test is also known as the Autoanalysis Collect System.
9A description of the Colisure Test, Feb 28, 1994, may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive,
Westbrook, Maine 04092. The Colisure Test may be read after an incubation time of 24 hours.
358
-------
Environmental Protection Agency
§141.21
10 A description of the E'Colite® Test, "Presence/Absence for Conforms and E Coli in Water," Dec 21, 1997, is available from
Charm Sciences, Inc., 36 Franklin Street, Maiden, MA 02148-4120.
11A description of the m-Coli81ue24 ® Test, Aug 17, 1999. is available from the Hach Company, 100 Dayton Avenue, Ames,
IA 50010.
12 EPA strongly recommends that laboratories evaluate the false-positive and negative rates for the method(s) they use for
monitoring total conforms. EPA also encourages laboratories to establish false-positive and false-negative rates within their own
laboratory and sample matrix (drinking water or source water) with the intent that if the method they choose has an unacceptable
false-positive or negative rate, another method can be used. The Agency suggests that laboratories perform these studies on a
minimum of 5% of all tola! coliform-positive samples, except for those methods where verification/confirmation is already re-
quired, e.g., the M-Endo and LES Endo Membrane Filter Tests, Standard Total Cofiform Fermentation Technique, and Presence-
Absence Coliform Test. Methods for establishing false-positive and negative-rates may be based on lactose fermentation, the
rapid test for p-galactosidase and cytochrome oxidase, multi-test identification systems, or equivalent confirmation tests. False-
positive and false-negative information is often available in published studies and/or from the manufacturer(s).
13The Readycult® California 100 Presence/Absence Test is described in the document, "Readycult® Coliforms 100 Pres-
ence/Absence Test for Detection and Identification of Cpliform Bacteria and Escherichla coli in Finished Waters". November
2000, Version 1.0, available from EM Science (an affiliate of Merck KGgA, Darmstadt Germany), 480 S. Democrat Road,
Gibbstown, NJ 08027-1297, Telephone number is (800) 222-0342, e-mail address is: adellenbusch&ernscience.com.
14 Membrane Filter Technique using Chromocult® Colitorm Agar is described in the document, "Chromocult® Coliforrn Aqar
Presence/Absence Membrane Filter Test Method for Detection and Identification of Coliform Bacteria and Escherichla coli in Fin-
ished Waters", November 2000, Version 1.0, available from EM Science (an affiliate of Merck KQgA, Darmstadt Germany), 480
S, Democrat Road, Qibbstown, NJ 08027-1287. Telephone number is (800) 222-0342, e-mail address is:
atteltenbusch @emscienc@.com.
15Coiitag® product for the determination of the presence/absence of total conforms and £ cott is described in "Colitag®
Product as a Test for Detection and Identification of Coltforrns and f. coli Bacteria in Drinking Water and Source Water as Re-
quired in National Primary Drinking Water Regulations," August 2001, available from CPI International, Inc., 5580 Skylane Blvd.,
Santa Rosa, CA, 95403, telephone (800) 878-7654, Fax (707) 545-7901, Internet address http://www.cpi/nternational.com.
(4) [Reserved]
(5) Public water systems must con-
duct fecal coliform analysis in accord-
ance with the following procedure.
When the MTF Technique or Presence-
Absence (PA) Coliform Test is used to
test for total conforms, shake the lac-
tose-positive presumptive tube or P-A
vigorously and transfer the growth
with a sterile 3-mm loop or sterile ap-
plicator stick into brilliant green lac-
tose bile broth and EC medium to de-
termine the presence of total and fecal
coliforms, respectively. For EPA-ap-
proved analytical methods which use a
membrane filter, transfer the total
coliform-positive culture by one of the
following methods: remove the mem-
brane containing the total coliform
colonies from the substrate with a ster-
ile forceps and carefully curl and insert
the membrane into a tube of EC me-
dium (the laboratory may first remove
a small portion of selected colonies for
verification), swab the entire mem-
brane filter surface with a sterile cot-
ton swab and transfer the inoculum to
EC medium (do not leave the cotton
swab in the EC medium), or inoculate
individual total coliform-positive colo-
nies into EC Medium. Gently shake the
inoculated tubes of EC medium to in-
sure adequate mixing and incubate in a
waterbath at 44.5 ± 0.2 °C for 24 + 2
hours. Gas production of any amount
in the inner fermentation tube of the
EC medium indicates a positive fecal
coliform test. The preparation of EC
medium is described in Method 9221E
(paragraph la) in Standard Methods for
the Examination of Water and Waste-
water, 18th edition (1992), 19th edition
(1995), and 20th edition (1998); the cited
method in any one of these three edi-
tions may be used. Public water sys-
tems need only determine the presence
or absence of fecal coliforms; a deter-
mination of fecal coliform density is
not required.
(6) Public water systems must con-
duct analysis of Escherichia coli in ac-
cordance with one of the following ana-
lytical methods:
(i) EC medium supplemented with 50
\ig/mL of 4-methylumbelllferyl-beta-D-
glueuronide (MUG) (final concentra-
tion), as described in Method 9222G in
Standard Methods for the Examination
of Water and Wastewater, 19th edition
(1995) and 20th edition (1998). Either
edition may be used. Alternatively, the
18th edition (1992) may be used if at
least 10 mL of EC medium, as described
in paragraph (f)(5) of this section, is
supplemented with 50 ng/mL of MUG
before autoclaving. The inner inverted
fermentation tube may be omitted. If
the 18th edition is used, apply the pro-
cedure in paragraph (f)(5) of this sec-
tion for transferring a total coliform-
positive culture to EC medium supple-
mented with MUG, incubate the tube
at 44.5 ± 0.2 °C for 24 ± 2 hours, and then
observe fluorescence with an ultra-
violet light (366 nm) in the dark. If flu-
orescence is visible, B. coli are present.
(ii) Nutrient agar supplemented with
100 ng/mL of 4-methylumbelliferyl-
beta-D-glucuronide (MUG) (final con-
centration), as described in Method
359
-------
§141.21
40 CFR Ch. I (7-1-04 Edition)
9222G in Standard Methods for the Ex-
amination of Water and Wastewater,
19th edition (1995) and 20th edition
(1998). Either edition may be used for
determining if a total coliform-positive
sample, as determined by a membrane
filter technique, contains E. coll. Al-
ternatively, the 18th edition (1992) may
be used if the membrane filter con-
taining: a total coliform-positive col-
ony(ies) is transferred to nutrient agar,
as described in Method 9221B (para-
graph 3) of Standard Methods (18th edi-
tion), supplemented with 100 |ig/mL of
MUG. If the 18th edition is used, incu-
bate the agar plate at 35 °C for 4 hours
and then observe the colony(ies) under
ultraviolet light (366 run) in the dark
for fluorescence. If fluorescence is visi-
ble, E. coli are present.
(iii) Minimal Medium ONPG-MUG
(MMO-MUG) Test, as set forth in the
article "National Field Evaluation of a
Defined Substrate Method for the Si-
multaneous Detection of Total Con-
forms and Escherichia coli from Drink-
ing Water: Comparison with Presence-
Absence Techniques" (Edberg et al.),
Applied and Environmental Microbi-
ology, Volume 55, pp. 1003-1008, April
1989. (Note: The Autoanalysis Colilert
System is an MMO-MUG test). If the
MMO-MUG test is total coliform-posi-
tive after a 24-hour incubation, test the
medium for fluorescence with a 366-nm
ultraviolet light (preferably with a 6-
watt lamp) in the dark. If fluorescence
is observed, the sample is E. colt-posi-
tive. If fluorescence is questionable
(cannot be definitively read) after 24
hours incubation, incubate the culture
for an additional four hours (but not to
exceed 28 hours total), and again test
the medium for fluorescence. The
MMO-MUG Test with hepes buffer in
lieu of phosphate buffer is the only ap-
proved formulation for the detection of
E. coli,
(iv) The Colisure Test. A description
of the Colisure Test may be obtained
from the Millipore Corporation, Tech-
nical Services Department, 80 Ashby
Road, Bedford, MA 01730.
(v) The membrane filter method with
MI agar, a description of which is cited
in footnote 6 to the table in paragraph
(f)(3) of this section.
(vi) E*Colite® Test, a description of
which is cited in footnote 10 to the
table at paragraph (f)(3) of this section.
(vii) m-ColiBlue24® Test, a descrip-
tion of which is cited in footnote 11 to
the table in paragraph (f)(3) of this sec-
tion.
(viii) Readycult® Coliforms 100 Pres-
ence/Absence Test, a description of
which is cited in footnote 13 to the
table at paragraph (f)(3) of this section.
(ix) Membrane Filter Technique
using Chromocult® Coliform Agar, a
description of which is cited in foot-
note 14 to the table at paragraph (f)(3)
of this section.
(x) Colitag*, a description of which
is cited in footnote 15 to the table at
paragraph (f)(3) of this section.
(7) As an option to paragraph
(f)(6)(iii) of this section, a system with
a total coliform-positive, MUG-nega-
tive, MMO-MUG test may further ana-
lyze the culture for the presence of E.
coli by transferring a 0.1 ml, 28-hour
MMO-MUG culture to EC Medium +
MUG with a pipet. The formulation and
incubation conditions of EC Medium -t-
MUG, and observation of the results
are described in paragraph (f)(6)(i) of
this section.
(8) The following materials are incor-
porated by reference in this section
with the approval of the Director of the
Federal Register in accordance with 5
U.S.C. 552(a) and 1 CFE part 51. Copies
of the analytical methods cited in
Standard Methods for the Examination
of Water and Wastewater (18th, 19th,
and 20th editions) may be obtained
from the American Public Health Asso-
ciation et al.: 1015 Fifteenth Street,
NW., Washington, DC 20005-2605. Copies
of the MMO-MUG Test, as set forth in
the article "National Field Evaluation
of a Defined Substrate Method for the
Simultaneous Enumeration of Total
Coliforms and Escherichia coli from
Drinking Water: Comparison with the
Standard Multiple Tube Fermentation
Method" (Edberg et al.) may be ob-
tained from the American Water Works
Association Research Foundation, 6666
West Quincy Avenue, Denver, CO 80235.
Copies of the MMO-MUG Test as set
forth in the article "National Field
Evaluation of a Defined Substrate
360
-------
Environmental Protection Agency
§141.22
Method for the Simultaneous Enu-
meration of Total Coliforms and Esch-
erichia coli from Drinking Water: Com-
parison with the Standard Multiple
Tube Fermentation Method" (Edberg et
al.) may be obtained from the Amer-
ican Water Works Association Re-
search Foundation, 6666 West Quincy
Avenue, Denver, CO 80235. A descrip-
tion of the Colisure Test may be ob-
tained from the Millipore Corp., Tech-
nical Services Department, 80 Ashby
Road, Bedford, MA 01730. Copies may be
inspected at EPA's Drinking Water
Docket; 401 M St., SW,; Washington,
DC 20460, or at the National Archives
and Records Administration (NARA).
For information on the availability of
this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/
federal register/
code of_ fedeml_ regulations/
ibr locaiions.html.
(g) Response to violation. (1) A public
water system which has exceeded the
MCL for total coliforms in §141.63 must
report the violation to the State no
later than the end of the next business
day after it learns of the violation, and
notify the public in accordance with
subpart Q.
(2) A public water system which has
failed to comply with a coliform moni-
toring requirement, including the sani-
tary survey requirement, must report
the monitoring- violation to the State
within ten days after the system dis-
covers the violation, and notify the
public in accordance with subpart Q.
[54 FE 27562, June 29, 1989, as amended at 54
FB 30001, July 17, 1989; 55 FR 25064, June 19,
1990; 56 FB 642, Jan. 8, 1991; 57 PR 1852, Jan.
15, 1992; 57 PB 24747, June 10, 1892; 59 FB
62466, Deo. 5, 1994; 60 PR 34085, June 29, 1995;
64 FB 67461, Dec. 1, 1999; 65 FB 26022. May 4,
2000; 67 FR 65246, Oct. 23, 2002; 67 FR 65896.
Oct. 29, 2002; 69 FB 7160, Feb. 13, 2004]
§ 141.22 Turbidity sampling and ana-
lytical requirements.
The requirements in this section
apply to unfiltered systems until De-
cember 30, 1991, unless the State has
determined prior to that date, in writ-
ing pursuant to section 1412(b)(7)(iii),
that filtration is required. The require-
ments in this section apply to filtered
systems until June 29, 1993, The re-
quirements in this section apply to
unfiltered systems that the State has
determined, in writing pursuant to sec-
tion 1412(b)(7)(C)(iii), must install fil-
tration, until June 29, 1993, or until fil-
tration is installed, whichever is later.
(a) Samples shall be taken by sup-
pliers of water for both community and
non-community water systems at a
representative entry point(s) to the
water distribution system at least once
per day, for the purposes of making
turbidity measurements to determine
compliance with §141,13. If the State
determines that a reduced sampling
frequency in a non-community will not
pose a risk to public health, it can re-
duce the required sampling frequency.
The option of reducing the turbidity
frequency shall be permitted only in
those public water systems that prac-
tice disinfection and which maintain
an active residual disinfectant in the
distribution system, and in those cases
where the State has indicated in writ-
ing that no unreasonable risk to health
existed under the circumstances of this
option. Turbidity measurements shall
be made as directed in §141.74(a)(l).
(b) If the result of a turbidity anal-
ysis indicates that the maximum al-
lowable limit has been exceeded, the
sampling and measurement shall be
confirmed by resampling as soon as
practicable and preferably within one
hour. If the repeat sample confirms
that the maximum allowable limit has
been exceeded, the supplier of water
shall report to the State within 48
hours. The repeat sample shall be the
sample used for the purpose of calcu-
lating the monthly average. If the
monthly average of the daily samples
exceeds the maximum allowable limit,
or if the average of two samples taken
on consecutive days exceeds 5 TU, the
supplier of water shall report to the
State and notify the public as directed
in §§141.31 and subpart Q.
(c) Sampling for non-community
water systems shall begin within two
years after the effective date of this
part.
(d) The requirements of this §141.22
shall apply only to public water sys-
tems which use water obtained in
whole or in part from surface sources.
(e) The State has the authority to de-
termine compliance or initiate enforce-
ment action based upon analytical re-
sults or other information compiled by
361
-------
§141.23
40 CFR Ch. I (7-1-04 Edition)
their sanctioned representatives and
agencies.
[40 FR 59570, Dec. 24, 1975, as amended at 45
FR 57344, Aug. 27. 1980; 47 FR 8998, Mar. 3,
1982; 47 FR 10998, Mar. 12, 1982; 54 FR 27527,
Jane 29, 1989; 59 PR 62466, Deo. 5, 1994; 65 FR
26022, May 4, 2000]
§ 141,23 Inorganic chemical sampling
and analytical requirements.
Community water systems shall con-
duct monitoring to determine compli-
ance with the maximum contaminant
levels specified In §141.62 in accordance
with this section. Non-transient, non-
community water systems shall con-
duct monitoring to determine compli-
ance with the maximum contaminant
levels specified in §141.62 in accordance
with this section. Transient, non-com-
munity water systems shall conduct
monitoring to determine compliance
with the nitrate and nitrite maximum
contaminant levels in §§141.11 and
141.62 (as appropriate) in accordance
with this section.
(a) Monitoring shall be conducted as
follows:
(1) Qroundwater systems shall take a
minimum of one sample at every entry
point to the distribution system which
is representative of each well after
treatment (hereafter called a sampling
point) beginning in the initial compli-
ance period. The system shall take
each sample at the same sampling
point unless conditions make another
sampling point more representative of
each source or treatment plant.
(2) Surface water systems shall take
a minimum of one sample at every
entry point to the distribution system
after any application of treatment or
in the distribution system at a point
which is representative of each source
after treatment (hereafter called a
sampling point) beginning in the ini-
tial compliance period. The system
shall take each sample at the same
sampling point unless conditions make
another sampling point more rep-
resentative of each source or treatment
plant.
NOTE: For purposes of this paragraph, sur-
face water systems include systems with a
combination of surface and ground sources.
(3) If a system draws water from
more than one source and the sources
are combined before distribution, the
system must sample at an entry point
to the distribution system during peri-
ods of normal operating conditions
(i.e., when water is representative of
all sources being used).
(4) The State may reduce the total
number of samples which must be
analyzed by allowing' the use of
compositing. Composite samples from
a maximum of five samples are al-
lowed, provided that the detection
limit of the method used for analysis is
less than one-fifth of the MCL.
Compositing of samples must be done
in the laboratory.
(i) If the concentration in the com-
posite sample is greater than or equal
to one-fifth of the MCL of any inor-
ganic chemical, then a follow-up sam-
ple must be taken within 14 days at
each sampling point included in the
composite. These samples must be ana-
lyzed for the contaminants which ex-
ceeded one-fifth of the MCL in the
composite sample. Detection limits for
each analytical method and MCLs for
each inorganic contaminant are the
following:
DETECTION LIMITS FOR INORGANIC CONTAMINANTS
Contaminant
MCL (mg/l)
0.006
Q.0106
7 MFL'
2 ..
0.004
Methodology
ICP-Mass Spectrometry
Atomic Absorption; Platform— Stabilized Temperature
Atomic Absorption: Platform
Detection limit
(mg/l)
0.003
0.0008 5
0.0004
0.001
0.001
0.00057
0.001
0.0014"
0.01 MFL
0.002
0 1
0.002 (0.001)
0.0002
0.00002s
362
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Environmental Protection Agency
§141.23
DETECTION LIMITS FOR INORGANIC CONTAMINANTS—Continued
Contaminant
Mercury .„.,„.,„.,„.,.,„.„.,,,,,,
Nickel
Nitrate
Nitrite , , ,
MCL (mart)
0005
0.1
0 2
0.002
xl
10 (as N)
1 (as Nj ...
005
0002
Methodology
Atomic Absorption; furnace technique
Inductively Coupled Plasma
Distillation, Amenable, Spectrophotometric4
Distillation, Selective Electrode3
Distillation, Spectrophotometric
Manual Cold Vapor Technique
Automated Cold Vapor Technique
Atomic Absorption; Platform
ICP-Mass Spectrometry
Automated Cadmium Reduction
Spectrophotometric
Automated Cadmium Reduction .
Manual Cadmium Reduction
Atomic Absorption; gaseous hydride
ICP-Mass Soectrometrv
Detection limit
(mg/1)
00003
00003
0.0001
0001
0001
0.007 (0.001)
002
0005
0.02
0.05
00005
0.0006
0.0002
0.0002
0.001
0.0006s
0005
0.0005
001
001
0.05
1
001
0.01
0.05
0.01
0004
0002
0,002
0001
000075
0.0003
1 MFL = million fibers per liter >10 urn.
2 Using a 2X preconcentration step as noted in Method 200.7, Lower MDLs may be achieved when using a 4X
preconcentration.
3 Screening method for total cyanides.
4 Measures "free" cyanides.
5 Lower MDLs are reported using stabilized temperature graphite furnace atomic absorption.
6The value for arsenic is effective January 23S 2006, Unit then, the MCL is 0-05 mg/L.
7 The MDL reported for EPA method 200.9 (Atomic Absorption; Platform—Stablized Temperature) was determined using a 2x
concenlration step during sample digestion- The MDL determined for samples analyzed using direct analyses (i.e., no sample di-
gestion) will be higher Using multiple depositions, EPA 200.9 is capable of obtaining MDL of 0.0001 mg/L.
s Using selective ion monitoring, EPA Method 200.8 (ICP-MS) is capable of obtaining a MDL of 0,0001 mg/L,
(11) If the population served by the
system is >3,300 persons, then
compositing may only be permitted by
the State at sampling points within a
single system. In systems serving 53,300
persons, the State may permit
compositing among different systems
provided the 5-sample limit is main-
tained,
(iii) If duplicates of the original sam-
ple taken from each sampling point
used in the composite sample are avail-
able, the system may use these instead
of resampling. The duplicates must be
analyzed and the results reported to
the State within 14 days after com-
pleting analysis of the composite sam-
ple, provided the holding time of the
sample is not exceeded.
(5) The frequency of monitoring for
asbestos shall be in accordance with
paragraph (b) of this section: the fre-
quency of monitoring for antimony, ar-
senic, barium, beryllium, cadmium,
chromium, cyanide, fluoride, mercury,
nickel, selenium and thallium shall be
in accordance with paragraph (c) of
this section; the frequency of moni-
toring for nitrate shall be in accord-
ance with paragraph (d) of this section;
and the frequency of monitoring' for ni-
trite shall be in accordance with para-
graph (e) of this section,
(b) The frequency of monitoring con-
ducted to determine compliance with
the maximum contaminant level for
asbestos specified in §141.62(b) shall be
conducted as follows:
363
-------
§141.23
40 CFR Ch. I (7-1-04 Edition)
(1) Bach community and non-tran-
sient, non-community water system is
required to monitor for asbestos during
the first three-year compliance period
of each nine-year compliance cycle "be-
ginning in the compliance period start-
ing January 1, 1993,
(2) If the system believes it is not
vulnerable to either asbestos contami-
nation in its source water or due to
corrosion of asbestos-cement pipe, or
both, it may apply to the State for a
waiYer of the monitoring requirement
in paragraph (b)(l) of this section. If
the State grants the waiver, the sys-
tem is not required to monitor,
(3) The State may grant a waiver
based on a consideration of the fol-
lowing factors:
(i) Potential asbestos contamination
of the water source, and
(ii) The use of asbestos-cement pipe
for finished water distribution and the
corrosive nature of the water.
(4) A waiver remains in effect until
the completion of the three-year com-
pliance period. Systems not receiving a
waiver must monitor in accordance
with the provisions of paragraph (b)(l)
of this section.
(5) A system vulnerable to asbestos
contamination due solely to corrosion
of asbestos-cement pipe shall take one
sample at a tap served by asbestos-ce-
ment pipe and under conditions where
asbestos contamination is most likely
to occur.
(6) A system vulnerable to asbestos
contamination due solely to source
water shall monitor in accordance with
the provision of paragraph (a) of this
section.
(7) A system vulnerable to asbestos
contamination due both to its source
water supply and corrosion of asbestos-
cement pipe shall take one sample at a
tap served by asbestos-cement pipe and
under conditions where asbestos con-
tamination is most likely to occur.
(8) A system which exceeds the max-
imum contaminant levels as deter-
mined in §141.23(i) of this section shall
monitor quarterly beginning in the
next quarter after the violation oc-
curred.
(9) The State may decrease the quar-
terly monitoring requirement to the
frequency specified in paragraph (b)(l)
of this section provided the State has
determined that the system is reliably
and consistently below the maximum
contaminant level. In no case can a
State make this determination unless
a groundwater system takes a min-
imum of two quarterly samples and a
surface (or combined surface/ground)
water system takes a minimum of four
quarterly samples.
(10) If monitoring data collected after
January 1, 1990 are generally con-
sistent with the requirements of
§141.23(b), then the State may allow
systems to use that data to satisfy the
monitoring requirement for the initial
compliance period beginning January
1, 1993.
(c) The frequency of monitoring con-
ducted to determine compliance with
the maximum contaminant levels in
§141.62 for antimony, arsenic, barium,
beryllium, cadmium, chromium, cya-
nide, fluoride, mercury, nickel, sele-
nium and thallium shall be as follows:
(1) Groundwater systems shall take
one sample at each sampling point dur-
ing each compliance period. Surface
water systems (or combined surface/
ground) shall take one sample annually
at each sampling point.
(2) The system may apply to the
State for a waiver from the monitoring
frequencies specified in paragraph (c)(l)
of this section. States may grant a
public water system a waiver for moni-
toring of cyanide, provided that the
State determines that the system is
not vulnerable due to lack of any in-
dustrial source of cyanide.
(3) A condition of the waiver shall re-
quire that a system shall take a min-
imum of one sample while the waiver is
effective. The term during which the
waiver is effective shall not exceed one
compliance cycle (i.e., nine years).
(4) The State may grant a waiver pro-
vided surface water systems have mon-
itored annually for at least three years
and groundwater systems have con-
ducted a minimum of three rounds of
monitoring. (At least one sample shall
have been taken since January 1, 1990).
Both surface and groundwater systems
shall demonstrate that all previous an-
alytical results were less than the max-
imum contaminant level. Systems that
use a new water source are not eligible
364
-------
Environmental Protection Agency
§141.23
for a waiver until three rounds of mon-
itoring from the new source have been
completed.
(5) In determining the appropriate re-
duced monitoring frequency, the State
shall consider:
(i) Reported concentrations from all
previous monitoring;
(ii) The degree of variation in re-
ported concentrations; and
(iii) Other factors which may affect
contaminant concentrations such as
changes in groundwater pumping rates,
changes in the system's configuration,
changes in the system's operating pro-
cedures, or changes in stream flows or
characteristics.
(6) A decision by the State to grant a
waiver shall be made in writing and
shall set forth the basis for the deter-
mination. The determination may be
initiated by the State or upon an appli-
cation by the public water system. The
public water system shall specify the
basis for its request. The State shall
review and, where appropriate, revise
its determination of the appropriate
monitoring frequency when the system
submits new monitoring data or when
other data relevant to the system's ap-
propriate monitoring frequency be-
come available.
(7) Systems which exceed the max-
imum contaminant levels as calculated
in §141.23(1) of this section shall mon-
itor quarterly beginning in the nest
quarter after the violation occurred.
(8) The State may decrease the quar-
terly monitoring requirement to the
frequencies specified in paragraphs
(c)(l) and (c)(2) of this section provided
it has determined that the system is
reliably and consistently below the
maximum contaminant level. In no
case can a State make this determina-
tion unless a groundwater system
takes a minimum of two quarterly
samples and a surface water system
takes a minimum of four quarterly
samples.
(9) All new systems or systems that
use a new source of water that begin
operation after January 22, 2004 must
demonstrate compliance with the MCL
within a period of time specified by the
State. The system must also comply
with the initial sampling frequencies
specified by the State to ensure a sys-
tem can demonstrate compliance with
the MCL. Routine and increased moni-
toring frequencies shall be conducted
in accordance with the requirements in
this section.
(d) All public water systems (commu-
nity; non-transient, non-community;
and transient, non-community sys-
tems) shall monitor to determine com-
pliance with the maximum contami-
nant level for nitrate in §141.62.
(1) Community and non-transient,
non-community water systems served
by groundwater systems shall monitor
annually beginning January 1, 1993;
systems served by surface water shall
monitor quarterly beginning January
1, 1993.
(2) For community and non-tran-
sient, non-community water systems,
the repeat monitoring frequency for
groundwater systems shall be quar-
terly for at least one year following
any one sample in which the con-
centration is >50 percent of the MCL.
The State may allow a groundwater
system to reduce the sampling fre-
quency to annually after four consecu-
tive quarterly samples are reliably and
consistently less than the MCL.
(3) For community and non-tran-
sient, non-community water systems,
the State may allow a surface water
system to reduce the sampling fre-
quency to annually if all analytical re-
sults from four consecutive quarters
are <50 percent of the MCL. A surface
water system shall return to quarterly
monitoring if any one sample is £50
percent of the MCL.
(4) Each transient non-community
water system shall monitor annually
beginning January 1,1993.
(5) After the initial round of quar-
terly sampling is completed, each com-
munity and non-transient non-commu-
nity system which is monitoring annu-
ally shall take subsequent samples dur-
ing the quarter(s) which previously re-
sulted in the highest analytical result.
(e) All public water systems (commu-
nity; non-transient, non-community;
and transient, non-community sys-
tems) shall monitor to determine com-
pliance with the maximum contami-
nant level for nitrite in § 141.62(b).
(1) All public water systems shall
take one sample at each sampling
365
-------
§141.23
40 CFR Ch. I (7-1-04 Edition)
point in the compliance period begin-
ning January 1, 1993 and ending Decem-
ber 31, 1995.
(2) After the initial sample, systems
where an analytical result for nitrite is
<50 percent of the MCL shall monitor
at the frequency specified by the State.
(3) For community, non-transient,
non-community, and transient non-
community water systems, the repeat
monitoring frequency for any water
system shall be quarterly for at least
one year following any one sample in
which the concentration is >50 percent
of the MCL. The State may allow a sys-
tem to reduce the sampling frequency
to annually after determining the sys-
tem is reliably and consistently less
than the MCL.
(4) Systems which are monitoring an-
nually shall take each subsequent sam-
ple during the quarter(s) which pre-
viously resulted in the highest analyt-
ical result.
(f) Confirmation samples:
(1) Where the results of sampling for
antimony, arsenic, asbestos, barium,
beryllium, cadmium, chromium, cya-
nide, fluoride, mercury, nickel, sele-
nium or thallium indicate an exceed-
ance of the maximum contaminant
level, the State may require that one
additional sample be collected as soon
as possible after the initial sample was
taken (but not to exceed two weeks) at
the same sampling point.
(2) Where nitrate or nitrite sampling
results indicate an exceedance of the
maximum contaminant level, the sys-
tem shall take a confirmation sample
within 24 hours of the system's receipt
of notification of the analytical results
of the first sample. Systems unable to
comply with the 24-hour sampling re-
quirement must immediately notify
persons served by the public water sys-
tem in accordance with §141.202 and
meet other Tier 1 public notification
requirements under Subpart Q of this
part. Systems exercising this option
must take and analyze a confirmation
sample within two weeks of notifica-
tion of the analytical results of the
first sample.
(3) If a State-required confirmation
sample is taken for any contaminant,
then the results of the initial and
confirmation sample shall be averaged.
The resulting average shall be used to
determine the system's compliance in
accordance with paragraph (i) of this
section. States have the discretion to
delete results of obvious sampling er-
rors.
(g) The State may require more fre-
quent monitoring than specified in
paragraphs (b), (c), (d) and (e) of this
section or may require confirmation
samples for positive and negative re-
sults at its discretion.
(h) Systems may apply to the State
to conduct more frequent monitoring
than the minimum monitoring fre-
quencies specified in this section.
(i) Compliance with §§141.11 or
141.62(b) (as appropriate) shall be deter-
mined based on the analytical result(s)
obtained at each sampling point.
(1) For systems which are conducting
monitoring at a frequency greater than
annual, compliance with the maximum
contaminant levels for antimony, ar-
senic, asbestos, barium, beryllium, cad-
mium, chromium, cyanide, fluoride,
mercury, nickel, selenium or thallium
is determined by a running annual av-
erage at any sampling point. If the av-
erage at any sampling point is greater
than the MCL, then the system is out
of compliance. If any one sample would
cause the annual average to be exceed-
ed, then the system is out of compli-
ance immediately. Any sample below
the method detection limit shall be
calculated at zero for the purpose of de-
termining the annual average. If a sys-
tem fails to collect the required num-
ber of samples, compliance (average
concentration) will be based on the
total number of samples collected.
(2) For systems which are monitoring
annually, or less frequently, the sys-
tem is out of compliance with the max-
imum contaminant levels for anti-
mony, arsenic, asbestos, barium, beryl-
lium, cadmium, chromium, cyanide,
fluoride, mercury, nickel, selenium or
thallium if the level of a contaminant
is greater than the MCL. If confirma-
tion samples are required by the State,
the determination of compliance will
be based on the annual average of the
initial MCL exceedance and any State-
required confirmation samples. If a
system fails to collect the required
number of samples, compliance (aver-
age concentration) will be based on the
total number of samples collected.
366
-------
Environmental Protection Agency
§141.23
(3) Compliance with the maximum
contaminant levels for nitrate and ni-
trate is determined based on one sam-
ple if the levels of these contaminants
are below the MCLs. If the levels of ni-
trate and/or nitrite exceed the MCLs in
the initial sample, a confirmation sam-
ple is required in accordance with para-
graph (f)(2) of this section, and compli-
ance shall be determined based on the
average of the initial and confirmation
samples.
(4) Arsenic sampling results will be
reported to the nearest 0.001 mg/L.
(j) Each public water system shall
monitor at the time designated by the
State during each compliance period.
(k) Inorganic analysis:
(1) Analysis for the following con-
taminants shall be conducted in ac-
cordance with the methods in the fol-
lowing table, or their equivalent as de-
termined by EPA, Criteria for ana-
lyzing arsenic, barium, beryllium, cad-
mium, calcium, chromium, copper,
lead, nickel, selenium, sodium, and
thallium with digestion or directly
without digestion, and other analytical
test procedures are contained in Tech-
nical Notes on Drinking Water Methods,
EPA-800/R-94--173, October 1994. This
document also contains approved ana-
lytical test methods which remain
available for compliance monitoring
until July 1, 1996. These methods will
not be available for use after July 1,
1996. This document is available from
the National Technical Information
Service, NTIS PB95^104766, U.S. De-
partment of Commerce, 5285 Port
Royal Road, Springfield, Virginia 22161.
The toll-free number is 800-553-6847.
Contaminant and
methodology13
1. Alkalinity;
Titrimetric
EPA
Bectrometric Nitration
ASTM3
D1067—
92B.
SM<
(18th, 19th
ed.)
2320 B
SM4
(20th ed.)
2320 B
Other
1-1030-
BS5
2. Antimony;
Inductively Coupled Plasma (ICP)— Mass Spec-
trometry.
Hydride-Atomic Absorption
Atomic Absorption; Platform ,..,,„., ,...,.,..„.
3, Arsenic: 1 4
Inductively Coupled Plasma15 ,...,.,, ,
ICP-Mass Spectrometry ...,.....,,., ,,„„ .,„...,.,
Atomic Absorption; Platform ,.,.,.,,„.,„.,,..,....
4. Asbestos:
Transmission Electron Microscopy ,,..,......,..,
Transmission Electron Microscopy >....,...,,..„.......
5. Barium:
Inductively Coupled Plasma .,..,...,...,,...,
Atomic Absorption; Direct ....,,.,.,.,..,....
Atomic Absorption; Furnace
6. Beryllium;
Inductively Coupled Plasma ..,..„...,...,...,.,......,.,,..,.,.
Atomic Absorption; Platform ..,,..,,..,
Atomic Absorption; Furnace .......,.,.,.,.„„.,.,.,.,.,.,.
7, Cadmium:
ICP-Mass Spectrornelry
8, Calcium:
Atomic Absorption; Direct Aspiration ,,.,,.,„.„
Inductively Coupled Plasma ,,.,......,.,...,
9, Chromium;
200.8 2-
200.9 2
20Q.72 .....
200,8 2,
200,9 2,
100.1 9.
1G0.210.
200.72 . ...
200 8 2
200.72 ._.,.
200 &*.
200.9 z.
2QQ72
200.8 2
200 9 2
200.7s
D3697-92
D2972-
97C.
D2972-
97B.
D3645—
97B.
D511—
93A.
D511—
93B,
3113 B
3120 8
3113 B
3114 B
3120 B
3111 D
3113 B
3120 B
3113B
3113 B
3500-Ca
D.
3111 B.
3120 B
3120 B
3120 B
3120 B
3500-Ca
3120 B
367
-------
§141.23
40 CFR Ch. I {7-1-04 Edition)
Contaminant and
methodology13
ICP-Mass Spectromeiry
Atomic Absorption; Platform
10. Copper:
Atomic Absorption; Direct Aspiration
Atomic Absorption; Platform
1 1 . Conductivity:
Conductance - .......
12. Cyanide:
Manual Distillation followed by
Spectrophotometrlc Manual
Spectrophotometrlc, Amenable
UV/Distiliation/Spectrophotometric
13. Fluoride;
Ion Chromatography ,
Manual Distill • Color SPADNS
Automated Alizarin . ,
14. Lead:
ICP-Mass spectrometry
Atomic Absorption; Platform
15. Magnesium:
ICP
16. Mercury:
Automated, Cold Vapor
IGP-Mass Spectrometry
17. Nickel:
inductively Coupled Piasma
iCP-Mass Spectrometry
Atomic Absorption; Direct
Atomic Absorption; Furnace
18. Nitrate:
Ion Chromatography
Automated Cadmium Reduction
Ion Selective Electrode
Manual Cadmium Reduction
19. Nitrite:
EPA
200.7s ....
200.8 2.
200.9 2.
200 7 2
200 82
200 92
335 4«
300.0s
200.82.
200.92.
200 72
2451 2
245.2-.
200. 8 2.
200.72
200 8 2
200.92.
300.08
3S3-28
ASTM3
D1688-
95C.
D1688-
95A.
D112S-
95A.
D2Q36-
98A.
D2036-
98A.
D2036-
98B.
D4327-97
D1179-
93B.
D3559-
96D.
D511-93 B
D51 1-93 A
D3223-97
D4327-97
D3867-
90A.
D3867-
90B.
SM4
(18th, 19th
ed.)
3120B
3113 B
3113 B
3111 B
3120 B
2510 B
4500-CN-
C.
45Q0-CN-
E.
4500-CN -
G.
4500-CN -
F.
4110 B
4500-F"
B.D.
4500-F"
C.
45QO-F~
E.
3113 B.
3111 B
3120 B
3500-Mg
E.
3112 B
3120 B
3111 B.
3113 B
4110 B
4500-
NOi- F.
4500-
NO,- D.
4500-
NOj- E.
SM"
(20th ed.)
3120 B
3120 B
2510 B
4SOO-CN-
C.
4500-CN -
E.
4500-CN-
G.
4500-CN-
F.
4110 B.
45QQ-F-
B.D.
4500-F-
C.
4500-F-
E.
3120 B
3500-Mg
B.
3120 B.
4110 B
4500-
NO.- F.
4500-
NO,- D.
4500-
NO3- E.
Other
I-3300-
85 5
Kelada
01"
QuikChem
10-204-
00-1-
Xie
380-
75WE"
29-71W"
Method
1001 16
B-1011"
601 7
368
-------
Environmental Protection Agency
§141.23
Contaminant and
methodology13
Manual Cadmium Reduction ..........,..,...,..,,.„......,....
20. Ortho-phosphate: 1£
Colori metric, Automated, Ascorbic Acid ,.
Automated -segmented Flow; ,..,.,,,,,,.,
Automated Discrete ........„.,.,.,.,<„„,..,.,.......
21. pH:
22. Selenium;
!CP-Mass Spectrcmetry ,...,.,,,.„.,.,....,.,
Atomic Absorption; Platform .... ,....,........,...,,.,„
Atomic Absorption; Furnace
23. Silica;
Automated-segmented Flow ,,..,.,.,.,...
Automated tor Molybcl ate- reactive Silica ..,.,.,...,..,....
Inductively Coupled Plasma .,...,.,.,.,, .......,.,.,....,»>
24. Sodium;
25, Temperature:
26. Thallium;
ICP-Mass Spectrometry
Atomic Absorption; Platform ,.......„,..,.,.,.,.,.,..
EPA
300 O6
3S3.26
365,1s
300 O6
150.1 1
150.21.
200.8 2>
200.9 2.
200.72 .....
200 7 2
..
200.8 z,
200.92.
ASTM3
D4327-97
D3867-
90A.
03867-
908.
D515-88A
D4327-97
D1 293-95
D3859-
98A.
D3859-
98B.
D859-95.
SM"
(18th, 19th
ed.)
4110 B
4500-
NO.i-.
4SOO-
NOi- E.
4500-
NQ2~~ B.
4500-P F
4500-P E
4110 B ..
4500-H*
B.
3114 B.
3113 B.
4500-Sl D
4500-Si E
4500-Si F
3120 B
3111 B
2550
SM<
(20th ed.)
4110 B
4500-
NOi- F.
4500-
NO,- E.
4500
NO2~ B.
4500-P F.
4500-P E.
4110 B
4500-H +
B.
4500-SiOi
C.
4500-SiO,
D.
4500-SiO3
E.
3120 B.
2550.
Other
B-1011"
1-1601-
85s
1-2601-
90s
1-2598-
85s
1-1700-
85s
I-27QO-
85 5
The procedures shall be dons in accordance with the documents listed below. The incorporation by reterence of the following
documents listed in footnotes 1-11 and 16 was approved by the Director of the Federal Register in accordance with 5 U.S.C.
552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources fisted below. Information regarding ob-
taining these documents can be obtained from the Safe Drinking Water Hotline at 800-^26^*791, Documents may be inspected
at EPA'sDrinking Water Docket, EPA West, 1301 Constitution Avenue, NW, Room B135, Washington. DC (Telephone: 202-
566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at
NARA, call 202-741-6030. or go to: http://www.archives.govflederal register/code^ of federal regulations/ibr locations.html.
1 "Methods for Chemteal'Analysis of Water and Wastes*. EPA/60074-79/020, March 1983. Avaltabfe at NTIS. PB84-128677.
'"Methods for the Determination of Metals in Environmental Samples—Supplement I", EPA/8QQ/R-94/111, May 1994. Avail-
able at NTIS, PB9S-125472.
3 Annual Book of ASTM Standards, 1994, 1996, or 1999, Vols. 11.01 and 11.02, ASTM International; any year containing the
cited version of the method may be used. The previous versions of D1688-95A, D1688-95C (copper), D3559-95D (lead),
D1293-95 (pH). D1125-91A (conductivity) and D859-94 (silica) are also approved. These previous versions D1688-90A, C;
D3559-90D, D1293-84, D1125-91A and D859-88, respectively are located in the Annual Book of ASTM Standards, 1994, Vol.
11.01. Copies may be obtained from ASTM International, 100 Barr Harbor Drive, West Conshobocken, PA 19428.
•'Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition
(1998). American Public Health Association, 1015 Fifteenth Street, NW, Washington, DC 20005. The cited methods published in
any of these three editions may be used, except that the versions of 3111 B, 31 f 1 D, 3113 B and 3114 B in the 20th edition
may not be used.
5 Method 1-2601-90, Methods for Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of
Inorganic and Organic Constituents in Water and Fluvial Sediment, Open File Report 93-125, 1993; For Methods 1-1030-65; I-
1601-85,1-1700-85; I-2598-85; I-2700-85; and t-3300^85 See Techniques of Water Resources Investigation of the U.S. Geo-
logical Survey, Book 5, Chapter A-1, 3rd ed., 1989; Availabie from Information Services, U.S. Geoiogica! Survey, Federal Cen-
ter, Box 25286, Denver, CO 80225-0425.
6 "Methods for the Determination of Inorganic Substances in Environmental Samples", EPA/600/R-93/1QO, August 1993. Avail-
able at NTIS, PB94-120821.
369
-------
§141,23
40 CFR Ch. I (7-1-04 Edition)
7The procedure shall be done in accordance with the Technical Bulletin 601 "Standard Method of Test for Nitrate in Drinking
Water", July 1994, PN 221890-001, Analytical Technology, Inc. Copies may be obtained from ATI Orion, 529 Main Street, Bos-
ton, MA 02129.
8Method B-1011, "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chroma-
tography," August 198T. Copies may be obtained from Waters Corporation, Technical Services Division, 34 Maple Street, Mil-
ford, MA 01757.
'Method 100.1. "Analytical Method For Determination of Asbestos Fibers in Water", EPA/600/4-83/043, EPA, September
1983. Available at NTIS, PB83-260471.
10Method 100.2, "Determination of Asbestos Structure Over 10nm In Length In Drinking Water", EPA/600/R-94/134, June
1994. Available at NTIS, PB94-201902.
11 Industrial Method No. 129-71W, "Fluoride in Water and Wastewater", December 1972, and Method No. 380-75WE, "Fluo-
ride in Water and Wastewafer", February 1976, Technieon Industrial Systems. Copies may be obtained from Bran £ Luebbe,
1025 Busch Parkway, Buffalo Grove, IL 60089.
12Unflltered, no digestion or hydrolysis.
13 Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2X preconcentration step during sample
digestion, MDLs determined when samples are analyzed by direct analysis (i.e., no sample digestion) will be higher. For direct
analysis of cadmium and arsenic by Method 200.7, and arsenic by Method 3120 B sample preconcentration using pneumatic
nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of anti-
mony, lead, and thallium by Method 200 9; antimony and lead by Method 3113 B; and lead by Method D3559-90D unless mul-
tiple in-furnace depositions are made.
14 If ultrasonic nebulization is used in the determination of arsenic by Methods 200,7, 200.8, or SM 3120 B, the arsenic must
be in the pentavalent state to provide uniform signal response. For methods 200.7 and 3120 B, both samples and standards
must be diluted in the same mixed acid matrix concentration of nitric and hydrochloric acid with the addition of 100 |iL of 30%
hydrogen peroxide per 10prnl of solution. For direct analysis of arsenic with method 200.8 using ultrasonic nebulization, samples
and standards must contain one mg/L of sodium hypoehlorite.
1sStarting January 23, 2006, analytical methods using the ICP-AES technology, may not be used because the detection limits
for these methods are 0.008 mg,'L or higher. This restriction means that the two ICP-AES methods (EPA Method 200.7 and SM
3120 B) approved for use for the MCL of Q.05 mg/L may not be used for compliance determinations for the revised MCL of
0.010 mg/L. However, prior to January 23, 2006, systems may have compliance samples analyzed with these less sensitive
methods.
16The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395,
Erianger, KY 41018. Or from the Hach Company, P.O. Box 389, Loveland, CO 80539,
17 The description for the Kelada 01 Method, "Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide,
And Thiocyanate", Revision 1.2, August 2001, EPA # 821-B-01-009 for cyanide is available from the National Technical Infor-
mation Service (NTIS), PB 2001-108275, 5285 Port Royal Road, Springfield, VA 22161. The toll free telephone number is 800-
553-6847.
18The description for the QuikChem Method 10-204—00-1-X, "Digestion and distillation of total cyanide in drinking and
wastewaters using MICRO DIST and determination of cyanide by flow injection analysis". Revision 2.1, November 30, 2000 for
cyanide is available from Lachat Instruments, 6645 W. Mill Bd., Milwaukee, Wl 53218, USA. Phone: 414-358-4200.
(2) Sample collection for antimony,
arsenic, asbestos, barium, beryllium,
cadmium, chromium, cyanide, fluoride,
mercury, nickel, nitrate, nitrite, sele-
nium, and thallium under this section
shall be conducted using the sample
preservation, container, and maximum
holding time procedures specified in
the table below:
Contaminant
Thallium
Preservative 1
HNO3
Con-
I tainer2
. p or G
Time3
6 months
Contaminant
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium ..,,....
Cyanide
Fluoride
Mercury
Nickel
Nitrate
Nitrate-Nitrite6
Nitrite , ,
Selenium
Preservative 1
HNO3
Cone HNOi to
pH<2.
4 °C
HNO3
HNO3
HNO3
HNO3
4 »C, NaOH ....
None
HNO3
HNO3
4°C
H-"SO4
4°C
HNO3
Con-
tainer2
Pare
PorG
P or G
P or G
PorG
PorG
PorG
PorG
P or G
P or G
PorG
PorG
PorG
PorG
PorG
Time3
6 months
6 months
6 months
6 months
6 months
6 months
14 days
1 month
28 days
48 hours5
28 days
6 months
1 For cyanide determinations samples must be adjusted with
sodium hydroxide to pH 12 at the time off collection. When
chilling is indicated the sample must be shipped and stored at
4 °C or less. Acidification of nrtrate or metals samples may be
with a concentrated acid or a dilute (§0% by volume) solution
of the applicable concentrated acid. Acidification of samples
for metals analysis is encouraged and allowed at the labora-
tory rather than at the time of sampling provided the shipping
time and other instructions in Section 8.3 of EPA Methods
200.7 or 200.8 or 200,9 are followed,
2 P=plastic, hard or soft; G=glass, hard or soft.
3 In all cases samples should be analyzed as soon after col-
lection as possible. Follow additional (if any) information on
preservation, containers or holding times that is specified in
method.
4 Instructions for containers, preservation procedures and
holding times as specified in Method 100.2 must be adhered
to for all compliance analyses including those conducted with
Method 100.1.
si& the sample is chlorinated, the holding time for an
unacidified sample kept at 4 °C is extended to 14 days,
6 Nitrate-Nitrite refers to a measurement of total nitrate.
(3) Analysis under this section shall
only be conducted by laboratories that
have been certified by EPA or the
State. Laboratories may conduct sam-
ple analysis under provisional certifi-
cation until January I, 1996. To receive
certification to conduct analyses for
antimony, arsenic, asbestos, barium,
beryllium, cadmium, chromium, cya-
nide, fluoride, mercury, nickel, nitrate,
nitrite and selenium and thallium, the
laboratory must:
370
-------
Environmental Protection Agency
§141.24
(i) Analyze Performance Evaluation
(PE) samples provided by EPA, the
State or by a third party (with the ap-
proval of the State or EPA) at least
once a year.
(ii) For each contaminant that has
been included in the PE sample and for
each method for which the laboratory
desires certification achieve quan-
titative results on the analyses that
are within the following acceptance
limits:
Contaminant
Arsenic ...,.,.,.. ....,.,.
Barium
Beryllium ,.„,.,.,. ..,„,.„,..,
Fluoride ,.....,, ,...„.,.,.,.,.,.
Nickel ,.,.,,,.,
Nitrate
Nitrite
Selenium ,...,.......,........,»,.,,,,..
Thallium .„,....,,..,..........,.,..„..
Acceptance limit
±30 at £0.006 mg/1
±30 at £0.003 mg/L
on study statistics.
±15% at 20. 15 mg/1
±15% at ^0.001 mg/1
±20% at =-0.002 mg/1
+15% at ^0.01 mg/1
±25% at ^0.1 mg/1
±10% at £1 to 10 mg/1
±30% at £0.0005 mg/1
±15% at ^0.01 mg/1
±10% at =-0.4 mg/1
±15% at >04 mg/1
±20% at £0,01 mg/1
±30% at 50.002 mg/1
(1) Analyses for the purpose of deter-
mining compliance with §141.11 shall be
conducted using the requirements spec-
ified in paragraphs (1) through (q) of
this section.
(1) Analyses for all community water
systems utilizing surface water sources
shall be completed by June 24, 1978.
These analyses shall be repeated at
yearly intervals.
(2) Analyses for all community water
systems utilizing only ground water
sources shall be completed by June 24,
1979. These analyses shall be repeated
at three-year intervals.
(3) For non-community water sys-
tems, whether supplied by surface or
ground sources, analyses for nitrate
shall be completed by December 24,
1980. These analyses shall be repeated
at intervals determined by the State.
(4) The State has the authority to de-
termine compliance or initiate enforce-
ment action based upon analytical re-
sults and other information compiled
by their sanctioned representatives and
agencies.
(m) If the result of an analysis made
under paragraph (1) of this section indi-
cates that the level of any contami-
nant listed in §141.11 exceeds the max-
imum contaminant level, the supplier
of the water shall report to the State
within 7 days and initiate three addi-
tional analyses at the same sampling
point within one month.
(n) When the average of four analyses
made pursuant to paragraph (m) of this
section, rounded to the same number of
significant figures as the maximum
contaminant level for the substance In
question, exceeds the maximum con-
taminant level, the supplier of water
shall notify the State pursuant to
§141.31 and give notice to the public
pursuant to subpart Q. Monitoring1
after public notification shall be at a
frequency designated by the State and
shall continue until the maximum con-
taminant level has not been exceeded
in two successive samples or until a
monitoring schedule as a condition to a
variance, exemption or enforcement
action shall become effective.
(o) The provisions of paragraphs (m)
and (n) of this section notwithstanding,
compliance with the maximum con-
taminant level for nitrate shall be de-
termined on the basis of the mean of
two analyses. When a level exceeding
the maximum contaminant level for
nitrate is found, a second analysis shall
be initiated within 24 hours, and If the
mean of the two analyses exceeds the
maximum contaminant level, the sup-
plier of water shall report his findings
to the State pursuant to §141.31 and
shall notify the public pursuant to sub-
part Q.
(p) For the initial analyses required
by paragraph (1) (1), (2) or (3) of this
section, data for surface waters ac-
quired within one year prior to the ef-
fective date and data for ground waters
acquired within 3 years prior to the ef-
fective date of this part may be sub-
stituted at the discretion of the State.
(q) [Reserved]
[56 FR 3579, Jan. 30, 1991, as amended at 56
FR 30274, July 1, 1991; 57 FR 31838, July 17,
1992; 59 FR 34322, July 1, 1994; 59 FR 62486,
Dec. 5, 1994; 60 FR 34085, June 29, 1995;
64 FR 87461, Dec. 1, 1999; 65 FR 26022, May 4.
2000; 66 FR 7061, Jan. 22, 2001; 67 FR 65246,
Oct. 23, 2002; 67 FR 65897, Oct. 29, 2002; 67 FR
68911, Nov. 13, 2002: 68 FR 14506, Mar. 25, 2003]
§ 141.14 Organic chemicals, sampling
and analytical requirements.
(a)-(d) [Reserved]
(e) Analyses for the contaminants in
this section shall be conducted using
371
-------
§141.24
40 CFR Ch. I (7-1-04 Edition)
the following EPA methods or their
equivalent as approved by EPA.
(1) The following documents are in-
corporated by reference. This incorpo-
ration by reference was approved by
the Director of the Federal Register in
accordance with 5 U.S.C. 552(a) and 1
CPU part 51. Copies may be inspected
at EPA's Drinking Water Docket, 1301
Constitution Avenue, NW., EPA West,
Room B102, Washington DC 20460 (Tele-
phone: 202-566-2426); or at the National
Archives and Records Administration
(NARA), For information on the avail-
ability of this material at NARA, call
202-741-6030, or go to: http://
www.archives.gov/federal register/
code _of federal regulations/
ibr^locations.html. Method 508A and
515.1 are in Methods for the Determina-
tion of Organic Compounds in Drinking
Water, EPA/6QO/4-88-039, December 1988,
Revised, July 1991. Methods 547, 550 and
550.1 are in Methods for the Determina-
tion of Organic Compounds in Drinking
Water—Supplement I, EPA/600-4-90-020,
July 1990. Methods 548.1, 549.1, 552.1 and
555 are in Methods for the Determination
of Organic Compounds in Drinking
Water—Supplement II, EPA/600/R-93-129,
August 1992. Methods 502.2, 504.1, 505,
506, 507, 508, 508.1, 515.2, 524.2, 525.2,
531.1, 551.1 and 552.2 are in Methods for
the Determination of Organic Compounds
in Drinking Water—Supplement III, EPA/
600/R-95-131, August 1995. Method 1613
is titled "Tetra-through Octa-
Chlorinated Dioxins and Furans by Iso-
tope-Dilution HRGC/HRMS", EPA/821-
B-94-Q05, October 1994. These docu-
ments are available from the National
Technical Information Service, NTIS
PB91-231480, PB91-146027, PB92-207703,
PB95-261616 and PB95-104774, U.S. De-
partment of Commerce, 5285 Port
Royal Road, Springfield, Virginia 22161.
The toll-free number is 800-553-6847.
Method 6651 shall be followed in ac-
cordance with Standard Methods for the
Examination of Water and Wastewater,
18th edition (1992), 19th edition (1995),
or 20th edition (1998), American Public
Health Association (APHA); any of
these three editions may be used.
Method 6610 shall be followed in ac-
cordance with Standard Methods for the
Examination of Water and Wastewater,
(18th Edition Supplement) (1994), or with
the 19th edition (1995) or 20th edition
(1998) of Standard Methods for the Exam-
ination of Water and Wastewater; any of
these three editions may be used. The
APHA documents are available from
APHA, 1015 Fifteenth Street NW.,
Washington, D.C. 20005. Other required
analytical test procedures germane to
the conduct of these analyses are con-
tained in Technical Notes on Drinking
Water Methods, EPA/600/R-94-173, Octo-
ber 1994, NTIS PB95-104766. EPA Meth-
ods 515.3 and 549.2 are available from
U.S. Environmental Protection Agen-
cy, National Exposure Research Lab-
oratory (NERL)-Cincinnati, 26 West
Martin Luther King Drive, Cincinnati,
OH 45268. ASTM Method D 5317-93 is
available in the Annual Book of ASTM
Standards, (1999), Vol. 11.02, ASTM
International, 100 Barr Harbor Drive,
West Conshohocken, PA 19428, or in
any edition published after 1993. EPA
Method 515.4, "Determination of
Chlorinated Acids in Drinking Water
by Liquid-Liquid Microextraction,
Derivatization and Fast Gas Chroma-
tography with Electron Capture Detec-
tion," Revision 1.0, April 2000, EPA /815/
B-00/001 can be accessed and
downloaded directly on-line at
www.epa.gov/safewater/methods/
sourcalt.html. The Syngenta AQ-625,
"Atrazine in Drinking Water by
Immunoassay", February 2001 is avail-
able from Syngenta Crop Protection,
Inc., 410 Swing Road, Post Office Box
18300, Greensboro, NC 27419, Phone-
number (336) 632-6000. Method 531.2
"Measurement of N-
methylcarbamoyloximes and N-
methvlcarbamates in Water by Direct
Aqueous Injection HPLC with
Postcolumn Derivatization." Revision
1.0, September 2001, EPA 815/B/01/002
can be accessed and downloaded di-
rectly on-line at www.epa.gov/safewater/
methods/sourcalt. html.
Contaminant
1 EPA meth-
od1
5022
I 524.2.
Standard AQTH
methods 1 Ab™
;
j
Other
372
-------
Environmental Protection Agency
§141.24
Contaminant
6. 1 ,2-Dichloroethane
11- Ethylbenzene
14 1 1 1 -Trichloroethane
18, 1,1-Dichloroethylene
18 1 1 ,2-Trlcnloroethane
20. Vinyl chloride
21 Xylenes (total)
22 237 S-TCDD (dioxin)
23. 2,4-D4 (as acid, salts and esters)
24 2 4,5-TP 4 (Silvex)
25. Alachlor2 .
28. Carbofuran ,
29 Chlordane ..
EPA meth-
od'
502.2,
524.2,
551.1.
502.2,
S24.2.
502.2,
524,2.
502.2,
524.2.
S02.2,
S24.2.
502.2,
S24.2.
502,2,
324,2.
502.2,
524.2.
502.2,
524.2,
502.2,
524.2.
502.2,
524.2.
502.2,
524,2,
551.1.
502.2,
524.2,
SS1.1.
502.2,
524.2,
551.1.
502.2,
524 .2.
502.2,
524.2.
502.2,
524.2.
502.2,
524.2,
551.1.
502.2,
524.2.
502.2,
524.2.
1613
515.2, 555,
515.1,
515,3,
515.4.
515.2, 555,
515.1,
515.3.
515.4.
507, 525.2,
508.1,
505,
551.1.
507, 525 2
508.1,
505,
551.1.
52S.2, 550
550.1.
531.1,
531.2.
508 5252,
508.1,
505.
Standard
methods
6610.
ASTM
D5317-93.
D5317-93.
Other
AG-625.
373
-------
§141.24
40 CFR Ch, I (7-1-04 Edition)
Contaminant
31 Di(2-ethylhexyl)adipate
32 Di{2-ethylhexyl)phihalate
33, Dibromochioropropane (DI
34, Dinoseb4
36 Endothall
37 Endrin » ».
38, Ethylene dibromide (EDB)
39 Glyphosate .
40 Heptaehlor
43. Hexachlorocyclopentadien
46. Oxamyl
47. RGBs' (as decachlorobiph
48 PCBs * (as Aroclors)
JCP)
EPA meth-
od1
552.1,
515.1,
552.2,
515.3,
515.4.
506, 525.2.
506, 525.2.
504.1,
551.1.
515.2, 555,
515.1,
515.3,
515.4.
549.2.
548.1.
508, 525.2,
508.1,
505,
551.1.
504.1,
551.1.
547
508, 525.2,
508.1,
505,
551.1.
508, 525.2,
508.1,
505,
551.1.
508, 525.2,
508.1,
505,
551.1.
508, 525.2,
508.1,
505,
551.1.
508, 525.2,
508.1,
505,
551.1.
508, 525.2,
508.1,
505,
551.1.
531.1,
531.2.
508A.
508.1,508,
525.2,
505.
515.2,
525.2,
555,
515.1,
515.3,
515.4.
515.2, 555,
515.1,
515.3,
515.4.
507, 525.2,
508.1,
505,
551.1.
508,508.1,
525.2,
505.
Standard
methods
6651.
6610.
ASTM
D5317-93.
D5317-93.
Other
374
-------
Environmental Protection Agency
§141.24
Contaminant
EPAmeth- i
od<
502.2, 1
524.2, |
551.1.
Standard
methods
ASTM
Other
1 For previously approved EPA methods which remain available tor compliance monitoring until June 1 , 2001 , see paragraph
(e)(2) of this section.
Substitution of the detector specified in Method 505, 507, 508 or 508.1 for the purpose ot achieving lower detection limits is
allowed as follows. Either an electron capture or nitrogen phosphorous detector may be used provided all regulatory require-
ments and quality control criteria are met.
3 PCBs are qualitatively Identified as Aroclors and measured for compliance purposes as decachlorobiphenyl. Users of Method
505 may
4Accu
515.2, 515.3, 515.4 and 555 and ASTM Method D5317-93
.
ay have more difficulty in achieving the required detection limits than users of Methods 508.1. 525 2 or 508,
curate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA Methods 515.1,
(2) The following- EPA methods
remain available for compliance moni-
toring until June 1. 2001, The following-
documents are incorporated by ref-
erence. This incorporation by reference
was approved by the Director of the
Federal Register in accordance with 5
U.S.C. 552(a) and 1 CFR Part 51. Copies
may be inspected at EPA's Drinking
Water Docket, 401 M St.. SW., Wash-
ington, DC 20460; or at the National Ar-
chives and Records Administration
(NARA). For information on the avail-
ability of this material at NARA. call
202-741-6030. or go to; http:/-'
www.archives.gov/federal register/
code^ of _ federal ^regulations/
ibr^ locations.html. EPA methods 502.2
Rev". 2.0, 505 Rev. 2.0, 507 Rev. 2.0, 508
Rev, 3.0. 531.1 Rev. 3.0 are in "Methods
for the Determination of Organic Com-
pounds in Drinking Water", December
1988, revised July 1991: methods 506 and
551 are in "Methods for the Determina-
tion of Organic Compounds in Drinking-
Water—Supplement I". July 1990; meth-
ods 515.2 Rev. 1,0 and 524.2 Rev. 4.0 are
in "Methods for the Determination of
Organic Compounds in Drinking
Water^Supplement II," August 1992:
and methods 504.1 Rev. 1.0. 508.1 Rev.
1.0, 525.2 Rev.1.0 are available from US
EPA NERL, Cincinnati, OH 45268
(f) Beginning with the initial compli-
ance period, analysis of the contami-
nants listed in §141.61! a) (1) through
(21) for the purpose of determining
compliance with the maximum con-
taminant level shall be conducted as
follows:
(1) Groundwater systems shall take a
minimum of one sample at every entry
point to the distribution system which
is representative of each well after
treatment (hereafter called a sampling
point). Each sample must be taken at
the same sampling point unless condi-
tions make another sampling point
more representative of each source,
treatment plant, or within the dis-
tribution system.
(2) Surface water systems (or com-
bined surface/ground) shall take a min-
imum of one sample at points in the
distribution system that are represent-
ative of each source or at each entry
point to the distribution system aftes-
treatment (hereafter called a sampling-
point). Bach sample must be taken at
the same sampling point unless condi-
tions make another sampling point
more representative of each source.
treatment plant, or within the dis-
tribution system,
(33 If the system draws water from
more than one source and the sources
are combined before distribution, the
system must sample at an entry point
to the distribution system during- peri-
ods of normal operating conditions
(i.e.. when water representative of all
sources is being used).
(4) Each community and non-tran-
sient non-community water system
shall take four consecutive quarterly
samples for each contaminant listed in
§141.61(a) (2) through (21) during each
compliance period, beginning in the
initial compliance period,
(5) If the initial monitoring for con-
taminants listed in §141.61(a) (1)
through (8) and the monitoring for the
contaminants listed in §141.61(a) (9)
through (21) as allowed in paragraph
(f)C18) has been completed by December
31, 1992, and the system did not detect
any contaminant listed in §141.61(a) (1)
through (21), then each ground and sur-
face water system shall take one sam-
ple annually beginning with the initial
compliance period.
375
203-160 D-13
-------
§141.24
40 CFR Ch. 1 (7-1-04 Edition)
(6) After a minimum of three years of
annual sampling, the State may allow
groundwater systems with, no previous
detection of any contaiminant listed in
§141.61(a) to take one sample during
each compliance period.
(7) Each community and non-tran-
sient non-community ground water
system which does not detect a con-
taminant listed in §141.61(a) (1)
through (21) may apply to the State for
a waiver from the requirements of
paragraphs (f)(5) and (f)(6) of this sec-
tion after completing the initial moni-
toring. (For purposes of this section,
detection is defined as 20.0005 rng/1.) A
waiver shall be effective for no more
than six years (two compliance peri-
ods). States may also issue waivers to
small systems for the initial round of
monitoring for 1,2,4-trichlorobenzene.
(8) A State may grant a waiver after
evaluating the following' factor(s):
(i) Knowledge of previous use (includ-
ing transport, storage, or disposal) of
the contaminant within the watershed
or zone of influence of the system. If a
determination by the State reveals no
previous use of the contaminant within
the watershed or zone of influence, a
waiver may be granted.
(ii) If previous use of the contami-
nant is unknown or it has been used
previously, then the following factors
shall be used to determine whether a
waiver is granted.
(A) Previous analytical results.
(B) The proximity of the system to a
potential point or non-point source of
contamination. Point sources include
spills and leaks of chemicals at or near
a water treatment facility or at manu-
facturing, distribution, or storage fa-
cilities, or from hazardous and munic-
ipal waste landfills and other waste
handling or treatment facilities.
(C) The environmental persistence
and transport of the contaminants.
(D) The number of persons served by
the public water system and the prox-
imity of a smaller system to a larger
system.
(B) How well the water source is pro-
tected against contamination, such as
whether it is a surface or groundwater
system, Groundwater systems must
consider factors such as depth of the
well, the type of soil, and wellhead pro-
tection. Surface water systems must
consider watershed protection.
(9) As a condition of the waiver a
groundwater system must take one
sample at each sampling point during
the time the waiver is effective (i.e.,
one sample during two compliance pe-
riods or six years) and update Its vul-
nerability assessment considering the
factors listed in paragraph (f)(8) of this
section. Based on this vulnerability as-
sessment the State must reconfirm
that the system is non-vulnerable. If
the State does not make this recon-
firmation within three years of the ini-
tial determination, then the waiver is
invalidated and the system is required
to sample annually as specified in
paragraph (5) of this section.
(10) Each community and non-tran-
sient non-community surface water
system which does not detect a con-
taminant listed in §141.61(a) (1)
through (21) may apply to the State for
a waiver from the requirements of (f)(5)
of this section after completing the ini-
tial monitoring. Composite samples
from a maximum of five sampling
points are allowed, provided that the
detection limit of the method used for
analysis is less than one-fifth of the
MOL. Systems meeting this criterion
must be determined by the State to be
non-vulnerable based on a vulner-
ability assessment during- each compli-
ance period. Each system receiving a
waiver shall sample at the frequency
specified by the State (if any).
(11) If a contaminant listed in
§141.61(a) (2) through (21) is detected at
a level exceeding 0.0005 mg/1 in any
sample, then:
(i) The system must monitor quar-
terly at each sampling point which re-
sulted in a detection.
(ii) The State may decrease the quar-
terly monitoring requirement speci
fied in paragraph (f)(ll)(i) of this sec-
tion provided it has determined that
the system is reliably and consistently
below the maximum contaminant
level. In no case shall the State make
this determination unless a ground-
water system takes a minimum of two
quarterly samples and a surface water
system takes a minimum of four quar-
terly samples.
(iii) If the State determines that the
system is reliably and consistently
376
-------
Environmental Protection Agency
§141.24
below the MCL, the State may allow
the system to monitor annually. Sys-
tems which monitor annually must
monitor during the quarter(s) which
previously yielded the highest analyt-
ical result.
(iv) Systems which have three con-
secutive annual samples with no detec-
tion of a contaminant may apply to the
State for a waiver as specified in para-
graph (f)(7) of this section.
(v) Groundwater systems which have
detected one or more of the following1
two-carbon organic compounds: tri-
chloroethylene, tetrachloroethylene,
1,2-dichloroethane, 1,1,1-trichloro-
ethane, cis-l,2-dichloroethylene, trans-
1,2-dichloroethylene, or 1,1-
dichloroethylene shall monitor quar-
terly for vinyl chloride. A vinyl chlo-
ride sample shall be taken at each sam-
pling point at which one or more of the
two-carbon organic compounds was de-
tected. If the results of the first anal-
ysis do not detect vinyl chloride, the
State may reduce the quarterly moni-
toring frequency of vinyl chloride mon-
itoring to one sample during each com-
pliance period. Surface water systems
are required to monitor for vinyl chlo-
ride as specified by the State.
(12) Systems which violate the re-
quirements of §141.61(a) (1) through
(21). as determined by paragraph (f)(15)
of this section, must monitor quar-
terly. After a minimum of four con-
secutive quarterly samples which show
the system is in compliance as speci-
fied in paragraph (f)(15) of this section
the system and the State determines
that the system is reliably and consist-
ently below the maximum contaminant
level, the system may monitor at the
frequency and times specified in para-
graph (f)(ll)(iii) of this section.
(13) The State may require a con-
firmation sample for positive or nega-
tive results. If a confirmation sample is
required by the State, the result must
be averaged with the first sampling re-
sult and the average is used for the
compliance determination as specified
by paragraph (f)(15). States have discre-
tion to delete results of obvious sam-
pling errors from this calculation,
(14) The State may reduce the total
number of samples a system must ana-
lyze by allowing the use of
compositing. Composite samples from
a maximum of five sampling points are
allowed, provided that the detection
limit of the method used for analysis is
less than one-fifth of the MCL.
Compositing of samples must be done
in the laboratory and analyzed within
14 days of sample collection,
(i) If the concentration in the com-
posite sample is greater than or equal
to 0.0005 mg/1 for any contaminant list-
ed in §141.61(a). then a follow-up sam-
ple must he taken within 14 days at
each sampling point included in the
composite, and be analyzed for that
contaminant.
(ii) If duplicates of the original sam-
ple taken from each sampling point
used in the composite sample are avail-
able, the system may use these instead
of resampling. The duplicates must be
analyzed and the results reported to
the State within 14 days after com-
pleting analysis of the composite sam-
ple, provided the holding time of the
sample is not exceeded.
(iii) If the population served by the
system is > 3,300 persons, then
compositing may only be permitted by
the State at sampling points within a
single system. In systems serving <
3,300 persons, the State may permit
compositing among different systems
provided the 5-sample limit is main-
tained.
(iv) Compositing samples prior to GC
analysis.
(A) Add 5 ml or equal larger amounts
of each sample (up to 5 samples are al-
lowed) to a 25 ml glass syringe. Special
precautions must be made to maintain
zero headspace in the syringe.
(B) The samples must be cooled at 4
°C during this step to minimize vola-
tilization losses.
(C) Mix well and draw out a 5-ml ali-
quot for analysis.
(D) Follow sample introduction,
purging, and desorption steps described
in the method.
(E) If less than five samples are used
for compositing, a proportionately
small syringe may be used.
(v) Compositing samples prior to GC/
MS analysis.
(A) Inject 5-ml or equal larger
amounts of each aqueous sample (up to
5 samples are allowed) into a 25-ml
377
-------
§141.24
40 CFR Ch. I (7-1-04 Edition)
purging device using the sample intro-
duction technique described in the
method.
(B) The total volume of the sample in
the purging device must he 25 ml.
(C) Purge and desorb as described in
the method.
(15) Compliance with §141.61(a) (1)
through (21) shall be determined based
on the analytical results obtained at
each sampling point. If one sampling
point is in violation of an MCL, the
system is in violation of the MCL.
(i) For systems monitoring more
than once per year, compliance with
the MOL is determined by a running
annual average at each sampling point.
(ii) Systems monitoring annually or
less frequently whose sample result ex-
ceeds the MCL must begin quarterly
sampling. The system will not be con-
sidered in violation of the MCL until it
has completed one year of quarterly
sampling.
(iii) If any sample result will cause
the running annual average to exceed
the MCL at any sampling point, the
system is out of compliance with the
MCL immediately.
(iv) If a system fails to collect the re-
quired number of samples, compliance
will be based on the total number of
samples collected.
(v) If a sample result is less than the
detection limit, aero will be used to
calculate the annual average.
(16) [Reserved]
(17) Analysis under this section shall
only be conducted by laboratories that
are certified by EPA or the State ac-
cording to the following conditions
(laboratories may conduct sample
analysis under provisional certification
until January 1, 1996):
(i) To receive certification to conduct
analyses for the contaminants in
§141.61(a) (2) through (21) the labora-
tory must:
(A) Analyze Performance Evaluation
(PE) samples provided by EPA, the
State, or by a third party (with the ap-
proval of the State or EPA) at least
once a year by each method for which
the laboratory desires certification.
(B) Achieve the quantitative accept-
ance limits under paragraphs
(f)(17)(i)(0) and (D) of this section for
at least 80 percent of the regulated or-
ganic contaminants included in the PE
sample.
(C) Achieve quantitative results on
the analyses performed under para-
graph (f)(17)(i)(A) of this section that
are within ±20% of the actual amount
of the substances in the Performance
Evaluation sample when the actual
amount is greater than or equal to 0.010
nag/1.
(D) Achieve quantitative results on
the analyses performed under para-
graph (f)(17)(l)(A) of this section that
are within ±40 percent of the actual
amount of the substances in the Per-
formance Evaluation sample when the
actual amount is less than 0.010 mg/'l.
(E) Achieve a method detection limit
of 0.0005 mg/1, according to the proce-
dures in appendix B of part 136.
(ii) To receive certification to con-
duct analyses for vinyl chloride, the
laboratory must:
(A) Analyze Performance Evaluation
(PE) samples provided by EPA, the
State, or by a third party (with the ap-
proval of the State or EPA) at least
once a year by each method for which
the laboratory desires certification.
(B) Achieve quantitative results on
the analyses performed under para-
graph (f)(17)(ii)(A) of this section that
are within ±40 percent of the actual
amount of vinyl chloride in the Per-
formance Evaluation sample.
(C) Achieve a method detection limit
of 0.0005 mg/1, according to the proce-
dures in appendix B of part 136.
(D) Obtain certification for the con-
taminants listed in §141.61(a)(2)
through (21).
(18) States may allow the use of mon-
itoring data collected after January 1,
1988, required under section 1445 of the
Act for purposes of initial monitoring
compliance. If the data are generally
consistent with the other requirements
of this section, the State may use these
data (i.e., a single sample rather than
four quarterly samples) to satisfy the
initial monitoring requirement of para-
graph (f)(4) of this section. Systems
which use grandfathered samples and
did not detect any contaminant listed
§141.61(a)(2) through (21) shall begin
monitoring annually in accordance
with paragraph (f)(5) of this section be-
ginning with the initial compliance pe-
riod.
378
-------
Environmental Protection Agency
§141.24
(19) States may increase required
monitoring where necessary to detect
variations within the system.
(20) Each certified laboratory must
determine the method detection limit
(MDL), as defined in appendix B to part
136, at which it is capable of detecting
VOOs. The acceptable MDL is 0.0005
mg/1. This concentration is the detec-
tion concentration for purposes of this
section.
(21) Each public water system shall
monitor at the time designated by the
State within each compliance period,
(22) All new systems or systems that
use a new source of water that begin
operation after January 22, 2004 must
demonstrate compliance with the MOL
within a period of time specified by the
State. The system must also comply
with the initial sampling frequencies
specified by the State to ensure a sys-
tem can demonstrate compliance with
the MCL. Routine and increased moni-
toring frequencies shall be conducted
in accordance with the requirements in
this section.
(g) [Reserved]
(h) Analysis of the contaminants list-
ed in §141.61(c) for the purposes of de-
termining compliance with the max-
imum contaminant level shall be con-
ducted as follows:7
(1) Groundwater systems shall take a
minimum of one sample at every entry
point to the distribution system which
is representative of each well after
treatment (hereafter called a sampling'
point). Each sample must be taken at
the same sampling point unless condi-
tions make another sampling point
more representative of each source or
treatment plant.
(2) Surface water systems shall take
a minimum of one sample at points in
the distribution system that are rep-
resentative of each source or at each
entry point to the distribution system
after treatment (hereafter called a
sampling point). Each sample must be
taken at the same sampling point un-
less conditions make another sampling
point more representative of each
source or treatment plant.
'Monitoring for the contaminants
aldicarb, aldicarb sulfoxide, and aldicarb
sulfone shall be conducted in accordance
with §141,40.
NOTE: For purposes of this paragraph, sur-
face water systems include systems with a
combination of surface and ground sources.
(3) If the system draws water from
more than one source and the sources
are combined before distribution, the
system must sample at an entry point
to the distribution system during peri-
ods of normal operating conditions
(i.e., when water representative of all
sources is being used).
(4) Monitoring frequency:
(i) Each community and non-tran-
sient non-community water system
shall take four consecutive quarterly
samples for each contaminant listed in
§141.61{c) during each compliance pe-
riod beginning with the initial compli-
ance period.
(ii) Systems serving more than 3,300
persons which do not detect a contami-
nant in the initial compliance period
may reduce the sampling frequency to
a minimum of two quarterly samples in
one year during each repeat compli-
ance period.
(iii) Systems serving less than or
equal to 3,300 persons which do not de-
tect a contaminant in the initial com-
pliance period may reduce the sam-
pling frequency to a minimum of one
sample during each repeat compliance
period.
(5) Each community and non-tran-
sient water system may apply to the
State for a waiver from the require-
ment of paragraph (h)(4) of this sec-
tion. A system must reapply for a
waiver for each compliance period.
(6) A State may grant a waiver after
evaluating the following factor(s):
Knowledge of previous use (including
transport, storage, or disposal) of the
contaminant within the watershed or
zone of influence of the system. If a de-
termination by the State reveals no
previous use of the contaminant within
the watershed or zone of influence, a
waiver may be granted. If previous use
of the contaminant is unknown or it
has been used previously, then the fol-
lowing factors shall be used to deter-
mine whether a waiver is granted.
(i) Previous analytical results.
(ii) The proximity of the system to a
potential point or non-point source of
contamination. Point sources include
spills and leaks of chemicals at or near
379
-------
§141.24
40 CFR Ch. i (7-1-04 Edition)
a water treatment facility or at manu-
facturing, distribution, or storage fa-
cilities, or from hazardous and munic-
ipal waste landfills and other waste
handling or treatment facilities. Non-
point sources include the use of pes-
ticides to control insect and weed pests
on agricultural areas, forest lands,
home and gardens, and other land ap-
plication uses.
(iii) The environmental persistence
and transport of the pesticide or PCBs.
(iv) How well the water source is pro-
tected against contamination due to
such factors as depth of the well and
the type of soil and the integrity of the
well casing.
(v) Elevated nitrate levels at the
water supply source.
(vi) Use of PCBs in equipment used in
the production, storage, or distribution
of water (i.e., PCBs used in pumps,
transformers, etc.).
(7) If an organic contaminant listed
in §141.61(c) is detected (as defined by
paragraph (h)(18) of this section) in any
sample, then:
(i) Each system must monitor quar-
terly at each sampling point which re-
sulted in a detection.
(ii) The State may decrease the quar-
terly monitoring requirement specified
in paragraph (h)(7)(i) of this section
provided it has determined that the
system is reliably and consistently
below the maximum contaminant
level. In no case shall the State make
this determination unless a ground-
water system takes a minimum of two
quarterly samples and a surface water
system takes a minimum of four quar-
terly samples.
(iii) After the State determines the
system is reliably and consistently
below the maximum contaminant level
the State may allow the system to
monitor annually. Systems which mon-
itor annually must monitor during the
quarter that previously yielded the
highest analytical result.
(iv) Systems which have 3 consecu-
tive annual samples with no detection
of a contaminant may apply to the
State for a waiver as specified in para-
graph (h)(6) of this section.
(v) If monitoring results in detection
of one or more of certain related con-
taminants (aldicarb, aldicarb sulfone,
aldicarb sulfoxide and heptachlor, hep-
tachlor epoxide), then subsequent mon-
itoring shall analyze for all related
contaminants.
(8) Systems which violate the re-
quirements of §141.61(c) as determined
by paragraph (h)(ll) of this section
must monitor quarterly. After a min-
imum of four quarterly samples show
the system is in compliance and the
State determines the system is reliably
and consistently below the MCL, as
specified in paragraph (h)(ll) of this
section, the system shall monitor at
the frequency specified in paragraph
(h)(7)(iii) of this section.
(9) The State may require a con-
firmation sample for positive or nega-
tive results. If a confirmation sample Is
required by the State, the result must
be averaged with the first sampling re-
sult and the average used for the com-
pliance determination as specified by
paragraph (h)(ll) of this section. States
have discretion to delete results of ob-
vious sampling errors from this cal-
culation.
(10) The State may reduce the total
number of samples a system must ana-
lyze by allowing the use of
compositing. Composite samples from
a maximum of five sampling points are
allowed, provided that the detection
limit of the method used for analysis is
less than one-fifth of the MCL.
Compositing of samples must be done
in the laboratory and analyzed within
14 days of sample collection.
(i) If the concentration in the com-
posite sample detects one or more con-
taminants listed in §141.61(c), then a
follow-up sample must be taken within
14 days at each sampling point included
in the composite, and be analyzed for
that contaminant.
(ii) If duplicates of the original sam-
ple taken from each sampling point
used in the composite sample are avail-
able, the system may use these instead
of resampling. The duplicates must be
analyzed and the results reported to
the State within 14 days after comple-
tion of the composite analysis or before
the holding time for the initial sample
is exceeded whichever is sooner.
(iii) If the population served by the
system is >3,300 persons, then
compositing may only be permitted by
the State at sampling points within a
single system. In systems serving <
380
-------
Environmental Protection Agency
§141.24
3,300 persons, the State may permit
compositing among different systems
provided the 5-sample limit is main-
tained,
(11) Compliance with §14L61(c) shall
be determined based on the analytical
results obtained at each sampling
point. If one sampling point is in viola-
tion of an MOL, the system is in viola-
tion of the MCL.
(i) For systems monitoring more
than once per year, compliance with
the MCL is determined by a running
annual average at each sampling point,
(ii) Systems monitoring' annually or
less frequently whose sample result ex-
ceeds the regulatory detection level as
defined by paragraph (h)(18) of this sec-
tion must begin quarterly sampling.
The system will not be considered in
violation of the MCL until it has com-
pleted one year of quarterly sampling.
(iii) If any sample result will cause
the running annual average to exceed
the MCL at any sampling point, the
system Is out of compliance with the
MCL immediately,
(iv) If a system fails to collect the re-
quired number of samples, compliance
will be based on the total number of
samples collected.
(v) If a sample result is less than the
detection limit, zero will be used to
calculate the annual average.
(12) [Reserved]
(13) Analysis for PCBs shall be con-
ducted as follows using the methods in
paragraph (e) of this section:
(i) Each system which monitors for
PCBs shall analyze each sample using
either Method 508.1, 525.2, 508 or 505.
Users of Method 505 may have more dif-
ficulty in achieving the required
Aroclor detection limits than users of
Methods 508.1, 525.2 or 508.
(ii) If PCBs (as one of seven Aroclors)
are detected (as designated in this
paragraph) in any sample analyzed
using Method 505 or 508, the system
shall reanalyze the sample using Meth-
od 508A to quantitate PCBs (as
decachlorobiphenyl).
Aroclor
: Detection limit {mg/
i I)
1260
0.0002
Aroclor
1016
1221
1232 . .
1242
12S4
Detection limit (mg/
I)
0.00008
002
00005
0.0003
0.0001
0.000 1
(iii) Compliance with the PCB MCL
shall be determined based upon the
quantitative results of analyses using
Method 508A.
(14) If monitoring data collected after
January 1, 19§0, are generally con-
sistent with the requirements of
§141.24(h), then the State may allow
systems to use that data to satisfy the
monitoring: requirement for the initial
compliance period beginning January
1,1993.
(15) The State may increase the re-
quired monitoring frequency, where
necessary, to detect variations within
the system (e.g., fluctuations in con-
centration due to seasonal use, changes
in water source).
(18) The State has the authority to
determine compliance or initiate en-
forcement action based upon analytical
results and other information compiled
by their sanctioned representatives and
agencies.
(17) Each public water system shall
monitor at the time designated by the
State within each compliance period.
(18) Detection as used in this para-
graph shall be defined as greater than
or equal to the following concentra-
tions for each contaminant.
Contaminant
Alachlor
Aldiearb
Aldicarb suitoxide
Aldicarb sultone
Atrazine ....
Benzo[a]pyrene ,
Carbofuran , .
Chlordane
Daiapon
1 ,2-Dibromo-3-ebl0ropropane (DBCP)
Di |2-ethylhexyl) adipate
Di (2-ethylhexyl) phthaiate
Dinoseb
Diqual
2,4-D
Endothall -
Endrin
Ethylene dibromide (EDS)
Glyphosate
Heptachlor
Heplaehlor epoxide
Hexachiorobenzene
Hexachiorocyclopentadiene
Undane
Methoxychlor
Oxamyl
Picioram
Detection
limit {mg/l}
.0002
0005
.0005
.0008
,0001
.00002
.0009
.0002
.001
.00002
.0006
.0006
.0002
,0004
.0001
009
00001
.00001
.006
.00004
.00002
.0001
.0001
.00002
0001
,002
.0001
381
-------
§141.25
40 CFR Ch. I (7-1-04 Edition)
Contaminant |M$$0
Polychiorinated biphenyls (PCBs) (as '•
decachlorabiphenyl) >.,......, ..,,,.,......,.... j .0001
Pentachlorophenol ......,.,.,,„,.„ ,,..,.„,,„..,.„ .00004
Simazine „,....,,........,,,,,,,.,,,...... .0000?
237 8-TCDD {Dioxin) . , 000000005
(19) Anaylsia under this section shall
Contaminant
Simazine ,.....>,,....,.,.,,,,,
Toxaphene ,.....,.,.,.,.„...
Aldicarb ,,,,,,, ,,
Aldicarb sulfoxide ..................
2.3,7,8-TCDD (Dioxin) ,„.„.....
2,4-D ..................................
2,4,5-TP (Siivex) .........
Acceptance limits (percent)
2 standard deviations.
±45.
2 standard deviations.
2 standard deviations
2 standard deviations.
±50.
±50.
only be conducted by laboratories that
have received certification by EPA or
the State and have met the following
conditions:
(i) To receive certification to conduct
analyses for the contaminants in
§141.61(c) the laboratory must:
(A) Analyze Performance Evaluation
(PE) samples provided by EPA, the
State, or by a third party (with the ap-
proval of the State or EPA) at least
once a year by each method for which
the laboratory desires certification.
(B) For each contaminant that has
been included in the PE sample achieve
quantitative results on the analyses
that are within the following accept-
ance limits:
Contaminant
DBCP ..,...,.,...,...,...,...,.....,.,.„.
EDB .............
Benzo[a]pyrene
Df(2-ethy!hexyl)adipate ...„..„.
Di(2-ethylhexyi)phihalate .......
Dinoseb
Endofhall ., „.,.
Endrin ,.„,«...,..„, ,,,.„,.,.,
Gtyphosate ,,.,,.,,, ,,...,.,,.„,..
Heptachlor ,,..,,,...,....,...
Heptachlor epoxide
Hexachiorobenzene ...............
Hexachioro- cyciopenladiene
Lindane „,....,..,..,.,.......,.,.,.„...
Methoxychfor .,..,,..,,
PCBs (as
Decachlorobipheny!)
Acceptance limits (percent)
±40
±40.
+45
+45,
2 standard deviations,
+45
+45
2 standard deviations.
2 standard deviations,
2 standard deviations.
2 standard deviations.
2 standard deviations.
+30.
2 standard deviations,
±45,
±45.
2 standard deviations,
2 standard deviations.
+45.
±45-
0-200,
(ii) [Reserved]
(20) All new systems or systems that
use a new source of water that begin
operation after January 22, 2004 must
demonstrate compliance with the MCL
within a period of time specified by the
State. The system must also comply
with the initial sampling frequencies
specified by the State to ensure a sys-
tem can demonstrate compliance with
the MCL. Routine and increased moni-
toring frequencies shall be conducted
in accordance with the requirements in
this section.
(Approved by the Office of Management and
Budget under control number 2040-0090)
[40 PR 59570, Dec. 24, 1975, as amended at 44
FR 68641, Nov. 29, 1979; 45 PR 57345, Aug. 27,
1980: 47 FR 10998, Mar. 12, 1982: 52 FR 25712,
July 8, 1987: 53 FR 5147, Peb. 19, 1988; 53 FR
25110, July 1, 1988; 56 FR 3583, Jan. 30, 1991; 56
FR 30277, July 1, 1991; 57 FR 22178, May 27,
1992; 57 FR 31841, July 17. 1992; 59 FR 34323,
July 1, 1994; 59 FR 62468. Deo. 5. 1994; 60 FR
34085, June 29, 1995: 64 FR 67464, Deo, 1, 1999;
6S FR 26022, May 4, 2000; 66 FR 7063, Jan. 22,
2001; 67 FR 65250, Oct. 23, 2002; 67 FR 65898,
Oct. 29, 2002]
§ 141.25 Analytical methods for radio-
activity.
(a) Analysis for the following con-
taminants shall be conducted to deter-
mine compliance with §141.66 (radioac-
tivity) in accordance with the methods
in the following table, or their equiva-
lent determined by EPA in accordance
with §141.27.
382
-------
Naturally occurring
Gross alpha' '
and beta.
Gross alpha1 1 .,
Radium 226 .....
Methodology
Evaporation
Co-precipitation
Radon emanation ...
Radiocherru- cai
Radium 228 ,.,, Radiocherni- cal .. ..
Uranium12 ,..., ,. Radiochemi- cal ,... .
I Fluorometnc ... . ....
Alpha spectrometry
! Laser
Phosphorinnetry.
Man-made:
Radioact-
Radiochemi"
ive cesium ........ 1 cat ..............
: Gamma ray spec-
trometry.
OO Radioact- ....
Radioaot- ....„..,.
ive Strontium
Radiochemi-
cal
Gamma ray spec-
trometry.
Radiochemi-
cai
89. 90.
Tnlium | Liquid scintillation ...
Gamma emitters
Gamma ray
Spectrometry
Reference (method or page number)
EPA' i EPA2 j EPA3 | EPA" SM =
r |~~ T
900.0 ,p1 - 00-01 p1 ' 302, 7110 B
903.1
903-0
904.0
00-02
p 16 Ra-04
7110 C
p 19 305,7500-HaC
p 13 Ra-03 304,7500-Ra B
p24 Ra-05
p 19 7500-Ra D
908.0 I 7500-U B
908.1 | I 7500-U C (17th Ed.)
I
00-07 |p 33 7500-U C (18th, 19th or
i
I 20th Ed.).
901.0 j p4 j
| 7500-CsB
! I
901.1 ; : p B2 ! 7120
902.0 p6, p 9
901.1
905.0
906.0
901,1
902.0,
901.0.
p29 Sr-04
7500-I B, 7500-i C,
7500-I D.
p92 7120
p 65 303. 7500-Sf B
p 34 H-02 ! P 87 i 306, 7500-3H B
p92 7120
7500-Cs B, 7500-I B
I
ASTM6
D 3454-97
D 2460-97
D2907-97
D 3972-97
D 5174-97
D 2459-72
D 3649-91 ...
D 3649-91 .. .
D 4785-93
D 4107-91
D 3649-91
D 4785-93
uses 7
R-1120-76 ....
R-1141-76 ....
R 1140-76 ....
R 1142-76 ....
R-11 80-76.
R-11 81 -76.
R-11 82-76 ...
R-11 11-76 ...
R- 1110-76 ...
R-1 180-76 .. .
R-11 71-76 ....
R-11 10-76 ....
DOE' F Other
':
Ra-04
N.Y.9
N.Y.9,
N.J,10
U-34
U-Q2
4,5.2.3
4.5.2.3
Sr-01. Sr-
02 j
Ga-01-R
The procedures snail be done in accordance with the documents listed beiow. The incorporation by reference of documents 1 through 10 was approved by Ihe Director of the Federal
Register in accordance with 5 U.S.C. 552{a) and 1 CFR pari 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these documents
can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket EPA West, 1301 Constitution Avenue, NW., Room
B135S Washington, DC (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www,archives.gov/fe0eral register/co&e of federal regulations/ibr locations html.
1''Prescribed Procedures for the Measurement of Radioactivity in Drinking Water , EPA 600/4-80-032. August 1980, Available at the U.S. Department of Commerce, National Technical
Information Service (NTIS), 5285 Port Royal Road, Springfield. VA 22161 (Telephone 800-553-6847), PB 80-224744.
2"lnterim Radiochemical Methodology for Drinking Water", EPA 600/4-75-008(revised), March 1976. Available NTIS. ibid. PB 253258.
3-Radiochemistry Procedures Manual", EPA 520/5-84-006, December, 1987. Available NTIS, ibid. PB 84-215581.
4 "RadiochemicaS Analytical Procedures for Analysis of Environmental Samples", March 1979. Available at NTIS, ibid. EMSL LV 053917
5"Star>dard Methods for the Examination of Water and Wastewater". 13th, 17th, 18th. 19th Editions, or 20th edition, 1971. 1989, 1992. 1995, 1998. Available at American Public Health
Association, 1015 Fifteenth Street NW,, Washington. DC 20005 . Methods 302, 303. 304. 305 and 306 are only in the 13lh edition. Methods 711 OB, 7500-Ra B, 7500-Ra C. 7500-Ra D,
7SOO-U B, 7500-Cs B, 7500-I B, 7500-I C, 7500-I D, 7500-Sr B, 7SOO-3H B are in the 17th, 18th, 19th and 20th editions. Method 7110 C is in the 18th. 19th and 20th editions. Method
7500-U C Fluorometric Uranium is only in the 17th Edition, and 7500-U C Alpha spectrometry is only in the 18th, 19th and 20th edition:. Method 7120 is only in the 19th and 20th editions.
Methods 302, 303, 304, 305 and 306 are only in the I3ih edition.
6 Annual Book of ASTM Standards, Vol. 11.01 and 11.02. 1999; ASTM International any year containing the cited version oi the method may be used. Copies may be obtained from
ASTM International 100 Barr Harbor Drive, West Conshohocken PA 19428,
K)
-------
CO
OS
7"Methods for Determination of Radioactive Substances in Water and Fluvial Sediments", Chapter AS in Book 5 of Techniques of Water-Resources Investigations of the United States Ge- *&*
ological Survey, 1977- Available at U.S. Geological Survey (USQS) Information Services, Box 25286, Federal Center, Denver, CO 80225-0425. —•
8"EML Procedures Manual", 28th (1997) or 27th (1990) Editions, Volumes 1 and 2; either edition may be used, in the 27th Edition Method Ra-04 is listed as Ra-05 and Method Ga-01- *5
R is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S. Department of Energy (DOE), 376 Hudson Street, New York, NY 10014-3621, •
'"Determination of Ra-226 and Ra-228 (Ra-02)", January 1980, Revised June 1982. Available at Radiological Sciences Institute for Laboratories and Research, New York State Depart- K
ment of Health, Empire State Plaza, Albany, NY 12201.
^"Determination of Radium 228 in Drinking Water", August 1980. Available at State of New Jersey, Department of Environmental Protection, Division of Environmental Quality, Bureau of
Radiation and Inorganic Analytical Services, 9 Ewing Street, Trenton, NJ 08625.
11 Natural uranium and thoriurn-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods; americiurn-241 is approved with co-
precipitation methods,
12ln uranium (U) is determined by mass, a 0.67 pCi/iig of uranium conversion factor must be used. This conversion factor is based on the 1:1 activity ration of U-234 and U-238 that is
characteristic of naturally occurring uranium.
TO
o
o
-------
Environmental Protection Agency
§141.25
(b) When the identification and meas-
urement of radionuclides other than
those listed in paragraph (a) of this
section is required, the following ref-
erences are to be used, except in cases
where alternative methods have been
approved in accordance with §141.27.
(1) Procedures for Radiochemical Anal-
ysis of Nuclear Reactor Aqueous Solu-
tions, H. L. Krieger and S. Gold, EPA-
R4-73--014. USEPA. Cincinnati. Ohio,
May 1973.
(2) HASL Procedure Manual, Edited by
John H. Harley. HASL 300, ERDA
Health and Safety Laboratory. New
York, NY., 1973.
(c) For the purpose of monitoring ra-
dioactivity concentrations in drinking
water, the required sensitivity of the
radioanalysis is defined in terms of a
detection limit. The detection limit
shall be that concentration which can
be counted with a precision of plus or
minus 100 percent at the 95 percent
confidence level (1,960 where o is the
standard deviation of the net counting
rate of the sample).
(1) To determine compliance with
§141,66(b), (c), and (e) the detection
limit shall not exceed the concentra-
tions in Table B to this paragraph.
TABLE B.—DETECTION LIMITS FOR GROSS
ALPHA PARTICLE ACTIVITY, RADIUM 226, RA-
DIUM 228, AND URANIUM
Contaminant
Gross alpha particle activity
Radium 226
Radium 228
Uranium
3 pCi/L
i 1 pCi/L.
1 pCi/L,
Reserve
(2) To determine compliance with
§141.66(d) the detection limits shall not
exceed the concentrations listed in
Table C to this paragraph.
TABLE C—DETECTION LIMITS FOR MAN-MADE
BETA PARTICLE AND PHOTON EMITTERS
Radionuclide
Detection limit
Tritium
Sirontium-89
Strontium-90
lodine-131
Cesrum-134
Gross beta
Other radionuclides
1,OOOpCi/1.
10pCi/1.
2pCi/1.
. 1 pCi/1.
; 10 pCi/1.
i 4pCi/1.
: I/TO of the applicable limit.
(d) To judge compliance with the
maximum contaminant levels listed in
§141.66, averages of data shall be used
and shall be rounded to the same num-
ber of significant figures as the max-
imum contaminant level for the sub-
stance in question.
(e) The State has the authority to de-
termine compliance or initiate enforce-
ment action "based upon analytical re-
sults or other information compiled by
their sanctioned representatives and
agencies.
[41 FR 28404, July 9, 1976, as amended at 45
FB 57345, Aug. 27, 1980; 62 FR 10173, Mar. 5,
1997; 65 FR 76745, Dec. 7, 2000: 67 FR 65250,
Oct. 23, 2002]
EFFECTIVE DATE NOTE i: At 69 FR 31012,
June 2, 2004, §141.25 was amended in the table
in paragraph (a) by revising the entry for
uranium, revising" footnotes 1, 2, 3, 5, 6, 8, and
12, and adding footnote 13, effective Aug. 31,
2004. For the convenience of the user, the re-
vised and added text is set forth as follows:
385
-------
1141.25 Analytical methods for radioactivity,
Reference (method or page number)
Contaminant Methodology - ...................................... ---------- • - [[[
SM5 ASTM6 USGS7 DOE8
Uranium12 ................................ Radioehemical ......................... 908.0 .......................................... 7500-U B
Fiuorometric ............................. 908.1 ......................................... 7500-U C (17th Ed.) D 2907-97 R-1 1 80-76, R- U-04
1181-76
ICP-MS .................................. "200.8 ... ...................................... 3125 D5873-G3
Alpha spectrometry .............................................. 00-07 p-33 7500-U C (18th, 19th or 20th D3972-97 R-1182-76 U-02
Ed.)
Laser Phosphorimetry [[[ D5174-97
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 and 13 was approved by the Director of the Fed-
eral Register in accordance with 5 U.S.C. 552{a) and 1 CFR part 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these docu-
ments can be obtained from the Sale Drinking Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW,
Room B135, Washington. DC (Telephone: 202-566-2426): or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call
202-741-6030, or go to: http://www.arch:ves.gov/federal_ register/code of federat_regulations/ibr_ Socations.html.
1 "Prescribed Procedures for the Measurement of Radioactivity in Drinking Water", EPA 600/4-80-032, August 1980. Available at the U.S. Department of Commerce, National Technical
Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800-553-6847), PB 80-224744, except Method 200.8, "Determination of Trace Elements in Waters
and Wastes by Inductively Coupled Plasma-Mass Spectrometry," Revision 5.4, which is published in "Methods for the Determination of Metals in Environmental Samples—Supplement I."
EPA 600-H-94-111. May 1994. Available at NTIS, PB9S-125472.
2 "Interim Radiochemical Methodology for Drinking Water", EPA 600/4-75-008(revised), March 1976. Available at NTIS. ibid. PB 253258.
3"Radiochemistry Procedures Manual", EPA 520/5-84-006, December, 1987. Available at NTIS, ibid. PB 84-215581.
A "Radiochemical Analytical Procedures for Analysis of Environmental Samples", March 1979. Available at NTIS, ibid. EMSL LV 053917.
5"Standard Methods for the Examination of Water and Wastewater", 13th, 17th, 18th, 19th Editions, or 20th edition, 1971, 1989, 1992, 1995. 1998. Available at American Public Health
Association. 1015 Fifteenth Street NW,, Washington, DC 20005. Methods 302, 303, 304. 305 and 306 are only in the 13th edition. Methods 7110B, 7500-Ra B, 7500-Ra C, 7500-Ra D,
7500-U B, 7500-Cs B, 7500-I B, 7500-I C, 7500-I D, 7500-Sr B, 7500-3H B are in the 17th, 18th, 19th and 20th editions. Method 7110 C is in the 18th, 19th and 20th editions. Method ^
7500-U C Fiuorometric Uranium is only in the 17th Edition, and 7500-U C Alpha spectrometry is only in the 18th, 19th and 20th editions. Method 7120 is only in the 19th and 20th editions. §
Methods 302, 303, 304, 305 and 306 are only in the 13th edition. Method 3125 is only in the 20th edition.
"Annual Book of ASTM Standards, Vol. 11.01 and 11.02. 1999; ASTM International any year containing (he-cited version of the method may be used. Copies of these two volumes and O
the 2003 version of D 5673-03 may be obtained from ASTM International. 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA, 19428-2959. yg
'"Methods tor Determination of Radioactive Substances in Water and Fluvial Sediments", Chapter AS in Book 5 of Techniques of Water-Resources Investigations of the United States Ge-
ological Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal Center, Denver, CO 80225-0425. O
«"EML Procedures Manual", 28th (1997) or 27th (1990) Editions, Volumes 1 and 2; either edition may be used. In the 27ih Edition Method Ra-04 is listed as Ra-05 and Method Ga-01- ?"
R is listed as Sect. 4.5.2,3. Available at the Environmental Measurements Laboratory, U.S. Department of Energy (DOE), 376 Hudson Street, New York, NY 10014-3621, _
12lf uranium (U) is determined by mass, a 0.67 pCi/^g of uranium conversion factor must be used. This conversion factor is based on the 1:1 activity ratio of U-234 and U-238 that is *H
characteristic of naturally occurring uranium. _*
""Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry," Revision 5.4, which is published in "Methods for the Determination of I
-------
Environmental Protection Agency
§141.26
EFFECTIVE DATE NOTE 2; At 69 PR 38855,
Jane 29, 2004, §141,25 was amended in para-
graph (c){l) in the entry for cranium in the
second column of Table B by removing the
word "reserve" and adding in its place "1 pg/
V, effective July 29, 2004.
§141.26 Monitoring frequency and
compliance requirements for radio-
nuclides in community water sys-
tems.
(a) Monitoring and compliance require-
ments for gross alpha particle activity, ra-
dium-226, radium-228, and uranium. (1)
Community water systems (CWSs)
must conduct initial monitoring to de-
termine compliance with §141.66(b), (c),
and (e) by December 31, 2007. For the
purposes of monitoring for gross alpha
particle activity, radium-226, radium-
228, uranium, and beta particle and
photon radioactivity in drinking water,
"detection limit" is defined as in
§ 141.25(c).
(i) Applicability and sampling location
for existing community water systems or
sources. All existing CWSs using ground
water, surface water or systems using
both ground and surface water (for the
purpose of this section hereafter re-
ferred to as systems) must sample at
every entry point to the distribution
system that is representative of all
sources being used (hereafter called a
sampling point) under normal oper-
ating conditions. The system must
take each sample at the same sampling
point unless conditions make another
sampling point more representative of
each source or the State has designated
a distribution system location, in ac-
cordance with paragraph (a)(2)(ii)(C) of
this section.
(ii) Applicability and sampling location
for new community water systems or
sources. All new CWSs or CWSs that use
a new source of water must begin to
conduct initial monitoring for the new
source within the first quarter after
initiating use of the source. CWSs must
conduct more frequent monitoring
when ordered by the State in the event
of possible contamination or when
changes in the distribution system or
treatment processes occur which may
increase the concentration of radioac-
tivity in finished water,
(2) Initial monitoring: Systems must
conduct initial monitoring for gross
alpha particle activity, radium-226, ra-
dium-228, and uranium as follows:
(i) Systems without acceptable his-
torical data, as defined below, must
collect four consecutive quarterly sam-
ples at all sampling points before De-
cember 31, 2007.
(ii) Grandfathering of data: States
may allow historical monitoring data
collected at a sampling point to satisfy
the initial monitoring requirements for
that sampling point, for the following
situations.
(A) To satisfy initial monitoring re-
quirements, a community water sys-
tem having only one entry point to the
distribution system may use the moni-
toring data from the last compliance
monitoring period that began between
June 2000 and December 8, 2003.
(B) To satisfy initial monitoring re-
quirements, a community water sys-
tem with multiple entry points and
having appropriate historical moni-
toring data for each entry point to the
distribution system may use the moni-
toring data from the last compliance
monitoring period that began between
June 2000 and December 8, 2003.
(C) To satisfy initial monitoring re-
quirements, a community water sys-
tem with appropriate historical data
for a representative point in the dis-
tribution system may use the moni-
toring- data from the last compliance
monitoring period that began between
June 2000 and December 8, 2003, pro-
vided that the State finds that the his-
torical data satisfactorily demonstrate
that each entry point to the distribu-
tion system is expected to be in com-
pliance based upon the historical data
and reasonable assumptions about the
variability of contaminant levels be-
tween entry points. The State must
make a written finding indicating how
the data conforms to the these require-
ments.
(iii) For gross alpha particle activity,
uranium, radium-226, and radium-228
monitoring, the State may waive the
final two quarters of initial monitoring
for a sampling point if the results of
the samples from the previous two
quarters are below the detection limit.
(iv) If the average of the initial moni-
toring- results for a sampling point is
above the MCL, the system must col-
lect and analyze quarterly samples at
387
-------
§141.26
40 CFR Ch, I (7-1-04 Edition)
that sampling point until the system
lias results from four consecutive quar-
ters that are at or below the MCL, un-
less the system enters Into another
schedule as part of a formal compli-
ance agreement with the State.
(3) Reduced monitoring: States may
allow community water systems to re-
duce the future frequency of moni-
toring from once every three years to
once every six or nine years at each
sampling point, based on the following-
criteria.
(i) If the average of the initial moni-
toring results for each contaminant
(i.e., gross alpha particle activity, ura-
nium, radium-226, or radium-228) is
below the detection limit specified in
Table B, in §141.25(c)(l), the system
must collect and analyze for that con-
taminant using at least one sample at
that sampling point every nine years.
(ii) For gross alpha particle activity
and uranium, if the average of the ini-
tial monitoring results for each con-
taminant is at or above the detection
limit but at or below l/i the MCL, the
system must collect and analyze for
that contaminant using1 at least one
sample at that sampling point every
six years. For combined radium-226 and
radium-228, the analytical results must
be combined. If the average of the com-
bined initial monitoring results for ra-
dium-226 and radium-228 is at or above
the detection limit but at or below 1A
the MCL, the system must collect and
analyze for that contaminant using- at
least one sample at that sampling-
point every six years.
(iii) For gross alpha particle activity
and uranium, if the average of the ini-
tial monitoring results for each con-
taminant is above Va the MCL but at or
below the MCL, the system must col-
lect and analyze at least one sample at
that sampling point every three 5rears,
For combined radium-226 and radium-
228, the analytical results must be
combined. If the average of the com-
bined initial monitoring results for ra-
dium-226 and radium-228 is above Vi the
MCL but at or below the MCL, the sys-
tem must collect and analyze at least
one sample at that sampling point
every three years.
(iv) Systems must use the samples
collected during the reduced moni-
toring period to determine the moni-
toring frequency for subsequent moni-
toring periods (e.g., if a system's sam-
pling point is on a nine year moni-
toring period, and the sample result is
above Vz MCL, then the next moni-
toring period for that sampling point is
three years).
(v) If a system has a monitoring re-
sult that exceeds the MCL while on re-
duced monitoring, the system must
collect and analyze quarterly samples
at that sampling point until the sys-
tem has results from four consecutive
quarters that are below the MCL, un-
less the system enters into another
schedule as part of a formal compli-
ance agreement with the State.
(4) Compositing: To fulfill quarterly
monitoring requirements for gross
alpha particle activity, radium-226. ra-
dium-228, or uranium, a system may
composite up to four consecutive quar-
terly samples from a single entry point
if analysis is done within a year of the
first sample. States will treat analyt-
ical results from the composited as the
average analytical result to determine
compliance with the MCLs and the fu-
ture monitoring frequency. If the ana-
lytical result from the composited
sample is greater than % MCL, the
State may direct the system to take
additional quarterly samples before al-
lowing the system to sample under a
reduced monitoring schedule.
(5) A gross alpha particle activity
measurement may be substituted for
the required radium-226 measurement
provided that the measured gross alpha
particle activity does not exceed 5 pCi/
1. A gross alpha particle activity meas-
urement may be substituted for the re-
quired uranium measurement provided
that the measured gross alpha particle
activity does not exceed 15 pCi/1. The
gross alpha measurement shall have a
confidence interval of 95% (1.650, where
0 is the standard deviation of the net
counting rate of the sample) for ra-
dium-226 and uranium. When a system
uses a gross alpha particle activity
measurement in lieu of a radium-226
and/or uranium measurement, the
gross alpha particle activity analytical
result will be used to determine the fu-
ture monitoring frequency for radium-
226 and/or uranium. If the gross alpha
particle activity result is less than de-
tection, l/2 the detection limit will be
388
-------
Environmental Protection Agency
§141.26
used to determine compliance and the
future monitoring frequency.
(b) Monitoring and compliance require-
ments for beta particle and photon radio-
activity. To determine compliance with
the maximum contaminant levels in
§141.66(d) for beta particle and photon
radioactivity, a system must monitor
at a frequency as follows:
(1) Community water systems (both
surface and ground water) designated
by the State as vulnerable must sample
for beta particle and photon radioac-
tivity. Systems must collect quarterly
samples for beta emitters and annual
samples for tritium and strontium-90
at each entry point to the distribution
system (hereafter called a sampling
point), beginning within one quarter
after being notified by the State. Sys-
tems already designated by the State
must continue to sample until the
State reviews and either reaffirms or
removes the designation.
(i) If the gross beta particle activity
minus the naturally occurring potas-
sium-40 beta particle activity at a sam-
pling point has a running annual aver-
age (computed quarterly) less than or
equal to 50 pCi/L (screening level), the
State may reduce the frequency of
monitoring at that sampling point to
once every 3 years. Systems must col-
lect all samples required in paragraph
(b)(l) of this section during the reduced
monitoring period.
(li) For systems in the vicinity of a
nuclear facility, the State may allow
the CWS to utilize environmental sur-
veillance data collected by the nuclear
facility in lieu of monitoring at the
system's entry point(s), where the
State determines if such data is appli-
cable to a particular water system. In
the event that there is a release from a
nuclear facility, systems which are
using surveillance data must begin
monitoring at the community water
system's entry point(s) in accordance
with paragraph (b)(l) of this section.
(2) Community water systems (both
surface and ground water) designated
by the State as utilizing waters con-
taminated by effluents from nuclear fa-
cilities must sample for beta particle
and photon radioactivity. Systems
must collect quarterly samples for beta
emitters and iodine-131 and annual
samples for tritium and strontium-90
at each entry point to the distribution
system (hereafter called a sampling
point), beginning within one quarter
after being notified by the State. Sys-
tems already designated by the State
as systems using waters contaminated
by effluents from nuclear facilities
must continue to sample until the
State reviews and either reaffirms or
removes the designation.
(i) Quarterly monitoring for gross
beta particle activity shall be based on
the analysis of monthly samples or the
analysis of a composite of three month-
ly samples. The former is rec-
ommended.
(ii) For iodine-131, a composite of five
consecutive daily samples shall be ana-
lyzed once each quarter. As ordered by
the State, more frequent monitoring
shall be conducted when iodine-131 is
identified in the finished water.
(iii) Annual monitoring for stron-
tium-90 and tritium shall be conducted
by means of the analysis of a com-
posite of four consecutive quarterly
samples or analysis of four quarterly
samples. The latter procedure is rec-
ommended.
(iv) If the gross beta particle activity
beta minus the naturally occurring po-
tassium-40 beta particle activity at a
sampling point has a running annual
average (computed quarterly) less than
or equal to 15 pCi/L, the State may re-
duce the frequency of monitoring at
that sampling point to every 3 years.
Systems must collect all samples re-
quired in paragraph (b)(2) of this sec-
tion during the reduced monitoring pe-
riod.
(v) For systems in the vicinity of a
nuclear facility, the State may allow
the CWS to utilize environmental sur-
veillance data collected by the nuclear
facility in lieu of monitoring at the
system's entry point(s), where the
State determines if such data is appli-
cable to a particular water system. In
the event that there is a release from a
nuclear facility, systems which are
using surveillance data must begin
monitoring at the community water
system's entry point(s) in accordance
with paragraph (b){2) of this section.
(3) Community water systems des-
ignated by the State to monitor for
beta particle and photon radioactivity
can not apply to the State for a waiver
389
-------
§141.26
40 CFR Ch. I (7-1-04 Edition)
from the monitoring frequencies speci-
fied in paragraph (b)(l) or (b)(2) of this
section.
(4) Community water systems may
analyze for naturally occurring potas-
sium-40 beta particle activity from the
same or equivalent sample used for the
gross beta particle activity analysis.
Systems are allowed to subtract the
potassium-40 beta particle activity
value from the total gross beta particle
activity value to determine if the
screening level is exceeded. The potas-
sium-40 beta particle activity must be
calculated by multiplying elemental
potassium concentrations (in mg/L) by
a factor of 0.82.
(5) If the gross beta particle activity
minus the naturally occurring potas-
sium-40 beta particle activity exceeds
the screening level, an analysis of the
sample must be performed to identify
the major radioactive constituents
present in the sample and the appro-
priate doses must be calculated and
summed to determine compliance with
§141.66(d)(l), using the formula in
§141.66(d)(2). Doses must also be cal-
culated and combined for measured
levels of tritium and strontium to de-
termine compliance.
(6) Systems must monitor monthly
at the sampling polnt(s) which exceed
the maximum contaminant level in
§141.66(d) beginning the month after
the exceedance occurs. Systems must
continue monthly monitoring until the
system has established, by a rolling av-
erage of 3 monthly samples, that the
MCL is being met. Systems who estab-
lish that the MCL is being met must
return to quarterly monitoring until
they meet the requirements set forth
in paragraph (b)(l)(ii) or (b)(2)(i) of this
section.
(c) General monitoring and compliance
requirements for radionuclides. (1) The
State may require more frequent moni-
toring than specified in paragraphs (a)
and (b) of this section, or may require
confirmation samples at its discretion.
The results of the initial and confirma-
tion samples will be averaged for use in
compliance determinations.
(2) Bach public water systems shall
monitor at the time designated by the
State during each compliance period.
(3) Compliance: Compliance with
§141.66 (b) through (e) will be deter-
mined based on the analytical result(s)
obtained at each sampling point. If one
sampling point is in violation of an
MCL, the system is in violation of the
MCL.
(i) For systems monitoring more
than once per year, compliance with
the MCL is determined by a running
annual average at each sampling point.
If the average of any sampling point is
greater than the MCL, then the system
is out of compliance with the MCL.
(ii) For systems monitoring more
than once per year, if any sample re-
sult will cause the running average to
exceed the MCL at any sample point,
the system is out of compliance with
the MCL immediately.
(ill) Systems must include all sam-
ples taken and analyzed under the pro-
visions of this section in determining
compliance, even if that number is
greater than the minimum required.
(iv) If a system does not collect all
required samples when compliance is
based on a running annual average of
quarterly samples, compliance will be
based on the running average of the
samples collected.
(v) If a sample result is less than the
detection limit, zero will be used to
calculate the annual average, unless a
gross alpha particle activity is being
used In lieu of radium-226 and/or ura-
nium. If the gross alpha particle activ-
ity result is less than detection, Vz the
detection limit will be used to cal-
culate the annual average.
(4) States have the discretion to de-
lete results of obvious sampling or ana-
lytic errors.
(5) If the MCL for radioactivity set
forth in §141.66 (b) through (e) is ex-
ceeded, the operator of a community
water system must give notice to the
State pursuant to §141.31 and to the
public as required by subpart Q of this
part.
[65 PR 76V45, Dec. 7, 2000]
EFFECTIVE DATE NOTE: At 69 FR 38855, June
29, 2004, §141.26 was amended by revising
paragraphs (b)(2)£iv) and (b)(5) and in para-
graph (b){6) by removing the citation
"(b)(l)(il)" and adding In its place "(b)(l)(i)"
and by removing the citation "(b)(2)(i)" and
adding in its place "(b)(2)(iv)", effective July
29, 2004. For the convenience of the user, the
revised text is set forth as follows:
390
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Environmental Protection Agency
§141.30
$141.26 Monitoring frequency and compli-
ance requirements for radionuclides in
community water systems.
(b)* * *
(2)* * *
Civ) If the gross beta particle activity
minus the naturally occurring potassium-40
beta particle activity at a sampling point
has a running annual average (computed
quarterly) less than or equal to 15 pCi/L
(screening level), the State may reduce the
frequency of monitoring at that sampling
point to every 3 years. Systems must collect
the same type of samples required in para-
graph (b)(2) of this section during the re-
duced monitoring period.
(5) If the gross beta particle activity minus
the naturally occurring potassium-40 beta
particle activity exceeds the appropriate
screening level, an analysis of the sample
must be performed to identify the major ra-
dioactive constituents present in the sample
and the appropriate doses must be calculated
and summed to determine compliance with
§141.66(d)(l), using the formula in
§141.66(d)(2>. Doses must also be calculated
and combined for measured levels of tritium
and strontium to determine compliance.
§ 141.27 Alternate analytical tech-
niques.
(a) With the written permission of
the State, concurred in by the Admin-
istrator of the U.S. EPA, an alternate
analytical technique may be employed.
An alternate technique shall be accept-
ed only if it is substantially equivalent
to the prescribed test in both precision
and accuracy as it relates to the deter-
mination of compliance with any MCL.
The use of the alternate analytical
technique shall not decrease the fre-
quency of monitoring' required by this
part.
[45 FB 57345, Aug. 27, 1980]
§ 141.28 Certified laboratories.
(a) For the purpose of determining
compliance with §§141,21 through
141.27, 141.30, 141.40, 141.74 and 141.89,
samples may be considered only if they
have been analyzed by a laboratory
certified by the State except that
measurements for alkalinity, calcium,
conductivity, disinfectant residual,
orthophosphate, pH, silica, tempera-
ture and turbidity may be performed
by any person acceptable to the State.
(b) Nothing in this part shall be con-
strued to preclude the State or any
duly designated representative of the
State from taking samples or from
using the results from such samples to
determine compliance by a supplier of
water with the applicable requirements
of this part.
[45 PE 57345, Aug. 27, 1980; 47 FB 10999, Mar.
12, 1982, as amended at 59 FB 34323, July 1,
1994; 64 PR 67465, Dec. 1, 1999]
§ 141.29 Monitoring of consecutive
public water systems.
When a public water system supplies
water to one or more other public
water systems, the State may modify
the monitoring requirements Imposed
by this part to the extent that the
interconnection of the systems justi-
fies treating them as a single system
for monitoring purposes. Any modified
monitoring shall be conducted pursu-
ant to a schedule specified by the State
and concurred in by the Administrator
of the U.S. Environmental Protection
Agency.
§141.30 Total trihalomethanes sam-
pling, analytical and other require-
ments.
(a) Community water system which
serve a population of 10,000 or more in-
dividuals and which add a disinfectant
(oxidant) to the water in any part of
the drinking water treatment process
shall analyze for total trihalomethanes
in accordance with this section. For
systems serving 75,000 or more individ-
uals, sampling and analyses shall begin
not later than 1 year after the date of
promulgation of this regulation. For
systems serving 10,000 to 74.999 individ-
uals, sampling and analyses shall begin
not later than 3 years after the date of
promulgation of this regulation. For
the purpose of this section, the min-
imum number of samples required to be
taken by the system shall be based on
the number of treatment plants used
by the system, except that multiple
wells drawing raw water from a single
aquifer may, with the State approval.
be considered one treatment plant for
determining the minimum number of
391
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§141,30
40 CFR Ch, I (7-1-04 Edition)
samples. All samples taken within an
established frequency shall be collected
within a 24-hour period.
(b)(l) For all community water sys-
tems utilizing surface water sources in
whole or in part, and for all commu-
nity water systems utilizing only
ground water sources that have not
been determined by the State to qual-
ify for the monitoring requirements of
paragraph (c) of this section, analyses.
for total trihalomethanes shall be per-
formed at quarterly intervals on at
least four water samples for each treat-
ment plant used by the system. At
least 25 percent of the samples shall be
taken at locations within the distribu-
tion system reflecting the maximum
residence time of the water in the sys-
tem. The remaining 75 percent shall be
taken at representative locations in
the distribution system, taking into
account number of persons served, dif-
ferent sources of water and different
treatment methods employed. The re-
sults of all analyses per quarter shall
be arithmetically averaged and re-
ported to the State within 30 days of
the system's receipt of such results.
Results shall also be reported to EPA
until such monitoring requirements
have been adopted by the State. All
samples collected shall be used in the
computation of the average, unless the
analytical results are invalidated for
technical reasons. Sampling and anal-
yses shall be conducted in accordance
with the methods listed in paragraph
(e) of this section.
(2) Upon the written request of a
community water system, the moni-
toring frequency required by paragraph
(b)(l) of this section may be reduced by
the State to a minimum of one sample
analyzed for TTHMs per quarter taken
at a point in the distribution system
reflecting the maximum residence time
of the water in the system, upon a
written determination by the State
that the data from at least 1 year of
monitoring in accordance with para-
graph (b)(l) of this section and local
conditions demonstrate that total
trihalomethane concentrations will be
consistently below the maximum con-
taminant level.
(3) If at any time during which the
reduced monitoring frequency pre-
scribed under this paragraph applies,
the results from any analysis exceed
0.10 mg/1 of TTHMs and such results are
confirmed by at least one check sample
taken promptly after such results are
received, or if the system makes any
significant change to its source of
water or treatment program, the sys-
tem shall immediately begin moni-
toring in accordance with the require-
ments of paragraph (b)(l) of this sec-
tion, which monitoring shall continue
for at least 1 year before the frequency
may be reduced again. At the option of
the State, a system's monitoring fre-
quency may and should be increased
above the minimum in those cases
where it is necessary to detect vari-
ations of TTHM levels within the dis-
tribution system.
(c)(l) Upon written request to the
State, a community water system uti-
lizing only ground water sources may
seek to have the monitoring frequency
required by paragraph (b)(l) of this sec-
tion reduced to a minimum of one sam-
ple for maximum TTHM potential per
year for each treatment plant used by
the system taken at a point in the dis-
tribution system reflecting maximum
residence time of the water in the sys-
tem. The system shall submit the re-
sults of at least one sample for max-
imum TTHM potential using the proce-
dure specified in paragraph (g) of this
section. A sample must be analyzed
from each treatment plant used by the
system and be taken at a point in the
distribution system reflecting the max-
imum residence time of the water in
the system. The system's monitoring
frequency may only be reduced upon a
written determination by the State
that, based upon the data submitted by
the system, the system has a maximum
TTHM potential of less than 0.10 mg/1
and that, based upon an assessment of
the local conditions of the system, the
system is not likely to approach or ex-
ceed the maximum contaminant level
for total TTHMs. The results of all
analyses shall be reported to the State
within 30 days of the system's receipt
of such results. Results shall also be re-
ported to EPA until such monitoring
requirements have been adopted by the
State. All samples collected shall be
used for determining whether the sys-
tem must comply with the monitoring
requirements of paragraph (b) of this
392
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Environmental Protection Agency
§141.30
section, unless the analytical results
are invalidated for technical reasons.
Sampling and analyses shall be con-
ducted in accordance with the methods
listed in paragraph
-------
§141.31
40 CFR Ch. 1 (7-1-04 Edition)
required by the State for chlorate,
chlorite and chlorine dioxide when
chlorine dioxide is used. Standard plate
count analyses should also be required
by the State as appropriate before and
after any modifications;
(5) Consider inclusion in the plan of
provisions to maintain an active dis-
infectant residual throughout the dis-
tribution system at all times during
and after the modification.
(g) The water sampla for determina-
tion of maximum total trihalomethane
potential is taken from a point in the
distribution system that..reflects max-
imum residence time. Procedures for
sample collection and handling are
given in the methods. No reducing
agent is added to "quench" the chem-
ical reaction producing THMs at the
time of sample collection. The intent is
to permit the level of THM precursors
to be depleted and the concentration of
THMs to be maximized for the supply
being tested. Pour experimental pa-
rameters affecting maximum THM pro-
duction are pH, temperature, reaction
time and the presence of a disinfectant
residual. These parameters are dealt
with as follows: Measure the disinfect-
ant residual at the selected sampling
point. Proceed only if a measurable
disinfectant, residual is present. Collect
triplicate 40 ml water samples at the
pH prevailing at the time of sampling,
and prepare a method blank according
to the methods. Seal and store these
samples together for seven days at 25
°C or above. After this time period,
open one of the sample containers and
check for disinfectant residual. Ab-
sence of a disinfectant residual invali-
dates the sample for further analysis.
Once a disinfectant residual has been
demonstrated, open another of the
sealed samples and determine total
THM concentration using an approved
analytical method.
(h) The requirements in paragraphs
(a) through (g) of this section apply to
subpart H community water systems
which serve a population of 10,000 or
more until December 31, 2001. The re-
quirements in paragraphs (a) through
(g) of this section apply to community
water systems which use only ground
water not under the direct influence of
surface water that add a disinfectant
(oxidant) in any part of the treatment
process and serve a population of 10,000
or more until December 31, 2003. After
December 31, 2003, this section is no
longer applicable.
[44 PR 68641, Nov. 29, 1979, as amended at 45
FR 15545, 15547, Mar. 11, 1980; 58 FR 41345,
Aug. 3, 1993; 59 FR 62469, Deo. 5, 1994; 60 FR
34085, June 29, 1995; 63 FR 69464, Deo. 16, 1998;
65 FR 26022, May 4, 2000; 66 FR 3776, Jan. 16,
2001]
Subpart D—Reporting and
Recordkeeping
§ 141.31 Reporting requirements.
(a) Except where a shorter period is
specified in this part, the supplier of
water shall report to the State the re-
sults of any test measurement or anal-
ysis required by this part within (1)
The first ten days following the month
in which the result is received, or (2)
the first ten days following the end of
the required monitoring period as stip-
ulated by the State, whichever of these
is shortest.
(b) Except where a different reporting
period is specified in this part, the sup-
plier of water must report to the State
within 48 hours the failure to comply
with any national primary drinking
water regulation (including failure to
comply with1 monitoring' requirements)
set forth in this part.
(c) The supplier of water is not re-
quired to report analytical results to
the State in cases where a State lab-
oratory performs the analysis and re-
ports the results to the State office
which would normally receive such no-
tification from the supplier.
(d) The public water system, within
10 days of completing the public notifi-
cation requirements under Subpart Q
of this part for the initial public notice
and any repeat notices, must submit to
the primacy agency a certification that
it has fully complied with the public
notification regulations. The public
water system must include with this
certification a representative copy of
each type of notice distributed, pub-
lished, posted, and made available to
the persons served by the system and
to the media.
(e) The water supply system shall
submit to the State within the time
stated in the request copies of any
records required to tie maintained
394
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Environmental Protection Agency
§141.32
under §141.33 hereof or copies of any
documents then in existence which the
State or the Administrator is entitled
to inspect pursuant to the authority of
section 1445 of the Safe Drinking Water
Act or the equivalent provisions of
State law.
[40 PR 59570, Dec. 24, 1975, as amended at 45
FB 57345, Aug. 27. 1980; 65 FB 26022, May 4,
2000]
§ 141.32 Public notification,
The requirements in this section
apply until the requirements of Sub-
part Q of this part are applicable. Pub-
lic water systems where EPA directly
implements the public water system
supervision program must comply with
the requirements in Subpart Q of this
part on October 31, 2000. All other pub-
lic water systems must comply with
the requirements in Subpart Q of this
part on May 6, 2002 or on the date the
State-adopted rule becomes effective,
whichever comes first.
(a) Maximum contaminant levels
(MCLs), maximum residual disinfectant
levels (MRDLs). The owner or operator
of a public water system which fails to
comply with an applicable MCL or
treatment technique established by
this part or which fails to comply with
the requirements of any schedule pre-
scribed pursuant to a variance or ex-
emption, shall notify persons served by
the system as follows:
(1) Except as provided in paragraph.
(a)(3) of this section, the owner or oper-
ator of a public water system must
give notice:
(i) By publication in a daily news-
paper of general circulation in the area
served by the system as soon as pos-
sible, but in no case later than 14 days
after the violation or failure. If the
area served by a public water system is
not served by a daily newspaper of gen-
eral circulation, notice shall instead be
given by publication in a weekly news-
paper of general circulation serving the
area; and
(ii) By mail delivery (by direct mail
or with the water bill), or by hand de-
livery, not later than 45 days after the
violation or failure. The State may
waive mail or hand delivery if it deter-
mines that the owner or operator of
the public water system in violation
has corrected the violation or failure
within the 45-day period. The State
must make the waiver in writing and
within the 45-day period; and
(iii) For violations of the MCLs of
contaminants or MRDLs of disinfect-
ants that may pose an acute risk to
human health, by furnishing a copy of
the notice to the radio and television
stations serving the area served by the
public water system as soon as possible
but in no case later than 72 hours after
the violation. The following violations
are acute violations:
(A) Any violations specified by the
State as posing an acute risk to human
health.
(B) Violation of the MCL for nitrate
or nitrite as defined in §141.62 and de-
termined according to §141.23(i)(3).
(C) Violation of the MCL for total
coliforms, when fecal coliforms or E.
coli are present in the water distribu-
tion system, as specified in §141.63(b).
(D) Occurrence of a waterborne dis-
ease outbreak, as defined in §141.2, in
an unfiltered system subject to the re-
quirements of subpart H of this part,
after December 30. 1991 (see
(E) Violation of the MRDL for chlo-
rine dioxide as defined in §141.85 and
determined according to §141,133(c)(2).
(2) Except as provided in paragraph
(a)(3) of this section, following the ini-
tial notice given under paragraph (a Hi)
of this section, the owner or operator
of the public water system must give
notice at least once every three
months by mail delivery (by direct
mail or with the water bill) or by hand
delivery, for as long as the violation or
failure exists.
(3)(i) In lieu of the requirements of
paragraphs (a) (1) and (2) of this sec-
tion, the owner or operator of a com-
munity water system in an area that is
not served by a daily or weekly news-
paper of general circulation must give
notice by hand delivery or by contin-
uous posting in conspicuous places
within the area served by the system.
Notice by hand delivery or posting-
must begin as soon as possible, but no
later than 72 hours after the violation
or failure for acute violations (as de-
fined in paragraph (a)CD(iii) of this sec-
tion), or 14 days after the violation or
failure (for any other violation). Post-
ing must continue for as long as the
395
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§141.32
40 CFR Ch. I (7-1-04 Edition)
violation or failure exists. Notice by
hand delivery must be repeated at least
every three months for as long as the
violation or failure exists.
(ii) In lieu of the requirements of
paragraphs (a) (1) and (2). of this sec-
tion, the owner or operator of a non-
community water system may give no-
tice by hand delivery or by continuous
posting in conspicuous places within
the area served by the system. Notice
by hand delivery or posting must begin
as soon as possible, but no later than 72
hours after the violation or failure for
acute violations (as defined in para-
graph (a)(l)(iii) of this section), or 14
days after the violation or failure (for
any other violation). Posting must con-
tinue for as long as the violation or
failure exists. Notice by hand delivery
must be repeated at least every three
months for as long as the violation or
failure exists.
(b) Other violations, variances, exemp-
tions. The owner or operator of a public
water system which fails to perform
monitoring required by section 1445(a)
of the Act (including monitoring re-
quired by the National Primary Drink-
ing Water Regulations (NPDWRs) of
this part), fails to comply with a test-
ing procedure established by this part,
is subject to a variance granted under
section 1415(a)(l)(A) or 1415(a)(2) of the
Act, or is subject to an exemption
under section 1416 of the Act, shall no-
tify persons served by the system as
follows:
(1) Except as provided in paragraph
(b)(3) or (b)(4) of this section, the owner
or operator of a public water system
must give notice within three months
of the violation or granting of a vari-
ance or exemption by publication in a
daily newspaper of general circulation
in the area served by the system. If the
area served by a public water system is
not served by a daily newspaper of gen-
eral circulation, notice shall instead be
given by publication in a weekly news-
paper of general circulation serving the
area.
(2) Except as provided in paragraph
(b)(3) or (b)(4) of this section, following
the initial notice given under para-
graph (b)(l) of this section, the owner
or operator of the public water system
must give notice at least once every
three months by mail delivery (by di-
rect mail or with the water bill) or by
hand delivery, for as long as the viola-
tion exists. Repeat notice of the exist-
ence of a variance or exemption must
be given every three months for as long
as the variance or exemption remains
in effect.
(3)(i) In lieu of the requirements of
paragraphs (b)(l) and (b)(2) of this sec-
tion, the owner or operator of a com-
munity water system in an area that is
not served by a daily or weekly news-
paper of general circulation must give
notice, within three months of the vio-
lation or granting of the variance or
exemption, by hand delivery or by con-
tinuous posting in conspicuous places
with the area served by the system.
Posting must continue for as long as
the violation exists or a variance or ex-
emption remains in effect. Notice by
hand delivery must be repeated at least
every three months for as long as the
violation exists or a variance or ex-
emption remains in effect.
(ii) In lieu of the requirements of
paragraphs (b)(l) and (b)(2) of this sec-
tion, the owner or operator of a non-
community water system may give no-
tice, within three months of the viola-
tion or the granting of the variance or
exemption, by hand delivery or by con-
tinuous posting in conspicuous places
within the area served by the system.
Posting must continue for as long as
the violation exists, or a variance or
exemption remains in effect. Notice by
hand delivery must be repeated at least
every three months for as long as the
violation exists or a variance or ex-
emption remains in effect.
(4) In lieu of the requirements of
paragraphs (b)(l), (b)(2), and (b)(3) of
this section, the owner or operator of a
public water system, at the discretion
of the State, may provide less frequent
notice for minor,-monitoring violations
as defined by the State, if EPA has ap-
proved the State's application for a
program revision under §142,16. Notice
of such violations must be given no less
frequently than annually.
(c) Notice to new billing units. The
owner or operator of a community
water system must give a copy of the
most recent public notice for any out-
standing violation of any maximum
contaminant level, or any maximum
residual disinfectant level, or any
396
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Environmental Protection Agency
§141.32
treatment technique requirement, or
any variance or exemption schedule to
all new billing units or new hookups
prior to or at the time service begins.
(d) General content of public notice.
Each notice required by this section
must provide a clear and readily under-
standable explanation of the violation,
any potential adverse health effects,
the population at risk, the steps that
the public water system is taking to
correct such violation, the necessity
for seeking alternative water supplies,
if any, and any preventive measures
the consumer should take until the
violation is corrected. Each notice
shall be conspicuous and shall not con-
tain unduly technical language, unduly
small print, or similar problems that
frustrate the purpose of the notice.
Each notice shall Include the telephone
number of the owner, operator, or des-
Ignee of the public water system as a
source of additional information con-
cerning the notice. Where appropriate,
the notice shall be multi-lingual.
(e) Mandatory health effects language.
When providing the information on po-
tential adverse health effects required
by paragraph (d) of this section in no-
tices of violations of maximum con-
taminant levels or treatment tech-
nique requirements, or notices of the
granting or the continued existence of
exemptions or variances, or notices of
failure to comply with a variance or
exemption schedule, the owner or oper-
ator of a public water system shall in-
clude the language specified below for
each contaminant. (If language for a
particular contaminant is not specified
below at the time notice is required,
this paragraph does not apply.)
(1) Trichloroethylene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that tri-
chloroethylene is a health concern at
certain levels of exposure. This chem-
ical is a common metal cleaning and
dry cleaning fluid. It generally gets
into drinking water by improper waste
disposal. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed at lower levels over
long periods of time. EPA has set forth
the enforceable drinking water stand-
ard for trichloroethylene at 0.005 parts
per million (ppm) to reduce the risk of
cancer or other adverse health effects
which have been observed in laboratory
animals. Drinking water which meets
this standard Is associated with little
to none of this risk and should be con-
sidered safe.
(2) Carbon tetrachloride. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that car-
bon tetrachloride is a health concern
at certain levels of exposure. This
chemical was once a popular household
cleaning fluid. It generally gets into
drinking water by improper waste dis-
posal. This chemical has been shown to
cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed at lower levels over
long periods of of time. EPA has set
the enforceable drinking water stand-
ard for carbon tetrachloride at 0.005
parts per million (ppm) to reduce the
risk of cancer or other adverse health
effects which have been observed in
laboratory animals. Drinking water
which meets this standard is associated
with little to none of this risk and
should be considered safe.
(3) 1,2-Dichloroethane. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that 1,2-
dichloroethane is a health concern at
certain levels of exposure. This chem-
ical is used as a cleaning fluid for fats.
oils, waxes, and resins. It generally
gets into drinking water from improper
waste disposal. This chemical has been
shown to cause cancer in laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Chemicals that
cause cancer in laboratory animals
also may increase the risk of cancer in
humans who are exposed at lower lev-
els over long periods of time. EPA has
set the enforceable drinking water
standard for 1,2-dichloroethane at 0.005
parts per million (ppm) to reduce the
397
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§141.32
40 CFR Ch,! (7-1-04 Edition)
risk of cancer or other adverse health
effects which have been observed in
laboratory animals. Drinking water
which meets this standard is associated
with little to none of this risk and
should be considered safe.
(4) Vinyl chloride. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that vinyl chloride
is a health concern at certain levels of
exposure. This chemical is used in in-
dustry and is found in drinking water
as a result of the breakdown of related
solvents. The solvents are used as
cleaners and degreasers of metals and
generally get into drinking water by
improper waste disposal. This chemical
has been associated with significantly
increased risks of cancer among cer-
tain industrial workers who were ex-
posed to relatively large amounts of
this chemical during their working ca-
reers. This chemical has also been
shown to cause cancer in laboratory
animals when the animals are exposed
at high levels over their lifetimes.
Chemicals that cause increased risk of
cancer among exposed industrial work-
ers and in laboratory animals also may
increase the risk of cancer in humans
who are exposec, at lower levels over
long periods of time. EPA has set the
enforceable drinking water standard
for vinyl chloride at 0.002 part per mil-
lion (ppm) to reduce the risk of cancer
or other adverse health effects which
have been observed in humans and lab-
oratory animals. Drinking water which
meets this standard is associated with
little to none of this risk and should be
considered safe.
(5) Benzene. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that benzene is a health
concern at certain levels of exposure.
This chemical is used as a solvent and
degreaser of metals. It is also a major
component of gasoline. Drinking water
contamination generally results from
leaking undergound gasoline and petro-
leum tanks or improper waste disposal.
This chemical has been associated with
significantly increased risks of leu-
kemia among certain industrial work-
ers who were exposed to relatively
large amounts of this chemical during
their working careers. This chemical
has also been shown to cause cancer in
laboratory animals when the animals
are exposed at high levels over their
lifetimes. Chemicals that cause in-
creased risk of cancer among exposed
industrial workers and in laboratory
animals also may increase the risk of
cancer in humans who are exposed at
lower levels over long periods of time.
EPA has set the enforceable drinking
water standard for benzene at 0.005
parts per million (ppm) to reduce the
risk of cancer or other adverse health
effects which have been observed in hu-
mans and laboratory animals. Drinking
water which meets this standard is as-
sociated with little to none of this risk
and should be considered safe.
(6) 1,1-Dichloroetfiylene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that 1,1-
dichloroethylene is a health concern at
certain levels of exposure. This chem-
ical is used in industry and is found in
drinking water as a result of the break-
down of related solvents. The solvents
are used as cleaners and degreasers of
metals and generally get into drinking
water by improper waste disposal. This
chemical has been shown to cause liver
and kidney damage in laboratory ani-
mals such as rats and mice when the
animals are exposed at high levels over
their lifetimes. Chemicals which cause
adverse effects in laboratory animals
also may cause adverse health effects
in humans who are exposed at lower
levels over long periods of time. EPA
has set the enforceable drinking water
standard for 1,1-dichloroethylene at
0.007 parts per million (ppm) to reduce
the risk of these adverse health effects
which have been observed in laboratory
animals. Drinking water which meets
this standard is associated with little
to none of this risk and should be con-
sidered safe.
(7) Para-dichlorobenzene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
para-dichlorobenzene is a health con-
cern at certain levels of exposure. This
chemical is a component of deodor-
izers, moth balls, and pesticides. It
generally gets into drinking water by
improper waste disposal. This chemical
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Environmental Protection Agency
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has been shown to cause liver and kid-
ney damage in laboratory animals such
as rats and mice when the animals are
exposed to high levels over their life-
times. Chemicals which cause adverse
effects in laboratory animals also may
cause adverse health effects in humans
who are exposed at lower levels over
long periods of time. EPA has set the
enforceable drinking water standard
for para-dichlorobenzene at 0.075 parts
per million (ppm) to reduce the risk of
these adverse health effects which have
been observed in laboratory animals.
Drinking water which meets this
standard is associated with little to
none of this risk and should be consid-
ered safe.
(8) 1,1,1-Trichloroethane. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that the
1,1,1-trichloroethane is a health con-
cern at certain levels of exposure. This
chemical is used as a cleaner and
degreaser of metals. It generally gets
into drinking water by improper waste
disposal. This chemical has been shown
to damage the liver, nervous system,
and circulatory system of laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Some industrial
workers who were exposed to relatively
large amounts of this chemical during
their working careers also suffered
damage to the liver, nervous system,
a.nd circulatory system. Chemicals
which cause adverse effects among ex-
posed industrial workers and in labora-
tory animals also may cause adverse
health effects in humans who are ex-
posed at lower levels over long periods
of time. EPA has set the enforceable
drinking water standard for 1,1,1-tri-
chloroethane at 0.2 parts per million
(ppm) to protect against the risk of
these adverse health effects which have
been observed in humans and labora-
tory animals. Drinking" water which
meets this standard is associated with
little to none of this risk and should be
considered safe.
(9) Fluoride.
[NOTE: EPA is not specifying language that
must be included in a public notice for a vio-
lation of the fluoride maximum contaminant
level in this section because §143.5 of this
part includes the necessary information. See
paragraph (f) of this section.]
(10) Microbiological contaminants (for
use when there is a violation of the
treatment technique requirements for
filtration and disinfection in subpart H
or subpart P of this part). The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that the
presence of microbiological contami-
nants are a health concern at certain
levels of exposure. If water is inad-
equately treated, microbiological con-
taminants in that water may cause dis-
ease. Disease symptoms may include
diarrhea, cramps, nausea, and possibly
jaundice, and any associated headaches
and fatigue. These symptoms, however,
are not just associated with disease-
causing organisms in drinking water,
but also may be caused by a number of
factors other than your drinking
water. EPA has set enforceable require-
ments for treating drinking water to
reduce the risk of these adverse health
effects. Treatment such as filtering and
disinfecting the water removes or de-
stroys microbiological contaminants.
Drinking water which is treated to
meet EPA requirements is associated
with little to none of this risk and
should be considered safe.
(11) Total coliforms (To be used when
there is a violation of §l41.63(a). and
not a violation of §141.63(b)). The
United States Environmental Protec-
tion Agency (EPA) sets drinking water
standards and has determined that the
presence of total coliforms is a possible
health concern. Total coliforms are
common in the environment and are
generally not harmful themselves. The
presence of these bacteria in drinking
water, however, generally is a result of
a problem with water treatment or the
pipes which distribute the water, and
indicates that the water may be con-
taminated with organisms that can
cause disease. Disease symptoms may
include diarrhea, cramps, nausea, and
possibly jaundice, and any associated
headaches and fatigue. These symp-
toms, however, are not just associated
with disease-causing organisms in
drinking water, but also may be caused
by a number of factors other than your
drinking water. EPA has set an en-
forceable drinking water standard for
total coliforms to reduce the risk of
these adverse health effects. Under this
399
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§141,32
40 CFR Ch, 1 (7-1-04 Edition)
standard, no more than 5.0 percent of
the samples collected during a month
can contain these bacteria, except that
systems collecting fewer than 40 sam-
ples/month that have one total coli-
form-positive sample per month are
not violating the standard. Drinking
water which meets this standard is
usually not associated with a health
risk from disease-causing bacteria and
should be considered safe.
(12) Fecal Cottforms/E. coli (To be used
when there is a violation of §141.63(b)
or both §141.63 (a) and (b)). The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that the
presence of fecal coliforms- or E. coli is
a serious health concern. Fecal coli-
forms and E. coli are generally not
harmful themselves, but their presence
in drinking water is serious because
they usually are associated with sew-
age or animal wastes. The presence of
these bacteria in drinking water is gen-
erally a result of a problem with water
treatment or the pipes which distribute
the water, and indicates that the water
may be contaminated with organisms
that can cause disease. Disease symp-
toms may include diarrhea, cramps,
nausea, and possibly jaundice, and as-
sociated headaches and fatigue. These
symptoms, however, are not just asso-
ciated with disease-causing organisms
in drinking water, but also may be
caused by a number of factors other
than your drinking water. EPA has set
an enforceable drinking water standard
for fecal conforms and E. coli to reduce
the risk of these adverse health effects.
Under this standard all drinking water
samples must be free of these bacteria.
Drinking water which meets this
standard is associated with little or
none of this risk and should be consid-
ered safe. State and local health au-
thorities recommend that consumers
take the following precautions: [To be
inserted by the public water system,
according to instructions from State or
local authorities].
(13) Lead. The United States Environ-
mental Protection Agency (EPA) sets
drinking water standards and has de-
termined that lead is a health concern
at certain exposure levels. Materials
that contain lead have frequently been
used in the construction of water sup-
ply distribution systems, and plumbing
systems in private homes and other
buildings. The most commonly found
materials include service lines, pipes,
brass and bronze fixtures, and solders
and fluxes. Lead in these materials can
contaminate drinking water as a result
of the corrosion that takes place when
water comes into contact with those
materials. Lead can cause a variety of
adverse health effects in humans. At
relatively low levels of exposure, these
effects may include interference with
red blood cell chemistry, delays In nor-
mal physical and mental development
in babies and young children, .slight
deficits in the attention span, hearing,
and learning abilities of children, and
slight increases in the blood pressure of
some adults. EPA's national primary
drinking water regulation requires all
public water systems to optimize cor-
rosion control to minimize lead con-
tamination resulting from the corro-
sion of plumbing materials. Public
water systems serving 50,000 people or
fewer that have lead concentrations
below 15 parts per billion (ppb) in more
than 90% of tap water samples (the
EPA "action level") have optimized
their corrosion control treatment. Any
water system that exceeds the action
level must also monitor their source
water to determine whether treatment
to remove lead In source water is need-
ed. Any water system that continues to
exceed the action level after installa-
tion of corrosion control and/or source
water treatment must eventually re-
place all lead service lines contributing
in excess of 15 (ppb) of lead to drinking
water. Any water system that exceeds
the action level must also undertake a
public education program to inform
consumers of ways they can reduce
their exposure to potentially high lev-
els of lead in drinking water.
(14) Copper. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that copper is a health con-
cern at certain exposure levels. Copper,
a reddish-brown metal, is often used to
plumb residential and commercial
structures that are connected to water
distribution systems. Copper contami-
nating drinking water as a corrosion
byproduct occurs as the result of the
corrosion of copper pipes that remain
400
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Environmental Protection Agency
§141,32
in contact with water for a prolonged
period of time. Copper is an essential
nutrient, but at high doses it has been
shown to cause stomach and intestinal
distress, liver and kidney damage, and
anemia. Persons with Wilson's disease
may be at a higher risk of health ef-
fects due to copper than the general
public. BPA's national primary drink-
ing water regulation requires all public
water systems to install optimal corro-
sion control to minimize copper con-
tamination resulting from the corro-
sion of plumbing materials. Public
water systems serving 50,000 people or
fewer that have copper concentrations
below 1.3 parts per million (ppm) in
more than 90% of tap water samples
(the EPA "action level") are not re-
quired to install or improve their
treatment. Any water system that ex-
ceeds the action level must also mon-
itor their source water to determine
whether treatment to remove copper in
source water is needed.
(15) Asbestos, The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that asbestos fibers greater
than 10 micrometers in length are a
health concern at certain levels of ex-
posure. Asbestos is a naturally occur-
ring" mineral. Most asbestos fibers in
drinking water are less than 10 mi-
crometers in length and occur in drink-
ing water from natural sources and
from corroded asbestos-cement pipes in
the distribution system. The major
uses of asbestos were in the production
of cements, floor tiles, paper products,
paint, and caulking; in transportation-
related applications; and in the produc-
tion of textiles and plastics. Asbestos
was once a popular insulating and fire
retardent material. Inhalation studies
have shown that various forms of as-
bestos have produced lung tumors in
laboratory animals. The available in-
formation on the risk of developing
gastrointestinal tract cancer associ-
ated with the ingestion of asbestos
from drinking water is limited. Inges-
tion of intermediate-range chrysotile
asbestos fibers greater than 10 microm-
eters in length is associated with caus-
ing benign tumors in male rats. Chemi-
cals that cause cancer in laboratory
animals also may increase the risk of
cancer in humans who are exposed over
long periods of time. EPA has set the
drinking water standard for asbestos at
7 million long fibers per liter to reduce
the potential risk of cancer or other
adverse health effects which have been
observed in laboratory animals. Drink-
ing water which meets the EPA stand-
ard is associated with little to none of
this risk and should be considered safe
with respect to asbestos.
(16) Barium. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that barium is a health
concern at certain levels of exposure.
This inorganic chemical occurs natu-
rally in some aquifers that serve as
sources of ground water. It is also used
in oil and gas drilling muds, auto-
motive paints, bricks, tiles and jet
fuels. It generally gets into drinking
water after dissolving from naturally
occurring minerals in the ground. This
chemical may damage the heart and
cardiovascular system, and is associ-
ated with high blood pressure in lab-
oratory animals such as rats exposed
to high levels during their lifetimes. In
humans, EPA believes that effects from
barium on blood pressure should not
occur below 2 parts per million (ppm)
in drinking water. EPA has set the
drinking water standard for barium at
2 parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to barium,
(17) Cadmium. The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that cadmium is a health
concern at certain levels of exposure.
Food and the smoking of tobacco are
common sources of general exposure.
This inorganic metal is a contaminant
in the metals used to galvanize pipe. It
generally gets into water by corrosion
of galvanized pipes or by improper
waste disposal. This chemical has been
shown to damage the kidney in ani-
mals such as rats and mice when the
animals are exposed at high levels over
their lifetimes. Some industrial work-
ers who were exposed to relatively
large amounts of this chemical during
working careers also suffered damage
401
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§141.32
40 CFR Ch. I (7-1-04 Edition)
to the kidney. EPA has set the drink-
ing water standard for cadmium at
0.005 parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to cadmium,
(18) Chromium. The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that chromium is a health
concern at certain levels of exposure.
This inorganic metal occurs naturally
in the ground and is often used in the
electroplating of metals. It generally
gets into water from runoff from old
mining operations and improper waste
disposal from plating operations. This
chemical has been shown to damage
the kidney, nervous system, and the
circulatory system of laboratory ani-
mals such as rats and mice when the
animals are exposed at high levels.
Some humans who were exposed to
high levels of this chemical suffered
liver and kidney damage, dermatitis
and respiratory problems. EPA has set
the drinking water standard for chro-
mium at 0.1 parts per million (ppm) to
protect against the risk of these ad-
verse health effects. Drinking water
that meets the EPA standard is associ-
ated with little to none of this risk and
is considered safe with respect to chro-
mium.
(19) Mercury. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that mercury is a health
concern at certain levels of exposure.
This inorganic metal is used in elec-
trical equipment and some water
pumps. It usually gets into water as a
result of improper waste disposal. This
chemical has been shown to damage
the kidney of laboratory animals such
as rats when the animals are exposed
at high levels over their lifetimes. EPA
has set the drinking water standard for
mercury at 0.002 parts per million
(ppm) to protect against the risk of
these adverse health effects. Drinking
water that meets the EPA standard is
associated with little to none of this
risk and is considered safe with respect
to mercury.
(20) Nitrate. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that nitrate poses an acute
health concern at certain levels of ex-
posure. Nitrate is used in fertilizer and
is found in sewage and wastes from
human and/or farm animals and gen-
erally gets into drinking water from
those activities. Excessive levels of ni-
trate in drinking water have caused se-
rious illness and sometimes death in
infants under six months of age. The
serious illness in infants is caused be-
cause nitrate is converted to nitrite in
the body. Nitrite interferes with the
oxygen carrying capacity of the child's
blood. This is an acute disease in that
symptoms can develop rapidly in in-
fants. In most cases, health deterio-
rates over a period of days. Symptoms
include shortness of breath and blue-
ness of the skin. Clearly, expert med-
ical advice should be sought imme-
diately if these symptoms occur. The
purpose of this notice is to encourage
parents and other responsible parties
to provide infants with an alternate
source of drinking water. Local and
State health authorities are the best
source for information concerning al-
ternate sources of drinking water for
infants. EPA has set the drinking
water standard at 10 parts per million
(ppm) for nitrate to protect against the
risk of these adverse effects. EPA has
also set a drinking water standard for
nitrite at 1 ppm. To allow for the fact
that the toxicity of nitrate and nitrite
are additive, EPA has also established
a standard for the sum of nitrate and
nitrite at 10 ppm. Drinking water that
meets the EPA standard is associated
with little to none of this risk and is
considered safe with respect to nitrate.
(21) Nitrite. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that nitrite poses an acute
health concern at certain levels of ex-
posure. This inorganic chemical is used
in fertilizers and is found in sewage and
wastes from humans and/or farm ani-
mals and generally gets into drinking-
water as a result of those activities.
While excessive levels of nitrite in
drinking water have not been observed,
other sources of nitrite have caused se-
rious illness and sometimes death in
infants under six months of age. The
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§141.32
serious illness in Infants is caused be-
cause nitrite interferes with the oxy-
gen carrying capacity of the child's
blood. This is an acute disease in that
symptoms can develop rapidly. How-
ever, in most cases, health deteriorates
over a period of days. Symptoms in-
clude shortness of breath and blueness
of the skin. Clearly, expert medical ad-
vice should be sought immediately if
these symptoms occur. The purpose of
this notice is to encourage parents and
other responsible parties to provide in-
fants with an alternate source of drink-
ing water. Local and State health au-
thorities are the best source for infor-
mation concerning alternate sources of
drinking water for infants. EPA has set
the drinking water standard at 1 part
per million (ppm) for nitrite to protect
against the risk of these adverse ef-
fects. EPA has also set a drinking
water standard for nitrate (converted
to nitrite in humans) at 10 ppm and for
the sum of nitrate and nitrite at 10
ppm. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to nitrite.
(22) Selenium. The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that selenium is a health
concern at certain high levels of expo-
sure. Selenium is also an essential nu-
trient at low levels of exposure. This
inorganic chemical is found naturally
in food and soils and is used in elec-
tronics, photocopy operations, the
manufacture of glass, chemicals, drugs,
and as a fungicide and a feed additive.
In humans, exposure to high levels of
selenium over a long period of time has
resulted in a number of adverse health
effects, including a loss of feeling and
control In the arms and legs. EPA has
set the drinking water standard for se-
lenium at 0,05 parts per million (ppm)
to protect against the risk of these ad-
verse health effects. Drinking water
that meets the EPA standard is associ-
ated with little to none of this risk and
is considered safe with respect to sele-
nium.
(23) Acrylamide. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that acrylamide is
a health concern at certain levels of
exposure. Polymers made from acryl-
amide are sometimes used to treat
water supplies to remove particulate
contaminants. Acrylamide has been
shown to cause cancer in laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Chemicals that
cause cancer in laboratory animals
also may increase the risk of cancer in
humans who are exposed over long pe-
riods of time. Sufficiently large doses
of acrylamide are known to cause neu-
rological injury. EPA has set the
drinking water standard for acrylamide
using a treatment technique to reduce
the risk of cancer or other adverse
health effects which have been ob-
served in laboratory animals. This
treatment technique limits the amount
of acrylamide in the polymer and the
amount of the polymer which may be
added to drinking water to remove par-
ticulates. Drinking water systems
which comply with this treatment
technique have little to no risk and are
considered safe with respect to acryl-
amide,
(24) Alachlor. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that alachlor is a health
concern at certain levels of exposure.
This organic chemical is a widely used
pesticide. When soil and climatic con-
ditions are favorable, alachlor may get
into drinking water by runoff into sur- -
face water or by leaching into ground
water. This chemical has been shown
to cause cancer In laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer In laboratory animals also may
increase the risk of cancer in humans
who are exposed over long periods of
time, EPA has set the drinking water
standard for alachlor at 0.002 parts per
million (ppm) to reduce the risk of can-
cer or other adverse health effects
which have been observed in laboratory
animals, Drinking- water that meets
this standard is associated with little
to none of this risk and is considered
safe with respect to alachlor.
(25) Aldicarb. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that aldicarb is a health
403
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§141.32
40 CFR Ch. I (7-1-04 Edition)
concern at certain levels of exposure,
Aldiearb is a widely used pesticide.
Under certain soil and climatic condi-
tions (e.g., sandy soil and high rain-
fall), aldicarb may leach into ground
water after normal agricultural appli-
cations to crops such as potatoes or
peanuts or may enter drinking water
supplies as a result of surface runoff.
This chemical has been shown to dam-
age the nervous system in laboratory
animals such as rats and dogs exposed
to high levels. EPA has set the drink-
ing water standard for aldicarb at 0.003
parts per million (ppm) to protect
against the risk of adverse health ef-
fects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to aldicarb.
(26) Aldicarb sulfoxide. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
aldicarb sulfoxide is a health concern
at certain levels of exposure. Aldicarb
is a widely used pesticide. Aldicarb
sulfoxide in ground water is primarily
a breakdown product of aldicarb. Under
certain soil and climatic conditions
(e.g., sandy soil and high rainfall),
aldicarb sulfoxide may leach into
ground water after normal agricultural
applications to crops such as potatoes
or peanuts or may enter drinking
water supplies as a result of surface
runoff. This chemical has heen shown
to damage the nervous system in lab-
oratory animals such as rats and dogs
exposed to high levels. EPA.has set the
drinking water standard for aldicarb
sulfoxide at 0.004 parts per million
(ppm) to protect against the risk of adt
verse health effects. Drinking water
that meets the EPA standard is associ-
ated with little to none of this risk and
is considered safe with respect to
aldicarb sulfoxide.
(27) Aldicarb sulfone. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
aldicarb sulfone is a health concern at
certain levels of exposure. Aldicarb is a
widely used pesticide. Aldicarb sulfone
is formed from the breakdown of
aldicarb and is considered for registra-
tion as a pesticide under the name
aldoxycarb. Under certain soil and cli-
matic conditions (e.g.. sandy soil and
high rainfall), aldicarb sulfone may
leach into ground water after normal
agricultural applications to crops such
as potatoes or peanuts or may enter
drinking, water supplies as a, result of
surface runoff. This chemical has been
shown to damage the nervous system
in laboratory animals such as rats and
dogs exposed to high levels. EPA has
set the drinking water standard for
aldicarb sulfone at 0.002 parts per mil-
lion (ppm) to protect against the risk
of adverse health effects. Drinking
water that meets the EPA standard is
associated with little to none of this
risk and is considered safe with respect
to aldicarb sulfone.
(28) Atrazine. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that atrazine is a health
concern at certain levels of exposure.
This organic chemical is a herbicide.
When soil and climatic conditions are
favorable, atrazine may get into drink-
ing water by runoff into surface water
or by leaching- into ground water. This
chemical has been shown to affect off-
spring of rats and the heart of dogs.
EPA has set the drinking water stand-
ard for atrazine at 0.003 parts per mil-
lion (ppm) to protect against the risk
of these adverse health effects. Drink-
ing water that meets the EPA standard
is associated with little to none of this
risk and is considered safe with respect
to atrazine.
(29) Carbofuran, The United States
Environmental Protection Agency
(EPA) sets- drinking water standards
and has determined that carbofuran is
a health concern at certain levels of
exposure. This organic, chemical is a
pesticide. When soil and climatic con-
ditions are favorable, carbofuran may
get into drinking- water by runoff into
surface water or by leaching into
ground water. This chemical has been
shown to damage the nervous and re-
productive systems of laboratory ani-
mals such as rats and mice exposed at
high levels over their lifetimes. Some
humans who were exposed to relatively
large amounts of this chemical during
their working careers also suffered
damage to the nervous system. Effects
on the nervous system are generally
rapidly reversible. EPA has set the
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Environmental Protection Agency
§141.32
drinking water standard for carbofuran
at 0.04 parts per million (ppm) to pro-
tect against the risk of these adverse
health effects. Drinking water that
meets the EPA standard is associated
with little to none of this risk and is
considered safe with respect to
carbofuran.
(30) Chlordane. The United States En-
vironmental Protection Agency (EPA
sets drinking water standards and has
determined that chlordane is a health
concern at certain levels of exposure.
This organic chemical is a pesticide
used to control termites. Chlordane is
not very mobile in soils. It usually gets
into drinking water after application
near water supply intakes or wells.
This chemical has been shown to cause
cancer in laboratory animals such as
rats and mice when the animals are ex-
posed at high levels over their life-
times. Chemicals that cause cancer in
laboratory animals also may increase
the risk of cancer in humans who are
exposed over long periods of time. EPA
has set the drinking water standard for
chlordane at 0.002 parts per million
(ppm) to reduce the risk of cancer or
other adverse health effects which have
been observed in laboratory animals.
Drinking water that meets the EPA
standard is associated with little to
none of this risk and is considered safe
with respect to chlordane.
(31) Dibromachloropropane (DBCP).
The United States Environmental Pro-
tection Agency (EPA) sets drinking
water standards and has determined
that DBCP is a health concern at cer-
tain levels of exposure. This organic
chemical was once a popular pesticide.
When soil and climatic conditions are
favorable, dibromochloropropane may
get into drinking water by runoff into
surface water or by leaching into
ground water. This chemical has been
shown to cause cancer in laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Chemicals that
cause cancer in laboratory animals
also may increase the risk of cancer in
humans who are exposed over long pe-
riods of time. EPA has set the drinking
water standard for DBCP at 0.0002 parts
per million (ppm) to reduce the risk of
cancer or other adverse health effects
which have been observed in laboratory
animals. Drinking water that meets
the EPA standard is associated with
little to none of this risk and is consid-
ered safe with respect to DBCP.
(32) o-Dichlorobenzene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that o-
dichlorobenzene is a health concern at
certain levels of exposure. This organic
chemical is used as a solvent in the
production of pesticides and dyes. It
generally gets into water by improper
waste disposal. This chemical has been
shown to damage the liver, kidney and
the blood cells of laboratory animals
such as rats and mice exposed to high
levels during their lifetimes. Some in-
dustrial workers who were exposed to
relatively large amounts of this chem-
ical during working careers also suf-
fered damage to the liver, nervous sys-
tem, and circulatory system. EPA has
set the drinking water standard for o-
dichlorobenzene at 0.6 parts per million
(ppm) to protect against the risk of
these adverse health effects. Drinking
water that meets the EPA standard is
associated with little to none of this
risk and is considered safe with respect
to o-dichlorobenzene.
(33) cis-l,2-Dichlowethylene. The
United States Environmental Protec-
tion Agency (EPA) establishes drinking
water standards and has determined
that cis-l,2-dichloroethylene is a
health concern at certain levels of ex-
posure. This organic chemical is used
as a solvent and intermediate in chem-
ical production. It generally gets into
water by improper waste disposal. This
chemical has been shown to damage
the liver, nervous system, and cir-
culatory system of laboratory animals
such as rats and mice when exposed at
high levels over their lifetimes. Some
humans who were exposed to relatively
large amounts of this chemical also
suffered damage to the nervous system.
EPA has set the drinking water stand-
ard for cis-l,2-dichloroethylene at 0.07
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to cis-1,2-
dichloroethylene.
405
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§141.32
40 CFR Ch. I (7-1-04 Edition)
(34) trans-1,2-Dichloroethylene. The
United States Environmental Protec-
tion Agency (EPA) establishes drinking
water standards and has determined
that trans-l,2-dichloroethylene is a
health concern at certain levels of ex-
posure. This organic chemical is used
as a solvent and intermediate in chem-
ical production. It generally gets into
water by improper waste disposal. This
chemical has been shown to damage
the liver, nervous system, and the cir-
culatory system of laboratory animals
such as rats and mice when exposed at
high levels over their lifetimes. Some
humans who were exposed to relatively
large amounts of this chemical also
suffered damage to the nervous system.
EPA has set drinking water standard
for trans-1,2-dichloroethylene at 0.1
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to trans-1,2-
dichloroethylene.
(35) 1,2-Dichloropropane. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that 1,2-
dichloropropane is a health concern at
certain levels of exposure. This organic
chemical is used as a solvent and pes-
ticide. When soil and climatic condi-
tions are favorable, 1,2-dichloropropane
may get into drinking water by runoff
into surface water or by leaching- into
ground water. It may also get Into
drinking water through improper waste
disposal. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed over long periods of
time. EPA has set the drinking water
standard for 1,2-dichloropropane at
0.005 parts per million (ppm) to reduce
the risk of cancer or other adverse
health effects which have been ob-
served in laboratory animals. Drinking
water that meets the EPA standard is
associated with little to none of this
risk and is considered safe with respect
to 1,2-dichloropropane.
(36) 2,4-D. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that 2,4r-D is a health con-
cern at certain levels of exposure. This
organic chemical is used as a herbicide
and to control algae in reservoirs.
When soil and climatic conditions are
favorable, 2,4-D may get into drinking
water by runoff into surface water or
by leaching into ground water. This
chemical has been shown to damage
the liver and kidney of laboratory ani-
mals such as rats exposed at high lev-
els during their lifetimes. Some hu-
mans who were exposed to relatively
large amounts of this chemical also
suffered damage to the nervous system.
EPA has set the drinking water stand-
ard for 2,4-D at 0.0? parts per million
(ppm) to protect against the risk of
these adverse health effects. Drinking
water that meets the EPA standard is
associated with little to none of this
risk and is considered safe with respect
to 2,4-D.
(37) Epichlorohydrin. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
epichlorohydrin is a health concern at
certain levels of exposure. Polymers
made from epichlorohydrin are some-
times used in the treatment of water
supplies as a flocculent to remove par-
ticulates. Epichlorohydrin generally
gets into drinking water by improper
use of these polymers. This chemical
has been shown to cause cancer in lab-
oratory animals such as rats and mice
when the animals are exposed at high
levels over their lifetimes. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time. EPA has set the
drinking water standard for
epichlorohydrin using a treatment
technique to reduce the risk of cancer
or other adverse health effects which
have "been observed in laboratory ani-
mals. This treatment technique limits
the amount of epichlorohydrin in the
polymer and the amount of the poly-
mer which may be added to drinking
water as a flocculent to remove partic-
ulates. Drinking water systems which
comply with this treatment technique
406
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Environmental Protection Agency
§141.32
have little to no risk and are consid-
ered safe with respect to
epi chl orohy drin.
(38) Ethylbenzene. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined ethylbenzene is a
health concern at certain levels of ex-
posure. This organic chemical is a
major component of gasoline. It gen-
erally gets into water by Improper
waste disposal or leaking gasoline
tanks. This chemical has been shown
to damage the kidney, liver, and nerv-
ous system of laboratory animals such
as rats exposed to high levels during
their lifetimes. EPA has set the drink-
ing water standard for ethylbenzene at
0.7 part per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to ethylbenzene.
(39) Ethylene dibromide (EDB). The
United States Environmental Protec-
tion Agency (EPA) sets drinking water
standards and has determined that
EDB is a health concern at certain lev-
els of exposure. This organic chemical
was once a popular pesticide. When soil
and climatic conditions are favorable.
EDB may get into drinking- water by
runoff into surface water or by leach-
ing into ground water. This chemical
has been shown to cause cancer in lab-
oratory animals such as rats and mice
when the animals are exposed at high
levels over their lifetimes. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time. EPA has set the
drinking water standard for EDB at
0.00005 part per million (ppm) to reduce
the risk of cancer or other adverse
health effects which have been ob-
served in laboratory animals. Drinking
water that meets this standard is asso-
ciated with little to none of this risk
and is considered safe with respect to
EDB.
(40) Heptachlor. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that heptachlor is
a health concern at certain levels of
exposure. This organic chemical was
once a popular pesticide. When soil and
climatic conditions are favorable, hep-
tachlor may get into drinking water by
runoff into surface water or by leach-
ing into ground water. This chemical
has been shown to cause cancer in lab-
oratory animals such as rats and mice
when the animals are exposed at high
levels over their lifetimes. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time. EPA has set the
drinking water standards for hepta-
chlor at 0.0004 part per million (ppm) to
reduce the risk of cancer or other ad-
verse health effects which have been
observed in laboratory animals. Drink-
ing water that meets this standard is
associated with little to none of this
risk and is considered safe with respect
to heptachlor.
(41) Heptachlor epoxide. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that hep-
tachlor epoxide is a health concern at
certain levels of exposure. This organic
chemical was once a popular pesticide.
When soil and climatic conditions are
favorable, heptachlor expoxide may get
into drinking water by runoff into sur-
face water or by leaching into ground
water. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed o%rer long periods of
time. EPA has set the drinking water
standards for heptachlor epoxide at
0.0002 part per million (ppm) to reduce
the risk of cancer or other adverse
health effects which have been ob-
served in laboratory animals. Drinking
water that meets this standard is asso-
ciated with little to none of this risk
and is considered safe with respect to
heptachlor epoxide.
(42) Lindane. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that lindane is a health
concern at certain levels of exposure.
This organic chemical is used as a pes-
ticide. When soil and climatic condi-
tions are favorable, lindane may get
407
203-160 D-14
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§141.32
40 CFR Ch, I (7-1-04 Edition)
into drinking water by runoff into sur-
face water or by leaching into ground
water. This chemical has been ahown
to damage the liver, kidney, nervous
system, and immune system of labora-
tory animals such as rats, mice and
dogs exposed at high levels during their
lifetimes. Some humans who were ex-
posed to relatively large amounts of
this chemical also suffered damage to
the nervous system and circulatory
system. EPA has established the drink-
ing water standard for lindane at 0.0002
part per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to lindane.
(43) Methoxychlor. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that methoxychlor
is a health concern at certain levels of
exposure. This organic chemical is used
as a pesticide. When soil and climatic
conditions are favorable, methoxychlor
may get into drinking water by runoff
into surface water or by leaching into
ground water. This chemical has been
shown to damage the liver, kidney,
nervous system, and reproductive sys-
tem of laboratory animals such as rats
exposed at high levels during their life-
times. It has also been shown to
produce growth retardation in rats.
EPA has set the drinking water stand-
ard for methoxychlor at 0.04 part per
million (ppm) to protect against the
risk of these adverse health effects.
Drinking water that meets the EPA
standard is associated with little to
none of this risk and is considered safe
with respect to methoxychlor.
(44) Monochlorobemene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
monoehlorobenzene is a health concern
at certain levels of exposure. This or-
ganic chemical is used as a solvent. It
generally gets into water by improper
waste disposal. This chemical has been
shown to damage the liver, kidney and
nervous system of laboratory animals
such as rats and mice exposed to high
levels during their lifetimes. EPA has
set the drinking water standard for
monoehlorobenzene at 0.1 part per mil-
lion (ppm) to protect against the risk
of these adverse health effects. Drink-
ing water that meets the EPA standard
is associated with little to none of this
risk and is considered safe with respect
to monochlorobenzene.
(45) Poly chlorinated biphenyls (PCBs).
The United States Environmental Pro-
tection Agency (EPA) sets drinking
water standards and has determined
that polychlorinated biphenyls (PCBs)
are a health concern at certain levels
of exposure. These organic chemicals
were once widely used in electrical
transformers and other industrial
equipment. They generally get into
drinking water by improper waste dis-
posal or leaking electrical industrial
equipment. This chemical has been
shown to cause cancer in laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Chemicals that
cause cancer in laboratory animals
also may increase the risk of cancer in
humans who are exposed over long pe-
riods of time. EPA has set the drinking
water standard for PCBs at 0.0005 part
per million (ppm) to reduce the risk of
cancer or other adverse health effects
which have been observed in laboratory
animals. Drinking water that meets
this standard is associated with little
to none of this risk and is considered
- safe with respect to PCBs.
(46) Pentachlorophenol. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
pentachlorophenol is a health concern
at certain levels of exposure. This or-
ganic chemical is used as a wood pre-
servative, herbicide, disinfectant, and
defoliant. It generally gets into drink-
ing water by runoff into surface water
or leaching into ground water. This
chemical has been shown to produce
adverse reproductive effects and to
damage the liver and kidneys of lab-
oratory animals such as rats exposed
to high levels during their lifetimes.
Some humans who were exposed to rel-
atively large amounts of this chemical
also suffered damage to the liver and
kidneys. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed to hig-li levels over
their lifetimes. Chemicals that cause
408
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Environmental Protection Agency
§141.32
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed over long periods of
time. EPA has set the drinking water
standard for pentachlorophenol at 0.001
parts per million (ppm) to protect
against the risk of cancer or other ad-
verse health effects. Drinking water
that meets the EPA standard is associ-
ated with little to none of this risk and
is considered safe with respect to
pentachlorophenol.
(47) Styrene. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that styrene is a health
concern at certain levels of exposure.
This organic chemical is commonly
used to make plastics and is sometimes
a component of resins used for drinking
water treatment. Styrene may get into
drinking water from improper waste
disposal. This chemical has been shown
to damage the liver and nervous sys-
tem in laboratory animals when ex-
posed at high levels during their life-
times. EPA has set the drinking water
standard for styrene at 0.1 part per mil-
lion (ppm) to protect against the risk
of these adverse health effects, Drink-
ing water that meets the EPA standard
is associated with little to none of this
risk and is considered safe with respect
to styrene,
(48) Tetrachloroethylene. The United
States Environmental Protection
Agency (EPA) sets drinking: water
standards and has determined that
tetrachloroethylene is a health concern
at certain levels of exposure. This or-
ganic chemical has been a popular sol-
vent, particularly for dry cleaning. It,
generally gets into drinking water by
improper waste disposal. This chemical
has been shown to cause cancer in lab-
oratory animals such as rats and mice
when the animals are exposed at high
levels over their lifetimes. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time. EPA has set the
drinking water standard for
tetrachloroethylene at 0.005 part per
million (ppm) to reduce the risk of can-
cer or other adverse health effects
which have been observed in laboratory
animals. Drinking water that meets
this standard is associated with little
to none of this risk and is considered
safe with respect to
tetrachloroethylene.
(49) Toluene. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that toluene is a health
concern at certain levels of exposure.
This organic chemical is used as a sol-
vent and in the manufacture of gaso-
line for airplanes. It generally gets into
water by improper waste disposal or
leaking underground storage tanks.
This chemical has been shown to dam-
age the kidney, nervous system, and
circulatory system of laboratory ani-
mals such as rats and mice exposed to
high levels during their lifetimes.
Some industrial workers who were ex-
posed to relatively large amounts of
this chemical during- working' careers
also suffered damage to the liver, kid-
ney and nervous system. EPA has set
the drinking water standard for tol-
uene at 1 part per million (ppm) to pro-
tect against the risk of adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to toluene,
(50) Toxaphene. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that toxaphene is a
health concern at certain levels of ex-
posure. This organic chemical was once
a pesticide widely used on cotton, corn.
soybeans, pineapples and other crops.
When soil and climatic conditions are
favorable, toxaphene may get into
drinking water by runoff into surface
water or by leaching into ground
water. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed over long periods of
time. EPA has set the drinking water
standard for toxaphene at 0.003 part per
million (ppm) to reduce the risk of can-
cer or other adverse health effects
which have been observed in laboratory
animals. Drinking water that meets
this standard is associated with little
to none of this risk and is considered
safe with respect to toxaphene.
409
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§141.32
40 CFR Ch. I (7-1-04 Edition)
(51) 2,4,5-TP. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that 2,4,5-TP is a health
concern at certain levels of exposure.
This organic chemical is used as a her-
bicide. When soil and climatic condi-
tions are favorable, 2,4,5-TP may get
into drinking water by runoff into sur-
face water or by leaching into ground
water. This chemical has been shown
to damage the liver and kidney of lab-
oratory animals such as rats and dogs
exposed to high levels during their life-
times. Some industrial workers who
were exposed to relatively large
amounts of this chemical during work-
ing careers also suffered damage to the
nervous system. EPA has set the drink-
ing water standard for 2,4,5-TP at 0.05
part per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water that meets the
EPA standard is associated with little
to none of this risk and is considered
safe with respect to 2,4,5-TP.
(52) Xylenes. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that xylene is a health con-
cern at certain levels of exposure. This
organic chemical is used in the manu-
facture of g-asoline for airplanes and as
a solvent for pesticides, and as a clean-
er and degreaser of metals. It usually
gets into water by improper waste dis-
posal. This chemical has been shown to
damage the liver, kidney and nervous
system of laboratory animals such as
rats and dogs exposed to high levels
during their lifetimes. Some humans
who were exposed to relatively large
amounts of this chemical also suffered
damage to the nervous system. EPA
has set the drinking water standard for
xylene at 10 parts per million (ppm) to
protect against the risk of these ad-
verse health effects. Drinking water
that meets the BPA standard is associ-
ated with little to none of this risk and
is considered safe with respect to xy-
lene.
(53) Antimony. The United States En-
vironmental Protection Agency (EPA)
sets dilnking water standards and has
determined that antimony is a health
concern at certain levels of exposure.
This inorganic chemical occurs natu-
rally in soils, ground water and surface
waters and is often used in the flame
retardant industry. It is also used in
ceramics, glass, batteries, fireworks
and explosives. It may get into drink-
ing water through natural weathering
of rock, industrial production, munic-
ipal waste disposal or manufacturing
processes. This chemical has been
shown to decrease longevity, and al-
tered blood levels of cholesterol and
glucose in laboratory animals such as
rats exposed to high levels during" their
lifetimes. EPA has set the drinking
water standard for antimony at 0.006
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to anti-
mony.
(54) Beryllium, The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that beryllium is a health
concern at certain levels of exposure.
This inorganic metal occurs naturally
in soils, ground water and surface wa-
ters and is often used in electrical
equipment and electrical components.
It generally gets into water from run-
off from mining operations, discharge
from processing plants and improper
waste disposal. Beryllium compounds
have been associated with damage to
the bones and lungs and induction of
cancer in laboratory animals such as
rats and mice when the animals are ex-
posed at high levels over their life-
times. There is limited evidence to sug-
gest that beryllium may pose a cancer
risk via drinking water exposure.
Therefore, EPA based the health as-
sessment on noncancer effects with an
extra uncertainty factor to account for
possible carcinogenic! ty. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time. EPA has set the
drinking water standard for beryllium
at 0.004 part per million (ppm) to pro-
tect against the risk of these adverse
health effects. Drinking water which
meets the EPA standard is associated
with little to none of this risk and
should be considered safe with respect
to beryllium.
410
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Environmental Protection Agency
§141.32
(55) Cyanide. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that cyanide is a health
concern at certain levels of exposure.
This inorganic chemical is used in elec-
troplating, steel processing, plastics,
synthetic fabrics and fertilizer prod-
ucts. It usually gets into water as a re-
sult of improper waste disposal. This
chemical has been shown to damage
the spleen, brain and liver of humans
fatally poisoned with cyanide, EPA has
set the drinking water standard for cy-
anide at 0,2 parts per million (ppm) to
protect against the risk of these ad-
verse health effects. Drinking water
which meets the EPA standard is asso-
ciated with little to none of this risk
and should be considered safe with re-
spect to cyanide.
(56) [Reserved]
(57) Thallium. The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that thallium is a health
concern at certain high levels of expo-
sure. This inorganic metal is found
naturally in soils and is used in elec-
tronics, Pharmaceuticals, and the man-
ufacture of glass and alloys. This
chemical has been shown to damage
the kidney, liver, brain and Intestines
of laboratory animals when the ani-
mals are exposed at high levels over
their lifetimes. EPA has set the drink-
ing water standard for thallium at 0.002
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to thal-
lium.
(58) Bemola]pyrenc. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
benzo[a]pyrene is a health concern at
certain levels of exposure. Cigarette
smoke and charbroiled meats are com-
mon source of general exposure. The
major source of benzo[a]pyrene in
drinking water is the leaching from
coal tar lining and sealants in water
storage tanks. This chemical has been
shown to cause cancer in animals such
as rats and mice when the animals are
exposed at high levels. EPA has set the
drinking water standard for
benzo[a]pyrene at 0.0002 parts per mil-
lion (ppm) to protect against the risk
of cancer. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to
benzo[a]pyrene.
(59) Dalapon, The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that dalapon is a health
concern at certain levels of exposure.
This organic chemical is a widely used
herbicide. It may get into drinking
water after application to control
grasses in crops, drainage ditches and
along railroads. This chemical has been
shown to cause damage to the kidney
and liver in laboratory animals when
the animals are exposed to high levels
over their lifetimes, EPA has set the
drinking water standard for dalapon at
0.2 parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to
dalapon.
(60) Dichloromethane. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
dichloromethane (methylene chloride)
is a health concern at certain levels of
exposure. This organic chemical is a
widely used solvent. It is used in the
manufacture of paint remover, as a
metal degreaser and as an aerosol pro-
pellant. It generally gets into drinking"
water after improper discharge of
waste disposal. This chemical has been
shown to cause cancer in laboratory
animals such as rats and mice when
the animals are exposed at high levels
over their lifetimes. Chemicals that
cause cancer in laboratory animals
also may increase the risk of cancer in
humans who are exposed over long pe-
riods of time. EPA has set the drinking
water standard for dichloromethane at
0.005 parts per million (ppm) to reduce
the risk of cancer or other adverse
health effects which have been ob-
served in laboratory animals. Drinking
water which meets this standard is as-
sociated with little to none of this risk
411
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§141.32
40 CFR Ch, I (7-1-04 Edition)
and should be considered safe with re-
spect to dichlorometliane.
(81) Di (2-ethylhexyl)adipate. The
United States Environmental Protec-
tion Agency (EPA) sets drinking water
standards and has determined that
di(2-ethylhexyl)adipate is a health con-
cern at certain levels of exposure. Di(2-
ethylhexyDadipate is a widely used
plasticizer in a variety of products, in-
cluding synthetic rubber, food pack-
aging materials and cosmetics. It may
get into drinking water after improper
waste disposal. This chemical has been
shown to damage liver and testes in
laboratory animals such as rats and
mice exposed to high levels. EPA has
set the drinking water standard for
di(2-ethylhexyl)adipate at 0.4 parts per
million (ppm) to protect against the
risk of adverse health effects. Drinking
water which meets the EPA standards
is associated with little to none of this
risk and should be considered safe with
respect to di(2-ethylhexyl)adipate.
(62) Di(2-ethylhexyl)phthalate. The
United States Environmental Protec-
tion Agency (EPA) sets drinking- water
standards and has determined that
di(2-ethylhexyl)phthalate is a health
concern at certain levels of exposure.
Di(2-ethylhexyl)phthalate is a widely
used plasticizer, which is primarily
used in the production of polyvinyl
chloride (PVO) resins. It may get into
drinking water after improper waste
disposal. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice exposed to high
levels over their lifetimes. EPA has set
the drinking water standard for di(2-
ethylhexyDphthalate at 0.008 parts per
million (ppm) to reduce the risk of can-
cer or other adverse health effects
which have been observed in laboratory
animals. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to di(2-
ethylhexyl)phthalate.
(63) Dinoseb. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that dinoseb is a health
concern at certain levels of exposure.
Dinoseb is a widely used pesticide and
generally gets into drinking water
after application on orchards, vine-
yards and other crops. This chemical
has been shown to damage the thyroid
and reproductive organs in laboratory
animals such as rats exposed to high
levels. EPA has set the drinking1 water
standard for dinoseb at 0.007 parts per
million (ppm) to protect against the
risk of adverse health effects. Drinking
water which meets the EPA standard is
associated with little to none of this
risk and should be considered safe with
respect to dinoseb.
(64) Diquat. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that diquat is a health con-
cern at certain levels of exposure. This
organic chemical is a herbicide used to
control terrestrial and aquatic weeds.
It may get into drinking water by run-
off into surface water. This chemical
has been shown to damage the liver,
kidney and gastrointestinal tract and
causes cataract formation in labora-
tory animals such as dogs and rats ex-
posed at high levels over their life-
times. EPA has set the drinking water
standard for diquat at 0.02 parts per
million (ppm) to protect against the
risk of these adverse health effects.
Drinking- water which meets the EPA
standard is associated with little to
none of this risk and should be consid-
ered safe with respect to diquat.
(65) Endothall. The United States En-
vironmental Protection Agency (EPA)
has determined that endothall is a
health concern at certain levels of ex-
posure. This organic chemical is a her-
bicide used to control terrestrial and
aquatic weeds. It may get into water
by runoff into surface water. This
chemical has been shown to damage
the liver, kidney, gastrointestinal
tract and reproductive system of lab-
oratory animals such as rats and mice
exposed at high levels over their life-
times, EPA has set the drinking water
standard for endothall at 0.1 parts per
million (pprn) to protect against the
risk of these adverse health effects.
Drinking water which meets the EPA
standard is associated with little to
none of this risk and should be consid-
ered safe with respect to endothall.
(68) Endrin. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that endrin is a health con-
cern at certain levels of exposure. This
412
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Environmental Protection Agency
§141.32
organic chemical is a pesticide no
longer registered for use in the United
States. However, this chemical is per-
sistent in treated soils and accumu-
lates in sediments and aquatic and ter-
restrial biota. This chemical has been
shown to cause damage to the liver,
kidney and heart in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. EPA has set the drink-
ing water standard for endrin at 0.002
parts per million (ppm) to protect
against the risk of these adverse health.
effects which have been observed in
laboratory animals. Drinking water
that meets the EPA standard is associ-
ated with little to none of this risk and
should be considered safe with respect
to endrin.
(67) Glyphosate. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that glyphosate is
a health concern at certain levels of
exposure. This organic chemical is a
herbicide used to control grasses and
weeds. It may get into drinking water
by runoff into surface water. This
chemical has been shown to cause dam-
age to the liver and kidneys in labora-
tory animals such as rats and mice
when the animals are exposed at high
levels over their lifetimes. EPA has set
the drinking water standard for
glyphosate at 0.7 parts per million
(ppm) to protect against the risk of
these adverse health effects. Drinking
water which meets the EPA standard is
associated with little to none of this
risk and should "be considered safe with
respect to glyphosate.
(68) Hexachlorobenzene, The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
hexachlorobenzene Is a health concern
at certain levels of exposure. This or-
ganic chemical is produced as an impu-
rity in the manufacture of certain sol-
vents and pesticides. This chemical has
been shown to cause cancer in labora-
tory animals such as rats and mice
when the animals are exposed to high
levels during their lifetimes. Chemicals
that cause cancer in laboratory ani-
mals also may increase the risk of can-
cer in humans who are exposed over
long periods of time, EPA has set the
drinking water standard for
hexachlorobenzene at 0.001 parts per
million (ppm) to protect against the
risk of cancer and other adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to
hexachlorobenzene.
(69) Hexachlorocyclopentadiene. The
United States Environmental Protec-
tion Agency (EPA) establishes drinking
water standards and has determined
that hexachlorocyclopentadiene is a
health concern at certain levels of ex-
posure. This organic chemical is uaed
as an intermediate in the manufacture
of pesticides and flame retardants. It
may get into water by discharge from
production facilities. This chemical
has been shown to damage the kidney
and the stomach of laboratory animals
when exposed at high levels over their
lifetimes. EPA has set the drinking
water standard for
hexachlorocyclopentadiene at 0.05
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to
hexachlorocyclopentadiene.
(70) Oxamyl. The United States Envi-
ronmental Protection Agency (EPA)
establishes drinking water standards
and has determined that oxarnyl is a
health concern at certain levels of ex-
posure. This organic chemical is used
as a pesticide for the control of insects
and other pests. It may get into drink-
ing water by runoff into surface water
or leaching into ground water. This
chemical has been shown to damage
the kidneys of laboratory animals such
as rats when exposed at high levels
over their lifetimes. EPA has set the
drinking water standard for oxamyl at
0.2 parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to oxamyl.
(71) Picloram. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that picloram is a health
concern at certain levels of exposure.
413
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§141.32
40 CFR Ch. I (7-1-04 Edition)
This organic chemical is used as a pes-
ticide for broadleaf weed control. It
may get into drinking water by runoff
into surface water or leaching into
ground water as a result of pesticide
application and improper waste dis-
posal. This chemical has been shown to
cause damage to the kidneys and liver
in laboratory animals such as rats
when the animals are exposed at high
levels over their lifetimes, EPA has set
the drinking water standard for
picloram at 0.5 parts per million (ppm)
to protect against the risk of these ad-
verse health effects. Drinking water
which meets the EPA standard is asso-
ciated with little to none of this risk
and should be considered safe with re-
spect to picloram.
(72) Simazine. The United States En-
vironmental Protection Agency (EPA)
sets drinking water standards and has
determined that simazine is a health
concern at certain levels of exposure.
This organic chemical is a herbicide
used to control annual grasses and
broadleaf weeds. It may leach into
ground water or runs off into surface
water after application. This chemical
may cause cancer in laboratory ani-
mals such as rats and mice exposed at
high levels during their lifetimes.
Chemicals that cause cancer in labora-
tory animals also may increase the
risk of cancer in humans who are ex-
posed over long periods of time. EPA
has set the drinking water standard for
simazine at 0.004 parts per million
(ppm) to reduce the risk of cancer or
other adverse health effects. Drinking
water which meets the EPA standard is
associated with little to none of this
risk and should be considered safe with
respect to simazine.
(73) 1,2,4-Trichlorobemene. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
1,2,4-trichlorobenzene is a health con-
cern at certain levels of exposure. This
organic chemical is used as a dye car-
rier and as a precursor in herbicide
manufacture. It generally gets into
drinking water by discharges from in-
dustrial activities. This chemical has
been shown to cause damage to several
organs, including the adrenal glands.
EPA has set the drinking water stand-
ard for 1,2.4-trichlorobenzene at 0.07
parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to 1,2,4-
trichlorobenzene.
(74) 1,1,2-Trichloroethane, The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined 1,1,2-tri-
chloroethane is a health concern at
certain levels of exposure. This organic
chemical is an intermediate in the pro-
duction of 1,1-dichloroethylene. It gen-
erally gets into water by industrial dis-
charge of wastes. This chemical has
been shown to damage the kidney and
liver of laboratory animals such as rats
exposed to high levels during their life-
times. EPA has set the drinking water
standard for 1,1,2-trichloroethane at
0.005 parts per million (ppm) to protect
against the risk of these adverse health
effects. Drinking water which meets
the EPA standard is associated with
little to none of this risk and should be
considered safe with respect to 1,1,2-tri-
chloroethane.
(75) 2,3,7,8-TCDD (Dioxin). The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
dioxin is a health concern at certain
levels of exposure. This organic chem-
ical is an impurity in the production of
some pesticides. It may get into drink-
ing water by industrial discharge of
wastes. This chemical has been shown
to cause cancer in laboratory animals
such as rats and mice when the ani-
mals are exposed at high levels over
their lifetimes. Chemicals that cause
cancer in laboratory animals also may
increase the risk of cancer in humans
who are exposed over long periods of
time. EPA has set the drinking water
standard for dioxin at 0.00000003 parts
per million (ppm) to reduce the risk of
cancer or other adverse health effects
which have been observed in laboratory
animals. Drinking water which meets
this standard is associated with little
to none of this risk and should be con-
sidered safe with respect to dioxin.
(76) Chlorine. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that chlorine is a health
414
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Environmental Protection Agency
§141.32
concern at certain levels of exposure.
Chlorine is added to drinking water as
a disinfectant to kill bacteria and
other disease-causing microorganisms
and is also added to provide continuous
disinfection throughout the distribu-
tion system. Disinfection is required
for surface water systems. However, at
high doses for extended periods of time,
chlorine has been shown to affect blood
and the liver in laboratory animals.
EPA has set a drinking water standard
for chlorine to protect against the risk
of these adverse effects. Drinking
water which meets this EPA standard
is associated with little to none of this
risk and should be considered safe with
respect to chlorine.
(77) Chloramines. The United States
Environmental Protection Agency
(EPA) sets drinking water standards
and has determined that chloramines
are a health concern at certain levels
of exposure. Chloramines are added to
drinking water as a disinfectant to kill
bacteria and other disease-causing'
microorganisms and are also added to
provide continuous disinfection
throughout the distribution system.
Disinfection is required for surface
water systems. However, at high doses
for extended periods of time,
chloramines have been shown to affect
blood and the liver in laboratory ani-
mals. EPA has set a drinking water
standard for chloramines to protect
against the risk of these adverse ef-
fects. Drinking water which meets this
EPA standard is associated with little
to none of this risk and should be con-
sidered safe with respect to
chloramines.
(78) Chlorine dioxide. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and has determined that
chlorine dioxide is a health concern at
certain levels of exposure. Chlorine di-
oxide is used in water treatment to kill
bacteria and other disease-causing
microorganisms and can be used to
control tastes and odors. Disinfection
is required for surface water systems.
However, at high doses, chlorine diox-
ide-treated drinking water has been
shown to affect blood in laboratory
animals. Also, high levels of chlorine
dioxide given to laboratory animals in
drinking water have been shown to
cause neurological effects on the devel-
oping nervous system. These
neurodevelopmental effects may occur
as a result of a short-term excessive
chlorine dioxide exposure. To protect
against such potentially harmful expo-
sures. EPA requires chlorine dioxide
monitoring at the treatment plant,
where disinfection occurs, and at rep-
resentative points in the distribution
system serving water users. EPA has
set a drinking water standard for chlo-
rine dioxide to protect against the risk
of these adverse effects.
NOTE: In addition to the language in this
introductory text of paragraph (e)(78). sys-
tems must include either the language in
paragraph (e)(78Xi) or (e)(78)(ii> of Uiis sec-
tion. Systems with a violation at the treat-
ment plant, hut not in the distribution sys-
tem, are required to use the language in
paragraph (eK78)tl) of this section and treat
the violation as a nonacute violation. Sys-
tems with a violation in the distribution sys-
tem are required to use the language in para-
graph (e)(78)(ii) of this section and treat the
violation as an acute violation.
(i) The chlorine dioxide violations re-
ported today are the result of
exceedances at the treatment facility
only, and do not include violations
within the distribution system serving
users of this water supply. Continued
compliance with chlorine dioxide levels
within the distribution system mini-
mizes the potential risk of these viola-
tions to present consumers.
(it) The chlorine dioxide violations
reported today include exceedances of
the EPA standard within the distribu-
tion system serving water users. Viola-
tions of the chlorine dioxide standard
within the distribution system may
harm human health based on short-
term exposures. Certain groups, includ-
ing pregnant women, infants, and
young children, may be especially sus-
ceptible to adverse effects of excessive
exposure to chlorine dioxide-treated
water. The purpose of this notice is to
advise that such persons should con-
sider reducing their risk of adverse ef-
fects from these chlorine dioxide viola-
tions by seeking alternate sources of
water for human consumption until
such exceedances are rectified. Local
and State health authorities are the
best sources for information con-
cerning alternate drinking water.
415
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§141,33
40 CFR Ch, I (7-1-04 Edition)
(19) Disinfection byproducts and treat-
ment technique for DBFs. The United
States Environmental Protection
Agency (EPA) sets drinking water
standards and requires the disinfection
of drinking water. However, when used
in the treatment of drinking water,
disinfectants react with naturally-oc-
curring organic and inorganic matter
present in water to form chemicals
called disinfection byproducts (DBFs).
EPA has determined that a number of
DBFs are a health concern at certain
levels of exposure. Certain DBFs, in-
cluding some trihalomethanes (THMs)
and some haloacetic acids (HAAs), have
been shown to cause cancer in labora-
tory animals. Other DBFs have been
shown to affect the liver and the nerv-
ous system, and cause reproductive or
developmental effects in laboratory
animals. Exposure to certain DBFs
may produce similar effects in people.
EPA has set standards to limit expo-
sure to THMs. HAAs, and other DBFs.
(80) Bromate. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking' water standards and has
determined that bromate is a health
concern at certain levels of exposure.
Bromate is formed as a byproduct of
ozone disinfection of drinking water.
Ozone reacts with naturally occurring
bromide in the water to form bromate.
Bromate has been shown to produce
cancer in rats. EPA has set a drinking
water standard to limit exposure to
"bromate.
(81) Chlorite. The United States Envi-
ronmental Protection Agency (EPA)
sets drinking water standards and has
determined that chlorite is a health
concern at certain levels of exposure.
Chlorite is formed from the breakdown
of chlorine dioxide, a drinking water
disinfectant. Chlorite in drinking
water has been shown to affect blood
and the developing nervous system.
EPA has set a drinking water standard
for chlorite to protect against these ef-
fects. Drinking water which meets this
standard is associated with little to
none of these risks and should be con-
sidered safe with respect to chlorite.
(f) Public notices for fluoride. Notice of
violations of the maximum contami-
nant level for fluoride, notices of
variances and exemptions from the
maximum contaminant level for fluo-
ride, and notices of failure to comply
with variance and exemption schedules
for the maximum contaminant level
for fluoride shall consist of the public
notice prescribed in § 143.5(b), plus a de-
scription of any steps which the system
is taking to come into compliance.
(g) Public notification by the State. The
State may give notice to the public re-
quired by this section on behalf of the
owner or operator of the public water
system if the State complies with the
requirements of this section. However,
the owner or operator of the public
water system remains legally respon-
sible for ensuring that the require-
ments of this section are met.
[52 FB 41546, Oct. 28, 1987, as amended at 54
PR 15188, Apr. 17, 1989; 54 FR 27527, 27566,
June 29, 1989; 55 FR Jane 19, 1990: 56 FB
3587, Jan. 30, 1991; 56 FR 26548. June 7, 1991; 56
FB 30279, July 1, 1991; 57 FR 31843, July 17,
1992; 59 FR 34323, July 1, 1994; 60 FR 33932,
June 29, 1995; 63 FR 69464. 69515, Dec. 16, 1998;
65 FR 26022, May 4, 2000J
§ 141,33 Record maintenance.
Any owner or operator of a public
water system subject to the provisions
of this part shall retain on its premises
or at a convenient location near its
premises the following records:
(a) Records of bacteriological anal-
yses made pursuant to this part shall
be kept for not less than 5 years.
Records of chemical analyses made
pursuant to this part shall be kept for
not less than 10 years. Actual labora-
tory reports may tie kept, or data may
be transferred to tabular summaries,
provided that the following1 informa-
tion is included:
(1) The date, place, and time of sam-
pling, and the name of the person who
collected the sample;
(2) Identification of the sample as to
whether it was a routine distribution
system sample, check sample, raw or
process water sample or other special
purpose sample;
(3) Date of analysis;
(4) Laboratory and person responsible
for performing analysis;
(5) The analytical technique/method
used: and
(6) The results of the analysis.
(b) Records of action taken by the
system to correct violations of primary
drinking water regulations shall be
kept for a period not less than 3 years
416
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Environmental Protection Agency
§141.35
after the last action taken with respect
to the particular violation involved.
(c) Copies of any written reports,
summaries or communications relating
to sanitary surveys of the system con-
ducted by the system itself, by a pri-
vate consultant, or by any local, State
or Federal agency, shall be kept for a
period not less than 10 years after com-
pletion of the sanitary survey involved.
(d) Records concerning a variance or
exemption granted to the system shall
be kept for a period ending not less
than 5 years following the expiration of
such variance or exemption.
(e) Copies of public notices issued
pursuant to Subpart Q of this part and
certifications made to the primacy
agency pursuant to §141.31 must be
kept for three years after issuance.
[40 FR 59570, Dec. 24. 1975, as amended at 65
FR 26022, May 4, 2000]
§ 141.34 [Reserved]
S 141.35 Reporting of unregulated con-
taminant monitoring results.
(a) Does this reporting apply to me? (1)
This section applies to any owner or
operator of a public water system re-
quired to monitor for unregulated con-
taminants under §141.40. This section
requires you to report the results of
this monitoring.
(2) Exception. You do not need to re-
port results if you are a system serving
a population of 10,000 or less, since EPA
will arrange for testing and reporting
of the results. However, you will still
need to comply with consumer con-
fidence reporting and public notifica-
tion requirements for these results.
(bl To whom must I report? You must
report the results of unregulated con-
taminant monitoring to EPA and pro-
vide a copy to the State. You must also
notify the public of the monitoring re-
sults as provided in Subpart O (Con-
sumer Confidence Reports) and Subpart
Q (Public Notification) of this part.
(c) When must I report monitoring re-
sults? You must report the results of
unregulated contaminant monitoring
within thirty (30) days following the
month in which you received the re-
sults from the laboratory. EPA will
conduct its quality control review of
the data for sixty (60) days after you
report the data, which will also allow
for quality control review by systems
and States. After the quality control
review, EPA will place the data in the
national drinking water contaminant
occurrence database at the time of the
next database update. Exception: Re-
porting to EPA of monitoring results
received by public water systems prior
to May 13. 2002. must occur by August
9, 2002.
(d) What information must 1 report? (1)
You must provide the following "point
of contact" information: name, mailing
address, phone number, and e-mail ad-
dress for:
(i) PWS Technical Contact, the per-
son at your PWS that is responsible for
the technical aspects of your unregu-
lated contaminant monitoring regula-
tion (UCMR) activities, such as details
concerning sampling and reporting:
(ii) PWS Official, the person at your
PWS that is able to function as the of-
ficial spokesperson for your UCMR ac-
tivities: and
(ill) Laboratory Contact Person, the
person at your laboratory that is able
to address questions concerning the
analysis that they provided for you.
(2) You must update this information
if it changes during the course of
UCMR implementation.
(3) You must report the information
specified for data elements 1 through 16
in the following table for each sample.
TABLE 1—UNREGULATED CONTAMINANT MONITORING REPORTING REQUIREMENTS
Data Element
1. Public Water System (PWS) Identifica-
tion Number.
Definition
The code used to identify each PWS. The code begins with the standard two-char-
acter postal State abbreviation; the remaining seven characters are unique to
each PWS.
2. Public Water System Facility Identifica- ! The Sampling point identification number and sampling point type identification
tion Number—Sampling Point Identifica- j must either be static or Iraceabie to previous numbers and type identifications
tion Number and Sampling Point Type throughout the period of unregulated contaminant monitoring. The Sampling
Identification. point identification number is a three-part alphanumeric designation, made up of:
417
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§141.35
40 CFR Ch. I (7-1-04 Edition)
TABLE 1—UNREGULATED CONTAMINANT MONITORING REPORTING REQUIREMENTS—Continued
Data Element
3, Sample Collection Dale ,....
4, Sample identification Number .....
5. Contaminant/Parameter
6, Analytical Results—Sign
7. Analytical Resuft—Value .............
8, Analytical Result—Unit of Measure
9. Analytical Method Number .,.,.....,.....
10. Sample Analysis Type
11, Sample Batch Identification Number
12. Minimum Reporting Level ,
13. Minimum Reporting Level Unit of
Measure.
14, Analytical Precision
a. The Public Water System Facility identification Number is an identification num-
ber established by the State, or at the State's discretion the PWS, that is unique
to the PWS for an intake for each source of water, a treatment plant, a distribu-
tion system, or any other facility associated with water treatment or delivery and
provides for the relationship of facilities to each other to be maintained;
b, The Sampling Point Identification Number is an identification number established
by the State, or at the State's discretion the PWS, that is unique to each PWS
facility that identifies the specific sampling point and allows the relationship of
the sampling point to other facilities to be maintained; and
c. Sampling Point Type Identification is one of following:
Spj:—Untreated water collected at the source of the water system facility.
EP—Entry point to the distribution system,
MD—midpoint in the distribution system where the disinfectant residua! would be
expected to be typical for the system such as the location for sampling coliform
indicator bacteria as described in 40 CFR 141.21.
MR—point of maximum retention is the point located the furthest from the entry
point to the distribution system which is approved by the State for trihalomethane
(THM) (disinfectant byproducts (DBPJ) and/or total coliform sampling.
LD~—location in the distribution system where the disinfectant residual is the lowest
which is approved by the State for THM (DBF) and/or total coliform sampling.
The date the sample is collected reported as 4-digit year, 2-digit month, and 2-digtt
day.
An alphanumeric va?ue of up to 15 characters assigned by the laboratory to
uniquely identify containers or groups of containers containing water samples
collected at the same time and sampling point.
The unregulated contaminant or water quality parameter for which the sample is
being analyzed.
An alphanumeric value indicating whether the sample analysis result was:
a, {<) "'less than'' means the contaminant was not detected or was detected at a
level "less than" the MRL
b (as) "equal to" means the contaminant was detected at a level "equal to" the
value reported in "Analytical Result—Value.''
The actual numeric value of the analysis for chemical and microbiological results,
or the minimum reporting level (MRL) if the analytical result is less than the con-
taminant's MRL,
j The unit of measurement for the analytical results reported, [e.g., micrograms per
i liter, ffig/L); colony-forming units per 100 milliiiters, (CFU/100 mL), etc.]
The identification number of the analytical method used.
The type of sample collected. Permitted values include;
: a. RFS—Raw field sample—untreated samole collected and submitted for analysis
; under this ruie.
] b. ROS—Raw duplicate field sample—untreated lietd sample duplicate collected at
the same time and place as the raw field sample and submitted for analysis
under this rule.
c. TFS—Treated field sample-—treated sample collected and submitted for analysis
under this rule.
d. TDS-—Treated duplicate field sample—treated field sample duplicate collected at
the same time and place as the treated field sample and submitted for analysis
under this rule.
The sample batch identification number consists of three parts:
a. Up to a 10-character laboratory identification code assigned by EPA.
b. Up to a 15-character code assigned by the laboratory to uniquely identify each
extraction or analysis batch.
c. The date that the samples contained in each extraction batch extracted or in an
analysis batch were analyzed, reported as an 8-digrt number in the form 4-digit
year, 2-digit monih, and 2-digit day.
Minimum Reporting Level (MRL) refers to the lowest concentration of an anaiyte
that may be reported. Unregulated contaminant monitoring (UCM) MRLs are es-
tablished in §141.40 monitoring requirements for unregulated contaminants.
The unit of measure to express the concentration, count, or other value of a con-
taminant level for the Minimum Reporting Level reported, (e.g., jig/L, colony
forming units/100 mL (CFU/100 mL), etc.).
Precision is the degree of agreement between two repeated measurements and is
monitored through the use of duplicate spiked samples. For purposes of the Un-
regulated Contaminant Monitoring Regulation (UCMRj, Analytical Precision is
defined as the relative percent difference (RPD) between spiked matrix dupli-
cates. The RPD for the spiked matrix duplicates analyzed in the same batch of
samples as the analytical result being reported is to be entered in this field. Pre-
cision is calculated as Relative Percent Difference (RPD) of spiked matrix dupli-
cates from the mean using:
RPD = absolute value of f(X>—X,} /(X, i-Xj}/2 ] x 100%,
'< where:
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Environmental Protection Agency
§141.40
TABLE 1—UNREGULATED CONTAMINANT MONITORING REPORTING REQUIREMENTS—Continued
Data Element
Definition
15. Analytical Accuracy
16. Spiking Concentration
17. Presence/Absence
Xi is the concentration observed in spiked field sample minus the concentration
observed in unspiked field sample.
Xi is the concentration observed in duplicate spiked field sample minus the con-
centration observed in unspiked field sample.
Accuracy describes how close a result is to the true value measured through the
use of spiked field samples. For purposes of unregulated contaminant moni-
toring, accuracy is defined as the percent recovery of the contaminant in the
spiked matrix sample analyzed in the same analytical batch as the sample result
being reported and calculated using:
% recovery = [(amt. found in spiked sample—amt. found in sample)/amt. spiked] x
100%.
The concentration of method analyte(s) added to a sample to be analyzed for cal-
culating analytical precision and accuracy where the value reported use the
same unit of measure reported for Analytical Results.
Reserved.
(e) How must I report this information?
(1) You must report results from moni-
toring under this rule using EPA's
electronic reporting system. For qual-
ity control purposes, you must instruct
the organization(s) responsible for the
analysis of unregulated contaminant
samples taken under §141.40 to enter
the results into the reporting system,
in the format specified by EPA. You
are responsible for reviewing those re-
sults and approving the reporting (via
the electronic system) of the results to
EPA. You must also provide a copy of
the results to the State, as directed by
the State.
(2) If you report more than one set of
valid results for the same sampling
point and the same sampling event (for
example, because you have had more
than one organization (e.g., a labora-
tory* analyze replicate samples col-
lected under §141.40, or because you
have collected multiple samples during
a single monitoring event at the same
sampling point), EPA will use the high-
est of the reported values as the offi-
cial result.
(f) Does the laboratory to which I send
samples report the results for me? While
you must instruct the organization
conducting unregulated contaminant
analysis (e.g., a laboratory) to enter
the results into EPA's electronic re-
porting system, you are responsible for
reviewing and approving the submis-
sion of the results to EPA. If the ana-
lytical organization or laboratory can-
not enter these data for you using
EPA's electronic reporting system,
then you may explain to EPA in writ-
ing the reasons why alternate report-
ing is necessary and must receive
EPA's approval to use an alternate re-
porting procedure.
(g) Can I report previously collected
data to meet the testing and reporting re-
quirements for the contaminants listed in
§ 141.40(a)(3)? Yes, as long as the data
meet the specific requirements of
§141.40(a)(3), (4), (5), and Appendix A of
§ 141.40 and you report the data with
the information specified in paragraph
(d) of this section.
[64 FR 50611, Sept. 17, 1999, as amended at 66
FR 2300, Jan. 11, 2001; 66 FR 27215. May 16.
2001; 67 FR 11046, Mar. 12, 2002]
Subpart E—Special Regulations,
Including Monitoring Regula-
tions and Prohibition on Lead
Use
§ 141.40 Monitoring requirements for
unregulated contaminants.
(a) Requirements for owners and opera-
tors of public water systems. (1) Do I have
to monitor for unregulated contaminants?
(i) Transient systems. If you own or op-
erate a transient non-community
water system, you do not have to mon-
itor for unregulated contaminants.
(ii) Large systems not purchasing their
entire water supply from another system.
If you own or operate a wholesale or re-
tail public water system (other than a
transient system) that serves more
than 10,000 persons, as determined by
the State, and do not purchase your en-
tire water supply from another public
water system, you must monitor as fol-
lows:
419
-------
§141.40
40CFRCh. I (7-1-04 Edition)
(A) You must monitor for the un-
regulated contaminants on List 1 of
Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section.
(B) You must monitor for the unregu-
lated contaminants on List 2 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, if notified
by your State or EPA that you are part
of the Screening Surveys.
(C) You must monitor for the unregu-
lated contaminants on List 3 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, if notified
by your State or EPA that you are part
of the Pre-Screen Testing.
(iii) Large systems purchasing their en-
tire water supply from another system. If
you own or operate a public water sys-
tem (other than a transient system)
that serves more than 10,000 persons
and purchase your entire water supply
from a wholesale or retail public water
system, you must monitor as follows:
(A) You must monitor for the un-
regulated contaminants on List 1 of
Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section, that
have a "sampling location" indicated as
"distribution system".
(B) You must monitor for the unregu-
lated contaminants on List 2 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, that have a
"sampling location" indicated as "dis-
tribution system" if notified by your
State or EPA that you are part of the
Screening Surveys.
(C) You must monitor for the unregu-
lated contaminants on List 3 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, that have a
"sampling location" indicated as "dis-
tribution system" if notified by your
State or EPA that you are part of the
Pre-Screen Testing.
(iv) Small systems not purchasing their
entire water supply from another system.
If you own or operate a public water
system (other than a transient system)
that serves 10,000 or fewer persons and
do not purchase your entire water sup-
ply from another public water system,
you must monitor as follows:
(A) You must monitor for the un-
regulated contaminants on List 1 of
Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section, if you
are notified by your State or EPA that
you are part of the State Monitoring
Plan for small systems.
(B) You must monitor for the unregu-
lated contaminants on List 2 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, if you are
notified by your State or EPA that you
are part of the Screening Surveys.
(C) You must monitor for the unregu-
lated contaminants on List 3 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of tins section, if you are
notified by your State or EPA that you
are part of the Pre-Screen Testing.
(v) Small systems purchasing their en-
tire water supply from another system. If
you own or operate a public water sys-
tem (other than a transient system)
that serves 10,000 or fewer persons and
purchase your entire water supply from
another public water system, you must
monitor as follows:
(A) You must monitor for the un-
regulated contaminants on List 1 of
Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section, that
have a "sampling location" indicated as
"distribution system" if you are noti-
fied by your State or EPA that you are
part of the State Monitoring Plan for
small systems.
(B) You must monitor for the unregu-
lated contaminants on List 2 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, that have a
"sampling location" indicated as "dis-
tribution system" if you are notified by
your State or EPA that you are part of
the Screening Surveys.
(C) You must monitor for the unregu-
lated contaminants on List 3 of Table
1, Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section, that have a
"sampling location" indicated as "dis-
tribution system" if you are notified by
420
-------
Environmental Protection Agency
§141.40
your State or EPA that you are part of
the Pre-Screen Testing.
(2) How would 1 be selected for the. mon-
itoring under the State Monitoring Plan,
the Screening Surveys, or the Pre-Screen
Testing? (i) State Monitoring Plan.
Only a representative sample of small
systems must monitor for unregulated
contaminants. EPA will select a na-
tional representative sample of small
public water systems in each State
through the use of a random number
generator. Selection will be weighted
by population served within each sys-
tem water source type (surface or
ground water) and system size category
(systems serving 25-500, 501-3,300, and
3,301-10,000 persons). EPA may allocate
additional systems to water source
types or system size categories to in-
crease the statistical inferential abil-
ity for those categories. EPA will also
select a small group of systems to be
"Index systems." Systems selected as
Index systems are required to provide
information about their site and oper-
ation that will serve to allow extrapo-
lation of their results to other systems
of similar size, rather than collecting
detailed information at every small
system. Each State will have the op-
portunity to make some modifications
to the list of small systems that EPA
selects. You will be notified by the
State or EPA if your system is part of
the final State Monitoring Plan.
(ii) Screening Surveys. The purpose of
the Screening Surveys is to determine
the occurrence of contaminants in
drinking water or sources of drinking
water for which analytical methods
have recently been developed for un-
regulated contaminant monitoring.
EPA will select up to 300 systems to
participate in each survey by using a
random number generator. You will be
notified by the State or EPA if your
system is selected for monitoring
under the Screening Surveys.
(iii) Pre-screen Testing. The purpose of
Pre-Screen Testing is to determine the
occurrence of contaminants for which
EPA needs to evaluate new analytical
methods in locations where the con-
taminants are most likely to be found.
EPA will select up to 200 systems to
participate in this testing after consid-
ering the characteristics of the con-
taminants, precipitation, system oper-
ation, and environmental conditions.
You will be notified by the State or
EPA that your system has been se-
lected for monitoring under the Pre-
Screen Testing program.
(3) For which contaminants must I mon-
itor? Lists 1, 2 and 3 of unregulated con-
taminants are listed in the following
table:
TABLE 1—UNREGULATED CONTAMINANT MONITORING REGULATION (1999) LIST
List 1—Assessment Monitoring Chemical Contaminants
1 -Contaminant
2 4-dinitrotoluene
2, 6 dinitrotoluene
Acetochlor
DCPA mono-acid degradateh
2-CAS reg-
istry number
121-14-2
606-20-2
34256-82-1
887-54-7
3- Analytical
methods
EPA Method
525.2"
EPA Method
525.2"
EPA Method
525.2"
EPA Method
515.1", EPA
Method 51 5.2",
EPA Method
51 5.3 '•>, EPA
Method 51 5.4 k,
D5317-93",
AOAC 992.32-
"
4-Minimum
reporting
level
2 ng/L'-
2 ng/L =
2 ng/L»
1 ng/L'
5-Sampling
location "
EPTDS '
EPTDS1
EPTDS '
EPTDS1
6-Period
during
which
monitoring
to be
completed
2001-2003
2001-2003
2001-2003
2001-2003
421
-------
§141.40
40 CFR Ch. I (7-1-04 Edition)
TABLE 1—UNREGULATED CONTAMINANT MONITORING REGULATION (1999) LIST—Continued
List 1—Assessment Monitoring Chemical Contaminants
1 -Contaminant
DCPA di-acid degradate11
4 4'-DDE
EPTC
MTBE
2-CAS reg-
istry number
2136-79-0
72-55-9
759_94^t
2212-67-1
1634-04^t
98-95-3
14797 73 0
5902-51-2
3-Analytical
methods
EPA Method
515.1', EPA
Method 515.2",
EPA Method
51 5.3 io, EPA
Method 51 5.4 l,
D5317-93b.
AOAC 992.32'
EPA Method
508", EPA
Method 508.1 ",
EPA Method
525.2 •, D5812-
96 b, AOAC
990.06 =
EPA Method
507', EPA
Method 525.2-,
D5475-93",
AOAC 991. 07"
EPA Method
507", EPA
Method 525.2",
D5475-93",
AOAC 991 .07 <
EPA Method
502.2", SM
6200CJ", EPA
Method 524.2'',
D5790-95'', SM
6210D", SM
6200B"
EPA Method
524.2", D5790-
95 h, SM6210DJ,
SM6200B-J
EPA Method
314. 0'
EPA Method
507", EPA
Method 525.2",
D5475-93",
AOAC 991. 07-
4-Minimum
reporting
level
1 ^g/L°
08 fig/L =
1 ^g/L"
5 ug/L a
1 0 ug/L f
4 ng/Lm
5-Sampling
location
EPTDS '
EPTDS'
EPTDS'
EPTDS'
EPTDS'
EPTDS1
EPTDS1
EPTDS1
6-Period
during
which
monitoring
to be
completed
2001-2003
2001-2003
2001-2003
2001-2003
2001-2003
2001-2003
2001 2003
2001-2003
Column headings are:
'—Chemical or microbiological contaminant: the name of the contaminants to be analyzed.
2—CAS (Chemical Abstract Service Number} Registry No. or Identification Number: a unique number identifying the chemical
contaminants.
3—Analytical Methods: method numbers identifying the methods that must be used to test the contaminants.
4—Minimum Reporting Level: the value and unit of measure at or above which the concentration or density of the contaminant
must be measured using the Approved Analytical Methods.
5—Sampling Location: the locations within a PWS at which samples must be collected.
6—Years During Which Monitoring to be Completed: The years during which the sampling and testing are to occur for the indi-
cated contaminant.
The procedures shall be done in accordance with the documents listed next in these footnotes. The incorporation by reference
of the following documents listed in footnotes b-d, i, k and I was approved by the Director of the Federal Register in accordance
with 5 U.S.C. 552{a) and 1 CFR part 51. Copies of the documents may be obtained from the following sources. Information re-
garding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be
inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460 (Telephone: 202-260-3027); or at the
National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/federal register/code of federal regulations/ibr locations.html.
"The version of the EPA methods which you must follow for this Rule are listed at §141.24 (e).
422
-------
Environmental Protection Agency
§141.40
"Annual Book of ASTM Standards, 1996, 1998 and 1999, Vol. 11,02. American Society for Testing and Materials. Method
D5812-96, ''Standard Test Method for Determination of Qrganoohlorine Pesticides in Water by Capillary Column Gas Chroma-
iography", is located in the Annual Book of ASTM Standards, 1998 and 1999, Vol. 11,02. Methods 05790-95, "Standard Test
Method for Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Speetrom-
etry"; D5475-93, ''Standard Test Method for Nitrogen- and Phosphorus-Containing Pesticides in Water by Gas Chrornatography
with a Nitrogen-Phosphorus Detector"; and D5317-93, "Standard Test Method for Determination of Chlorinated Organic Acid
Compounds in Water by Gas Chromatogfaphy with an Electron Capture Detector" are located in the Annual Book of ASTM
Standards, 1996 and 1990, Vol 11.02. Copies may be obtained from the American Society for Testing and Materials, 100 Barr
Harbor Drive, West Conshohocken, PA 19428,
, ,
'-'Official Methods of Analysis of AOAC (Association of Official Analytical Chemist) Internationa!, Sixteenth Edition, 4th Revi-
, AOAC Internationa!, First Unio
379-2622,
sion. 1998, Volume I
nion National Bank Lockbox, PO Box 75198, Baltimore, MD 21275-5198. 800™
,
dSM 6210 D is only found in the 18th and 19th editions of Standard Methods for the Examination of Water and Wastewater,
1992 and 1995, American Public Health Association; either edition may be used. SM 6200 B and 6200 C are only found in the
20th edition of Standard Methods for the Examination of Water and Wastewater, 1998. Copies may be obtained from the Amer-
ican Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005.
e Minimum Reporting Level determined by rnuttiplying by 10 the least sensitive method's detection limit (detection limit
=standard deviation times the Student's t value for 99% confidence level with n-1 degrees of freedom), or when available, multi-
plying by 5 the least sensitive method's estimated detection limit (where the estimated detection limit equals the concentration ot
compound yielding approximately a 5 to 1 signal to noise ratio or the calculated detection limit, whichever is greater).
'"Entry Points to the Distribution System (EPTDS), after treatment, representing each non-emergency water source in use over
the twelve-month period of monitoring: this only includes entry points for sources in operation during the months in which sam-
pling is to occur. Sampling must occur at the EPTDS, unless the State has specified other sampling points that are used tor
compliance monitoring under 40 CFR 141,24 (f)(1). (2), and (3). See 40 CFR 141.40{a)(5)(ii)(C) for a complete explanation of re-
quirements, including the use of source (raw) water sampling points,
£ Minimum Reporting Levels (MRL) for Volatile Organic Compounds (VOC) determined by multiplying either the published de-
tection ismit or 0,5 ^g/L times 10, whichever is greater. The detection limit of 0.5 ug/L (0.0005 mg/L) was selected to conform to
VOC detection limit requirements of 40 CFR 141.24(f)(17)(E).
•"•The approved methods do not allow for the identification and quantrtation of the individual acids. The single analytical result
obtained should be reported as total DCPA mono- and di-acid degradates.
5 EPA Method 515.3, "Determination of Chlorinated Acids in Drinking Water by Liquid-Liquid Extraction, Deri validation and Gas
Chromatography with Electron Capture Detection," Revision 1-0 July 1996. EPA 815-R-GQ-014, "Methods for the Determination
of Organic and Inorganic compounds in Drinking Water, Volume 1," August 2000, Available from the National Technical Informa-
tion Service. NTiS PB2000-1 06981, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161 The toll
free number is 800-553-6847. Alternatively, the method can be assessed and downloaded directly on-line at www.epa,gov/
safe water/methods/sou re alt- html.
E Since EPA Method 515.3 does not include a solvent wash step following hydrolysis, the parent DCPA is not removed prior to
analysis, therefore, only non-defec! data may be reported using EPA Method 515.3. All samples with results above the MRL
must be analyzed by one of the other approved methods,
VEPA Method 515.4, "Determination of Chlorinated Acids in Drinxing Waier by Liquid-Liquid Microextraction, Derivatization and
Fast Gas Chromatography with Electron Capture Detection," Revision 1.0, April 2000, EPA #815/6-00/001. Available by request-
ing a copy from the EPA Safe Drinking Water Hotiine within the United States at 800-426-4791 (Hours are Monday through Fri-
day, excluding federal holidays, from 9 a.m. to 5:30 p.m. Eastern Time), Aiternativeiy, the method can be assessed and
downloaded directly on-fine at www, epa.gov/safewater/methods/sourcalt, html.
! EPA Method 314,0, "Determination of Perchlorate in Drinking Water Using Ion Chromatography," Revision 1.0, EPA 815*8-
99-003, November 1999, EPA 815-R-00-014, "Methods for the Determination of Organic and inorganic Compounds in Drinking
Water, Volume 1," August 2000, Available from the National Technical Information Service, NTIS PB2000-1 06961, U.S. Depart-
ment of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161 The toil free number is 800-553-6847, Alternatively, the
method can be assessed and downloaded direciiy on-line at www, epa.gov/safe water/mefhods/sourcalf html.
™MRL was established at a concentration, which is at least Vith the lowest known adverse health concentration, a! which ac-
ceptable precision and accuracy has been demonstrated in spiked matrix samples,
"Sample preservation techniques and holding times specified in EPA Method 524.2 must be used by laboratories using either
EPA Method 502-2 or Standard Methods 6200C.
?-Contaminant
List 2—Screening Survey Chemical Contaminants
1.2- ] 122-66-7
diphenyihydrazin- j
2-methy!-phenol
2,4-dJchbrophenol
2.4-dinitroph0nol ....
2A6-
trichlorophenoi.
Alachlcr ESA
Diazinon
95-48-7 ..
120-83-2
51-28-5 ..
8S-OS-2 ..
Reserved d
333-41-5
EPA Method 528" j 1 fig/L'
EPA Method 528 ^ ! 1 u.g/L<
EPA Method 528*' j 5 ug/L'
EPA Method 528 h 1 pgrt--'
: EPTDS1-' .
j EPTDS--' .
Reserved11 ,.,„,....
EPA Method 526'*
Reservedd
0,5 gg/Lf ...
,.,,.... ' Reserved d
Oisulfoton
EPA Method 528^
1 EPTDS--' ...
6-Period during
which
monitoring to be
completed
1 2001—Selected
j Systems serving
I <10tOOOper-
i sons;
! 2002—Selected
: systems serving
j > 10,000 per-
sons.
j Same as above.
• Same as above.
j Same as above-
Same as above,
Reserved'1
2001— Seieecfed
Systems serving
^10,000 per-
sons'.
2002—Selected
systems serving
> 10,000 per-
sons.
Same as above.
423
-------
§141,40
40 CFR Ch. I (7-1-04 Edition)
List 2—Screening Survey Chemical Contaminants
1 -Contaminant
DIuron
Nitrobenzene
RDX
2-CAS registry
number
330-54-1
944-22-9
330-55-2
98-95-3
1610-18-0
121—82-4
13071-79-9
3-AnaIytical
methods
EPA Method 532'
EPA Method 528*
EPA Method 532 =
EPA Method 526 «
EPA Method 526*
EPA Method 526 »
4-Minirnum
reporting
level
1»ig/L' ..................
0-5 jig/Lf ,,,,
1 ^g/Lr
0.5 M9/lf ...............
O.Siig/L1 ...... .
S-Sampiincj
location
EPTDS" ..............
EPTDS e . .
EPTDS e
EPTDSe ..„.„,.,.,..,.
EPTDS e .. .
EPTDS e , .,
8-Period during
which
monitoring to be
completed
Same as above.
Same as above.
2001— Selected
Systems serving
£10,000 per-
sons;
2002-Selected sys-
tems serving >
10,000 persons.
LIST 2—SCREENING SURVEY MICROBIOLOGICAL CONTAMINANTS To BE SAMPLED
, f. .. . , 2 — Identification 3— Analytical
1 -Contaminant number me^ds
A0romonas ,,.,.,.,.......,.., NA ,....,.,,.,.
........... EPA Method
1605h.
4— Minimum re- 5— Sampling loca-
porttng level tion
0,2— CFU/lGOmLf Distribution Sys-
tems
6 — Period during
which monitoring
to be completed
2003
Column headings are:
! —Chemical or microbiological contaminant; the name ot the contaminants to be analyzed,
~—CAS (Chemical Abstract Service Number) Registry No, or Identification Number: a unique number identifying the chemical
contaminants.
3—Analytical Methods: method numbers identifying the methods that must be used to test the contaminants.
4—Minimum Reporting Level; the value and unit of measure at or above which the concentration or density of the contaminant
must be measured using the Approved Analytical Methods,
*•••—Sampling Location: the locations within a PVYS at which samples must be collected.
£—Years During Which Monitoring to be Completed: the years during which the sampling and testing are to occur for the indi-
cated contaminant.
The procedures shall be done in accordance with the documents listed next in these footnotes. The incorporation by reference
of the following documents listed in footnotes a~c, was approved by the Director of the Federal Register in accordance with 5
U.S.C. 552{a) and 1 CFR part 51. Copies of the documents may be obtained from the following sources. Information regarding
obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Copies of the documents
may be obtained from the sources listed in these footnotes. Information regarding obtaining these documents can be obtained
from the Safe Drinking Water Hotline at 800-428-4791. Documents may be inspected at EPA's Drinking Water Docket, 401 M
Street, SW., Washington, DC 20460 (Telephone; 202-260-302?}; or at the National Archives and Records Administration
(NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: ttftp-S/www.archives.gov/
fedsra!_^r&gister/codeof__federal _f&gu!ationsfit>r locations.html.
«EPA Method 526, "Determination of Selected Semivolatile Organic Compounds in Drinking Water by Solid Phase Extraction
and Capillary Column Gas Chromatography/Mass Spectrometry (GO/MS)," Revision 1.0, June 2000- EPA 815-FMXMH4,
"Methods for !he Determination of Organic and Inorganic Compounds In Drinking Water, Volume 1 ,'* August 2000, Available from
the Nafionai Technical Information Service, NTIS PB2000-106981, U,S- Department of Commerce, 5285 Port Royal Road,
Springfield, Virginia 22181, The toll free number is 800-553-6847. Alternatively, the method can be assessed and downloaded
directly on-line at www.epa.gov/safewater/methods/sourcalt.html.
hEPA Method 528, "Determination of Phenols in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chroma-
tography/Mass Spectrometry {GC/MS};1 Revision 1.0, April 2000- EPA 815-R-00-014, "Methods for the Determination of Or-
ganic and Inorganic Compounds in Drinking Water, Volume 1," August 2000. Available from the National Technical Information
Service, NTIS PB2000-108981, U.S. Department of Commerce, 5285 Port Royal Road, Springfield. Virginia 22161, The toll free
number is 800-553-6847. Alternatively, the method can be assessed and downloaded directly on-line at www.epa.gov/
nerlcwww/ordmeth. htm.
1 EPA Method 532, "Determination of Phenylurea Compounds in Drinking Wafer by Soiid Phase Extraction and High Perform-
ance Liquid Ghromatography with UV Detection," Revision 1.0, June 2000. EPA 815-R-00-014, "Methods for the Determination
of Organic and Inorganic Compounds in Drinking Water, Volume 1," August 2000. Available from the National Technical Informa-
tion Service, NTIS PB20QO-106981, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll
free number is 800-553-6847. Alternatively, the method can be assessed and downloaded directly on-line at www.epa.gov/
safewater/methods/sourcalt.htmL
^To be specified at a Safer time.
€ Entry Points to the Distribution System (EPTDS), after treatment, representing each non-emergency water source in use over
the twelve-month period of monitoring: this only includes entry points for sources in operation during the months in which sam-
pling is to occur. Sampling must occur at the EPTDS, source wafer sampling points are not permitted for List 2 contaminant
monitoring.
fMinimum Reporting Level represents the value of Ihe lowest concentration precision and accuracy determination made during
methods development and documented in the method, if method options are permitted, the concentration used was for the least
sensitive option.
424
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Environmental Protection Agency
§141.40
j= Three samples must be taken from the distribution system, which is owned or controlled by the selected PWS, The sample
locations must include one sample from a point (MD from §141.35{d)(3); Table 1) where the disinfectant residual is representa-
tive of the distribution system. This sample location may be selected from sample locations which have been previously identified
for samples to be analyzed for coliform indicator bacteria- Cotiform sample locations encompass a variety of sites including mid-
point samples which may contain a disinfectant residual thai is typical of the system. Coiiform sample locations are described in
40 CFR 141.21, This same approach must be used for the Aeromonas midpoint sample where the disinfectant residual would
not have declined and would be typical for the distribution system. Additionally, two samples must be taken from two different to-
cations; the distal or dead-end location in the distribution sysfem {MR from §141.35(d)(3), Table 1), avoiding disinfectant booster
stations, and from a location where previous determinations have indicated the lowest disinfectant residual in the distribution sys-
tem (LD from §141.35{d)(3), Table 1). if these two locations of distal and low disinfectant residual sites coincide, then the sec-
ond sample must be taken at a location between the MD and MR sites. Locations in the distribution system where the disinfect-
ant residual is expected to be low are similar to TTHM sampling points. Sampling locations for TTHMs are described in 63 PR
69468.
''EPA Method 1605 ''A&romonas in Finished Water by Membrane Filtration using AmpiaHin-Dextrin Agar with Vancomycin
(ADA-V)". October 2001, EPA # 821-R-01-034. Tne method can be accessed and downloaded directly on-line at
List 3—Pre-screen Testing Radionuelides To Be Sampled After Notice ot Analytical Methods Availability
1 "Contaminant
Lead-210
Polonium-210
2-CAS registry
number
14255-04-0
13961-52-7
! 3-Anaiytical meth-
j ods
I Reserved :r
i Reserved'1 ,....,
4-Minimum
reporting
ievei
Reserved^
Reserved'* , ,
5~Sampiing
location
Reserved-1
Reserved" ,,,.,,
6-Period during
which
monitoring to be
completed
Reserved.-
Reserved."-
List 3—Pre-screen Testing Microorganisms To Be Sampled After Notice of Analytical Methods Availability
1-Contaminant
2-identificafion
number
3-Analytical meth-
ods
Cyanobacteria
(blue-green
algae, other
freshwater algae
and their toxins).
Echoviruses .„,..,....
Coxsackieviruses ...
Helicobacter pylori
Microsporidia
Calciviruses ...........
Adenoviruses
Reservedj
Reserved '•<
ReservedJ
Reserved"
Reserved -'
Reserved •'
ReservedJ
i Reserved-1
Reserved4
Reserved *
Reserveda
Reserved -1
Reservedy
Reserved-1
1 Reserved-1
! Reserved11
1 ReservedJ
I Reserveda
i Reserved-1
> Reserved -
Reserved •'
Reservedj
Reserved:i
Reserved'1
Reserved •'
Reserved-
Column headings are:
1-Chemical or microbiological contaminant; the name of the contaminants to be analyzed.
2-CAS (Chemical Abstract Service Number) Registry No, or identification Number: a unique number identifying the chemical
contaminants,
3™~AnaIyticai Methods; method numbers identifying the rnetnods that must be used to test the contaminants.
4-Minimum Reporting Level: the value and unft of measure at or above which the concentration or density of the contaminant
must be measured using the Approved Analytical Methods.
5-Sampiing Location; the locations within a PWS at which samples must be collected.
6-Years During Which Monitoring to be Completed; the years during which the sampling and tesling are to occur for the indi-
cated contaminant.
• To be determined at a later time.
(4) What general requirements must I
follow for monitoring List 1 contaminants?
(i) All systems. You must:
(A) Collect samples of the listed con-
taminants in accordance with para-
graph (a)(5) of this section and Appen-
dix A of this section and any other spe-
cific instructions provided to you by
the State or EPA.
(B) Analyze the additional param-
eters specified below in Table 2. "Water
Quality Parameters to be Monitored
with UCMR Contaminants" for each
relevant contaminant type. You must
analyze the parameters for each sam-
pling event of each sampling point.
using the method indicated, and report
using the data elements 1 through 10 in
Table 1, §141.35(d), Unregulated Con-
taminant Monitoring Reporting- Re-
quirements;
(C) Review the laboratory testing re-
sults to ensure reliability; and
(D) Report the results as specified in
§141.35.
425
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§141.40
40 CFR Ch. I (7-1-04 Edition)
TABLE 2—WATER QUALITY PARAMETERS To BE MONITORED WITH UCMR CONTAMINANTS
Parameter
pH
Turbidity
Temperature
Free Disinfectant Re-
sidual.
Total Disinfectant Re-
sidual.
Contaminant type
Microbiological
Microbiological
Microbiological
Analytical methods
EPA method Standard methods '
EPA Method 1SG.12,
EPA Method 150.22.
EPA Method 180.-H-' ..
4500-H* B
2130 B4
2550.
4500-CI D, 4500-CI F,
4500-CI G, 4500-CI
H, 4500-CIO, D,
4500-ClOi E, 4500-
O3B.
4500-CI D, 4500-CI
E,4 4500-CI F,
4500-CI G«, 4500-CI
I.
Other
ASTM D1293-843,
ASTM D1293-9S3.
GLI Method 24<>.
ASTM 1253-86'
ASTM D 1 253-86 3
The procedures shall be done in accordance with the documents listed in these footnotes. The incorporation by reference of
the following documents was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR
part 51, Copies of the documents may be obtained from the sources listed in these footnotes. Information regarding obtaining
these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be inspected at
EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460 (Telephone: 202-260-3027); or at the National Ar-
chives and Records Administration (NARA), For information on the availability of this material at NARA, call 202-741-6030, or
go to: http://www.archives.gov/federal register/code_of federal _ regulations/for focations.htm/.
1 The 18th and 19th Editions of Standard Methods lor the Examination ot Water and Wastewater, 1992 and 1995. Methods
2130 B; 2550; 4500-Ci D, E, F, 6, H, I; 4500-CIO; D, E; 45QO-H~* B; and 4500-O., B in the 20th edition Standard Methods for
the Examination of Water and Wastewater, 1998, American Public Health Association, 1015 Fifteenth St. NW, Washington D.C.,
20005.
ZEPA Methods 150.1 and 150.2 are available from US EPA, NERL, 26 W. Martin Luther King Dr., Cincinnati, Ohio 45268. The
identical methods are also in "Methods for Chemical Analysis of Water and Wastes," EPA-600/4-79-020, March 1983, available
from the National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Rd., Springfield, Vir-
ginia 22161, PB84-128677. (Note: NTIS toll-free number is 800-553-6847.)
"Annual Book of ASTM Standards, Editions 1994, 1996, 1998 and 1999, Volumes 11.01, American Society lor Testing and
Materials. 100 Barr Harbor Drive, West Conshohocken, PA 19428. Version D1293-84, "Standard Test Methods for pH of Water"
is located in the Annual Book of ASTM Standards, 1994, Volumes 11.01. Version D1293-95, "Standard Test Methods for pH of
Water" is located in the Annual Book of ASTM Standards, 1996, 1998 and 1999, Volumes 11.01.
4 "Technical Notes on Drinking Water," EPA-800/R-94-173. October 1994, Available at NTIS, PB95-104766.
'"Methods for the Determination of Inorganic Substances in Environmental Samples." EPA-600/R-93-100, August 1993.
Available at NTIS, PB94-121B11
BGLI Method 2, "Turbidity," November 2, 1992, Great Lakes Instruments Inc.. 8855 North 55th St., Milwaukee, Wisconsin
53223.
(ii) Large systems. In addition to para-
graph (a)(4)(i) of this section, you must
arrange for testing of the samples ac-
cording to the methods specified for
each contaminant in Table 1, Unregu-
lated Contaminant Monitoring Regula-
tion (1999) List, in paragraph (a)(3) of
this section, and in Appendix A of this
section.
(iii) Small systems. Unless directed
otherwise by the State or EPA, in addi-
tion to paragraph (a)(4)(i) of this sec-
tion , you must:
(A) Properly receive, store, maintain
and use the sampling equipment sent
to you from the laboratory designated
by EPA;
(B) Sample at the times specified by
the State or the EPA;
(C) Collect and pack samples in ac-
cordance with the instructions sent to
you by the laboratory designated by
EPA; and
(D) Send the samples to the labora-
tory designated by EPA.
(5) What specific sampling' and qual-
ity control requirements must I follow
for monitoring of List 1 contaminants?
(i) All systems. Unless the State or EPA
informs you of other sampling arrange-
ments, you must comply with the fol-
lowing requirements:
(A) Sample collection and shipping
time. If you must ship the samples for
testing, you must collect the samples
early enough in the day to allow ade-
quate time to send the samples for
overnight delivery to the laboratory
since some samples must be processed
at the laboratory within 30 hours of
collection. You must not collect sam-
ples on Friday, Saturday or Sunday be-
cause sampling on these days would
not allow samples to be shipped and re-
ceived at the laboratory within 30
hours.
(B) No compositing of samples. You
must not composite (that is, combine,
mix or blend) the samples. You must
collect, preserve and test each sample
separately.
426
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Environmental Protection Agency
§141.40
(C) Review and reporting of results.
After you have received the laboratory
results, you must review and confirm
the system information and data re-
garding sample collection and test re-
sults. You must report the results as
provided in §141.35.
(ii) Large systems. In addition to para-
graph (a)(5)(i) of this section, you must
comply with the following:
(A) Timeframe. You must collect the
samples In one twelve-month period
during the years indicated in column 6
of Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List.
(B) Frequency. You must collect the
samples within the timeframe and ac-
cording to the following frequency
specified by contaminant type and
water source type:
TABLE 3—MONITORING FREQUENCY BY CONTAMINANT AND WATER SOURCE TYPES
Contain i riant type
Water source type
Timeframe
Frequency
Chemical ,.„„ ...,.,,,,.. I Surface water ,.,, Twelve (12) months ...... Four quarterly samples taken as follows: Select
either the first, second, or third month of a
quarter and sample in that same month of
each of four (4) consecutive quarters-1 to en-
sure that one of those sampling events oc-
curs during the vulnerable tirne,h
i Ground water .....,...,.„... Twelve (12) months ...... Two {2} limes in a year taken as follows: Sam-
ple during one (1) month of the vulnerable
!imeh and during one (1) month five (5) to
seven (7) months earlier or later.-:
Microbiological „.,,... ^ Surface and ground Twelve (12) months ...... Six (6) times in a year taken as follows: Select
water. either the first, second, or third month of a
quarter and sample in that same month of
each of four (4) consecutive quarters, and
sample an additional 2 months during the
warmest {vulnerable} quarter of the year.d
j "Select either the first, second, or third month of a quarter and sample in that same month of each of four (4) consecutive
quarters" means that you must monitor during each of the four (4) months of either: January, April, July, October: or February,
May, August, November; or March, June, September, December.
h "Vulnerable time" means May 1 through July 31, unless the State or EPA informs you that It has selected a different time pe-
riod for sampling as your system's vulnerable time.
••""Sample during one (1) month of the vulnerable time and during one (1) month five (5) to seven (7) months earlier or later"
rneanSj for example, that if you select May as your "vulnerable time" month to sample, then one (1) month five (5) So seven (7)
months earlier would be either October, November or December of the preceding year, and one (!) month five (5) to seven (?)
months later would be either, October, November, or December of the same year.
"JJhis means that you must monitor during each of the six (6) months of either: January, April, July, August, September, Octo-
ber; or February, May, July, August, September, November; or March, June, July, August. September, December; unless the
Stale or EPA informs you that a different vulnerable quarter has been selected for your system.
(C) Location. You must, collect sam-
ples at the location specified for each
listed contaminant in column 5 of the
Table 1, UCMB (1999) List, in paragraph
(a)(3) of this section. The sampling- lo-
cation for chemical contaminants must
be the entry point to the distribution
system or the compliance monitoring
point specified by the State or EPA
under 40 CFR 141,24 (f)(l), (2), and (3).
Except as provided in this paragraph
(a)(5){ii)(C), if the compliance moni-
toring point as specified by the State is
for source (raw) water and any of the
contaminants in paragraph (a){3) of
this section are detected, then you
must complete the source water moni-
toring for the indicated timeframe and
also sample at the entry point to the
distribution system representative of
the affected source water only for the
contaminant(s) found in the source
water over the next twelve month
timeframe, beginning in the next re-
quired monitoring period as indicated
in paragraph (a)(5)di)(B), Table 3 of
this section, even though monitoring
might extend beyond the last year indi-
cated in column 6. Period during which
monitoring to be completed, in Table 1
of paragraph (a)(3). Exception: If the
State or EPA determines that sam-
pling at the entry point to the distribu-
tion system is unnecessary because no
treatment was instituted between the
source water and the distribution sys-
tem that would affect measurement of
the contaminants listed in paragraph
(a)(3) of this section, then you do not
have to sample at the entry point to
the distribution system. Note: The
sampling for List 2 chemical contami-
nants must be at the entry point to the
427
-------
§141.40
40 CFi Ch. I (7-1-04 Edition)
distribution system, as specified in
Table 1, List 2.
(D) Sampling instructions. You must
follow the sampling procedure for the
method specified in column 3 of List 1
of Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section, for
each contaminant.
(E) Testing and analytical methods.
For each listed contaminant, you must
use the analytical method specified in
column 3 of List 1 of Table 1, Unregu-
lated Contaminant Monitoring Regula-
tion (1999) List, in paragraph (a)(3) of
this section, the minimum reporting
levels in column 4 of List 1 of Table 1,
Unregulated Contaminant Monitoring
Regulation (1999) List, in paragraph
(a)(3) of this section, and the quality
control procedures specified in Appen-
dix A of this section.
(F) Sampling deviations. If you do not
collect a sample according to the pro-
cedures specified for a listed contami-
nant, you must resample within 14 days
of observing the occurrence of the error
(which may include notification from
the laboratory that you must re-
sample) following the procedures speci-
fied for the method. (This resampling
is not for confirmation sampling but to
correct the sampling error.)
(G) Testing. (1) Except as provided in
paragraph (a)(5)(ii)(G)(2) and (3) of this
section, you must arrange for the test-
ing of the contaminants identified in
List 1 of Table 1 by a laboratory cer-
tified under §141,28 for compliance
analysis using any of the analytical
methods listed in column 3 for each
contaminant in List 1 of Table 1, Un-
regulated Contaminant Monitoring
Regulation (1999) List, in paragraph
(a)(3) of this section, whether you use
the EPA analytical methods or non-
EPA methods listed in List 1 of Table
1. Laboratories are automatically cer-
tified for the analysis of UCMR con-
taminants in List 1 of Table 1 if they
are already certified to conduct com-
pliance monitoring for a contaminant
included in the same method being ap-
proved for UCMR analysis. Labora-
tories certified under §141.28 for com-
pliance analysis using EPA Method
515.3 are automatically approved to
conduct UCMR analysis using EPA
Method 515.4.
(2) You must arrange for the testing
of Perchlorate as identified in List 1 of
Table 1 by a laboratory certified under
§141.28 for compliance analysis using
an approved ion chromatographic
method as listed in §141.28 and that has
analyzed and successfully passed the
Performance Testing (PT) Program ad-
ministered by EPA.
(3) You must arrange for the testing
of the chemical contaminants identi-
fied in List 2 of Table 1 by a laboratory
certified under §141.28 for compliance
analysis using EPA Method 525.2 if per-
forming UCMR analysis using EPA
Methods 526 or 528, or a laboratory cer-
tified under §141.28 for compliance
analysis using EPA Methods 549.1 or
549.2 if performing UCMR analysis
using EPA Method 532. You must ar-
range for the testing for Aeromonas
using the approved method as identi-
fied in List 2 of Table 1 by a laboratory
which is both certified under §141.28 for
compliance analysis for coliform indi-
cator bacteria using an EPA approved
membrane filtration procedure and
which also has been granted approval
for UCMR monitoring of Aeromonas by
successfully passing the Aeromonas Per-
formance Testing (PT) Program admin-
istered by EPA.
(iii) Small systems that are part of the
State Monitoring Plan. Unless directed
otherwise by the State or EPA, in addi-
tion to paragraph (a)(5)(i) of this sec-
tion, you must comply with the fol-
lowing:
(A) Timeframe and frequency. You
must collect samples at the times spec-
ified for you by the State or EPA,
within the timeframe specified in para-
graph (a)(5)(ii)(A) of this section and
according to the frequency specified in
paragraph (a)(5)(ii)(B) of this section
for the contaminant type and water
source type.
(B) Location. You must collect sam-
ples at the locations specified for you
by the State or EPA.
(C) Sampling deviations. If you do not
collect a sample according to the in-
structions provided to you for a listed
contaminant, then you must report the
deviation on the sample reporting form
that you send to the laboratory with
the samples. You must resample fol-
lowing instructions that you will be
428
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Environmental Protection Agency
§141,40
sent from EPA's designated laboratory
or the State.
(D) Sample kits. You must store and
maintain the sample collection kits
sent to you by EPA's designated lab-
oratory in a secure place until used for
sampling. You should read the instruc-
tions for each kit when you receive it.
If indicated in the kit's instructions,
you must freeze the cold packs. The
sample kit will include all necessary
containers, packing materials and cold
packs, instructions for collecting the
sample and sample treatment (such as
dechlorination or preservation), report
forms for each sample, contact name
and telephone number for the labora-
tory, and a prepaid return shipping
docket and return address label. If any
of the materials listed in the kit's in-
structions are not included or arrive
damaged, you must notify EPA's des-
ignated laboratory which sent you the
sample collection kits,
(E) Sampling instructions. You must
comply with the instructions sent to
you by the State or EPA concerning
the use of containers, collection (how
to fill the sample bottle),
dechlorination and/or preservation, and
sealing and preparing the sample and
shipping containers for shipment. You
must also comply with the instructions
sent to you by EPA's designated lab-
oratory concerning the handling of
sample containers for specific contami-
nants.
(F) Duplicate samples. EPA will select
systems in the State Monitoring Plan
that must collect duplicate samples for
quality control. If your system is se-
lected, you will receive two sample
kits that you must use. You must use
the same sampling protocols for both
sets of samples, following the instruc-
tions in the duplicate sample kit,
(G) Sampling forms. You must com-
pletely fill out the sampling forms sent
to you by the laboratory, including the
data elements 1 through 4 listed in
§141.35(d) for each sample. If EPA re-
quests that you conduct field analysis
of water quality parameters specified
in paragraph (a)(4)(i)(B) of this section,
you must also complete the sampling-
form to include the information for
data elements 5 through 10 listed in
§141.35(d) for each sample. You must
sign and date the sampling forms.
(H) Sample submission. Once you have
collected the samples and completely
filled in the sampling forms, you must
send the samples and the sampling-
forms to the laboratory designated in
your instructions.
(6) What additional requirements must I
follow if my system is selected as an Index
system? If your system is selected as an
Index system in the State Monitoring
Plan, you must assist the State or EPA
in Identifying appropriate sampling lo-
cations and provide information on
which wells and intakes are in use at
the time of sampling, well casing and
screen depths (if known) for those
wells, and the pumping rate of each
well or intake at the time of sampling.
(?) What must I do if my system is se-
lected for the Screening Surveys or Pre-
Screen Testing? (i) All systems. You
must:
(A) Analyze the additional param-
eters specified in paragraph
§141.40(a)(4)(i), Table 2, "Water Quality
Parameters to be Monitored with
UCMR Contaminants" for each relevant
contaminant type. You must analyze
the parameters for each sampling event
of each sampling point, using the
method indicated, and report the re-
sults using the data elements 1 through
10 in Table 1, §141.35(d). Unregulated
Contaminant Monitoring- Reporting re-
quirements;
(B) Review the laboratory results to
ensure reliability; and
(C) Report the results as specified in
§141,35.
(ii) Large systems. If your system
serves over 10,000 persons, you must
collect and arrange for testing of the
contaminants in List 2 and List 3 of
Table 1, Unregulated Contaminant
Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section, in ac-
cordance with the requirements set out
in paragraphs (a)(4) and (5) of this sec-
tion, with one exception: you must
sample only at sampling locations
specified in Table 1. You must send the
samples to one of the laboratories ap-
proved under paragraph (G), this sec-
tion. You are also responsible for re-
porting these results as required in
§141.35.
(iii) Small systems. If your system
serves 10,000 or fewer persons, you must
collect samples in accordance with the
429
-------
§141.40
40 CFR Ch. I (7-1-04 Edition)
instructions sent to you by the EPA or
State, or, if informed by the EPA or
State that the EPA or State will col-
lect the sample, you must assist the
State or EPA in identifying the appro-
priate sampling- locations and in taking
the samples. EPA will report the re-
sults to you and the State.
(8) What is a violation of this Rule? (i)
Any failure to monitor in accordance
with §141.40(a)(3) through (7) and Ap-
pendix A is a monitoring violation, fii)
Any failure to report in accordance
with §141.35 is a reporting violation.
(b) Requirements for State and Tribal
Participation. (1) How can I. as the di-
rector of a State or Tribal drinking-
water program, participate in unregu-
lated contaminant monitoring, includ-
ing Assessment Monitoring (which in-
cludes the State Monitoring Plan for
small systems), the Screening Surveys,
and Pre-Screen Testing of all systems?
You can enter into a Memorandum of
Agreement (MOA) with the EPA that
describes your State's or Tribe's activi-
ties to:
(i) Accept or modify the initial plan.
EPA will first specify the systems serv-
ing 10,000 or fewer persons by water
source and size in an initial State Mon-
itoring Plan for sach State using a ran-
dom number generator. EPA will also
generate a replacement list of systems
for systems that may not have been
correctly specified on the initial plan.
This initial State Monitoring Plan will
also indicate the year and day, plus or
minus two (2) weeks from the day, that
each system must monitor for the con-
taminants in List 1 of Table 1 of this
section, Unregulated Contaminant
Monitoring Regulation (1999) List. EPA
will provide you with the initial moni-
toring- plan for your State or Tribe, in-
cluding systems to be Index systems
and those systems to be part of the
Screening Surveys. Within sixty (60)
days of receiving your State's initial
plan, you may notify EPA that you ei-
ther accept it as your State Monitoring
Plan or request to modify the initial
plan by removing systems that have
closed, merged or are purchasing water
from another system and replacing
them with other systems. Any pur-
chased water system associated with a
non-purchased water system must be
added to the State Monitoring Plan if
the State determines that its distribu-
tion system is the location of the max-
imum residence time or lowest dis-
infectant residual of the combined dis-
tribution system. In this case, the pur-
chased water system must monitor for
the contaminants for which the "dis-
tribution system" is identified as the
point of "maximum residence time" or
"lowest disinfectant residual," depend-
ing on the contaminant, and not the
community water system selling water
to it. You must replace any systems
you removed from the initial plan with
systems from the replacement list in
the order they are listed. Your request
to modify the initial plan must include
the modified plan and the reasons for
the removal and replacement of sys-
tems. If you believe that there are rea-
sons other than those previously listed
for removing and replacing one or more
other systems from the initial plan,
you may include those systems and
their replacement systems in your re-
quest to modify the initial plan. EPA
will review your request to modify
your State's initial plan. Please note
that information about the actual or
potential occurrence or non-occurrence
of contaminants at a system or a sys-
tem's vulnerability to contamination
is not a basis for removal from or addi-
tion to the plan.
(ii) Determine an alternate vulnerable
time. Within 60 days of receiving the
initial State Monitoring Plan, you may
also determine that the most vulner-
able time of the year for any or all of
the systems in the plan, and for any of
the large systems that must monitor,
is some period other than May 1
through July 31. If you make this de-
termination, you must modify the ini-
tial plan to indicate the alternate vul-
nerable time and to which systems the
alternate vulnerable time applies, EPA
will review these determinations when
you submit your request to modify
your State's initial monitoring plan to
the EPA. You must notify the small
system(s) in your final State Moni-
toring Plan and the large system(s) of
the most vulnerable time(s) of the year
that you have specified for them to
sample for one of their sampling
events. You must notify them at least
90 days before their first unregulated
contaminant sampling is to occur. You
430
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Environmental Protection Agency
§141.40
may need to consider the timing of
monitoring in paragraph (b)(l)(iii) of
this section.
(iii) Modify the timing of monitoring.
Within sixty (60) days of receiving" the
initial plan, you may also modify the
plan by selecting an alternative year
and day. plus or minus two (2) weeks,
within the years specified in column 6,
List 1 of Table 1, Unregulated Contami-
nant Monitoring Regulation (1999) List,
in paragraph (a)(3) of this section, for
monitoring for each system in the ini-
tial plan as long as approximately one-
third of the systems in the State Plan
monitor in each of the three (3) years
listed. This monitoring may be coordi-
nated with regulated contaminant
compliance monitoring at your discre-
tion. You must send the modified plan
to EPA.
(iv) Identify alternate sampling points
for small systems in the Stale Monitoring
Plan. All systems are required to mon-
itor for the contaminants at the sam-
pling- locations specified In column 5,
List 1 of Table 1, Unregulated Contami-
nant Monitoring Regulation (1999) List,
in paragraph (a)(3) of this section, un-
less the State specifies an alternate
compliance sampling point as the sam-
pling location. If the compliance sam-
pling points for the small systems in
the State Monitoring Plan are different
than those specified in paragraph (a)(3)
of this section, then you must indicate
these sampling points in the plan.
These alternative sampling points
must allow proper sampling and test-
ing for the unregulated contaminants.
(v) Notify small and large systems of
their monitoring responsibilities. You
must provide notification to systems in
the plan and, where appropriate, the
large systems, at least ninety (90) days
before sampling must occur.
(vi) Provide instructions to systems that
are part of the final State Monitoring
Plan. You must send a monitoring
schedule to each system listed in the
State Monitoring Plan and instruc-
tions on location, frequency, timing of
sampling, use of sampling equipment,
and handling and shipment of samples
based on these regulations. EPA will
provide you with guidance for these in-
structions. If you perform the sampling
or make alternative arrangements for
the sampling at the systems in the
plan, you must inform EPA at least six
(6) months before the first monitoring
is to occur and address the alternative
monitoring arrangements in the MOA.
fvli) Participate in monitoring for the
Screening Surveys for small and large sys-
tems. Within 120 days prior to sampling,
EPA will notify you which systems
have been selected to participate in the
Screening Surveys, the sampling dates,
the designated laboratory for testing,
and instructions for sampling. You
must review the small systems that
EPA selected for the State Monitoring
Plan to ensure that the systems are
not closed, merged or purchasing water
from another system (unless the sys-
tem is to conduct monitoring for a con-
taminant with the sampling location
specified as "distribution system"), and
then make any replacements in the
plan, as described in paragraph (b)(l)(i)
of this section. You must notify the se-
lected systems in your State of these
Screening Surveys requirements. You
must provide the necessary Screening
Surveys information to the selected
systems at least ninety (90) days prior
to the sampling date.
(viii) Participate in monitoring for Pre-
Screen Testing for small and large sys-
tems. You can participate in Pre-Screen
Testing in two ways,
(A) First, within ninety (90) days of
BPA's letter to you concerning' initi-
ation of Pre-Screen Testing for specific
contaminants, you can identify from
five (5) up to twenty-five (25) systems
in your State that you determine to be
representative of the most vulnerable
systems to these contaminants, modify
your State Monitoring Plan to include
these most vulnerable systems if any
serve 10,000 or fewer persons, and notify
EPA of the addition of these systems
to the State Plan. These systems must
be selected from all community and
non-transient noncommunity water
systems. EPA will use the State-identi-
fied vulnerable systems to select up to
200 systems nationally to be monitored
considering the characteristics of the
contaminants, precipitation, system
operation, and environmental condi-
tions.
(B) Second, within 120 days prior to
sampling, EPA will notify you which
systems have been selected, sampling
dates, the designated laboratory for
431
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§141.40
40 CFR Ch. I (7-1-04 Edition)
testing of samples for systems serving
10,000 or fewer persons and approved
laboratories for systems serving more
than 10,000 persons, and instructions
for sampling. You must notify the own-
ers or operators of the selected systems
in your State of these Pre-Screen Test-
ing requirements. At least ninety (90)
days prior to the sampling date, you
must provide the necessary Pre-Screen
Testing information to the owners or
operators of the selected systems and
then inform EPA that you took this
action to allow sufficient time for EPA
to ensure laboratory readiness.
(ix) Revise system's treatment plant lo-
cation(s) to include latitude and lon-
gitude. For reporting to the Safe Drink-
ing Water Information System, EPA
already requires reporting of either the
latitude and longitude or the street ad-
dress for the treatment plant location.
If the State enters into an MO A, the
State must report each system's treat-
ment plant location(s) as latitude and
longitude (in addition to street ad-
dress, if previously reported) by the
time of the system's reporting of As-
sessment Monitoring results to the Na-
tional Drinking Water Contaminant
Occurrence Database. The State may
use the latitude and longitude of facili-
ties related to the public water system
on the same site, or closely adjacent to
the same site as the treatment plant,
such as the latitude and longitude of
the intake or wellhead/field or the
entry point to the distribution system,
if such measurements are available.
(2) What if I decide not to participate
in an MOA? If you decide not to enter
into an MOA with EPA to develop the
State Monitoring Plan for small sys-
tems, the initial monitoring plan that
BPA sent you will become the final
State Monitoring Plan for your State
or Tribe, In that case, you may still
notify each public water system of its
selection for the plan and instructions
for monitoring as long as you notify
EPA that you will be undertaking this
responsibility at least six (6) months
prior to the first unregulated contami-
nant monitoring.
(3) Can I add contaminants to the Un-
regulated Contaminant Monitoring
List? Yes, the SDWA allows Governors
of seven (7) or more States to petition
the EPA Administratot to add one or
more contaminants to the Unregulated
Contaminant Monitoring Regulation
(1999) List, in paragraph (a)(3) of this
section. The petition must clearly
identify the reason(s) for adding the
contaminant(s) to the monitoring list
in paragraph (a)(3) of this section, in-
cluding, the potential risk to public
health, particularly any information
that might be available regarding dis-
proportional risks to the health and
safety of children, the expected occur-
rence documented by any available
data, any analytical methods known or
proposed to be used to test for the con-
taminants), and any other information
that could assist the Administrator in
determining which contaminants
present the greatest public health con-
cern and should, therefore, be included
on the Unregulated Contaminant Moni-
toring Regulation (1999) List, in para-
graph (a)(3) of this section.
(4) Can I waive monitoring require-
ments? Only with EPA approval and
under very limited conditions. Condi-
tions and procedures for obtaining the
only type of waiver available under
these regulations are as follows:
(i) Application. You may apply to
EPA for a State-wide waiver from the
unregulated contaminant monitoring
requirements for public water systems
serving more than 10,000 persons. To
apply for such a waiver, you must sub-
mit an application to BPA that in-
cludes the following information:
(A) the list of contaminants on the
Unregulated Contaminant Monitoring
List for which you request a waiver,
and
(B) documentation for each contami-
nant in your request demonstrating
that the contaminants have not been
used, applied, stored, disposed of, re-
leased, naturally present or detected in
the source waters or distribution sys-
tems in your State during the past 15
years, and that it does not occur natu-
rally in your State.
(ii) Approval. EPA will notify you if
EPA agrees to waive monitoring re-
quirements.
APPENDIX A TO §141.40—QUALITY CON-
TROL REQUIREMENTS FOB TESTING
ALL SAMPLES COLLECTED
Your system must ensure thai the quality
control remiirements listed below for testing
432
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Environmental Protection Agency
§141.40
of samples collected and submitted under
§141.40 are followed:
(1) Sample Collection/Preservation. Follow
the sample collection and preservation re-
quirements for the specified method for each
of the contaminants in Table 1, XJCMR (1999)
List, in paragraph (a)(3) of this section.
These requirements specify sample con-
tainers, collection, decMorination, preserva-
tion, storage, sample holding- time, and ex-
tract storage and/or holding time that the
laboratory must follow.
(2) Detection Limit, Calculate the labora-
tory detection limit for each contaminant in
Table 1. Unregulated Contaminant Moni-
toring Regulation (1999) List, of paragraph
i.a)(3) of this section using- the appropriate
procedure in the specified method with the
exception that the contaminant concentra-
tion used to fortify reagent water must be
less than or equal to the minimum reporting
level (MRL) for the contaminants as speci-
fied in column 4, Table 1, UCMR (1999) List,
in paragraph (a){3) of this section. The cal-
culated detection limit is equal to the stand-
ard deviation times the Student's t value for
99% confidence level with n-1 degrees of free-
dom. (The detection limit must be less than
or equal to one-half of the MRL.)
(3) Calibration, Follow the initial calibra-
tion requirements as specified in the method
utilized. Calibration must be verified ini-
tially with a low-level standard at a con-
centration at or below the MRL for each con-
taminant. Perform a continuing calibration
verification following every 10th sample. The
calibration verification must be performed
by alternating low-level and mid-level cali-
bration standards. The low-level standard is
defined as a concentration at or below the
MRL with an acceptance range of ±40%. The
mid-level standard is in the middle of the
calibration range with an acceptance range
of-20%,
(4) Reagent Blank Analysis. Analyze one
laboratory reagent: (method) blank per sam-
ple set/batch that is treated exactly as a
sample. The maximum allowable background
concentration is one-half of the MRL for all
contaminants. A field reagent blank is re-
quired only for EPA Method 524.2 (or equiva-
lent listed methods, D5790.95. SM6210D, and
SMG20QB).
(5} Quality Control Sample, Obtain a qual-
ity control sample from an external source
to check laboratory performance at least
once each quarter.
(6) Matrix Spike and Duplicate. Prepare
and analyze the sample matrix spike (SMS)
for accuracy and matrix spike duplicate
(MSD) samples for precision to determine
method accuracy and precision for all con-
taminants in Table 1. Unregulated Contami-
nant Monitoring Regulation (1999) List, in
paragraph (a)(3) of this section. SMS/MSD
samples must be prepared and analyzed at a
frequency of 5% (or one SMS/MSD set per
every 20 samples) or with each sample batch
whichever is more frequent. In addition, the
SMS'MSD spike concentrations must be al-
ternated between a low-level spike and mid-
level spike approximately 50% of the time.
(For example: a set of 40 samples will require
preparation and analysis of two SMS/MSD
sets. The first set must be spiked at either
the low-level or mid level, and the second set
must be spiked with the other standard, ei-
ther the low-level or mid-level, whichever
was not used for the initial SMS/MSD set).
The low-level SMS/MSD spike concentration
must be within ±20% of the MRL for each
contaminant. The mid-level SMS/MSD spike
concentration must be within ±20% of the
mid-level calibration standard for each con-
taminant, and should represent, where pos-
sible, an approximate average concentration
observed in previous analyses of that
analyte. The spiking concentrations must be
reported in the same units of measure as the
analytical results.
(7) Internal Standard Calibration. As ap-
propriate to a method's requirements to be
used, test and obtain an internal standard
for the methods for each chemical contami-
nant in Table 1. Unregulated Contaminant
Monitoring Regulation (1999) List, in para-
graph (a)(3) of this section, a pure contami-
nant of known concentration, for calibration
and quantitation purposes. The methods
specify the percent recovery or response that
you must obtain for acceptance.
(8) Method Performance Test. As appro-
priate to a method's requirements, test for
surrogate compounds, a pure contaminant
unlikely to be found in any sample, to be
used to monitor method performance. The
methods specii'y the percent recovery that.
you must obtain for acceptance.
(9) Detection Confirmation. Confirm any
chemical contaminant analyzed using a gas
chromatogTaphic method and detected above
the MRL, by gas ehromatographic/mass spec-
trometric (GO-MS) methods. If testing re-
sulted in first, analyzing the sample extracts
via specified gas chromatographic methods,
an initial confirmation by a second column
dissimilar to the primary column may be
performed. If the contaminant detection is
confirmed by the secondary column, then the
contaminant must be reconfirmed by GC MS
using three (3) specified ion peaks for con-
taminant identification. Use one of the fol-
lowing confirming techniques: perform sin-
gle point calibration of the GC/MS system
for confirmation purposes only as long as the
calibration standard is at a concentration
within ± 50% of the concentration deter-
mined by the initial analysis; or perform a
three (3) point calibration with single point
daily calibration verification of the GC/MS
system regardless of whether that
verification standard concentration is within
± 50% of sample response. If GO/MS analysis
confirms the initial contaminant detection.
433
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§141.41
40 CFR Ch. I (7-1-04 Edition)
report results determined from the initial
analysis.
(10) Reporting, Report the analytical re-
sults and other data, with the required data
listed in 40 CFR 141.35, Table 1. Report this
data electronically to EPA, unless EPA
specifies otherwise, and provide a copy to the
State. Systems must coordinate with their
laboratories for electronic reporting to EPA
to ensure proper formatting' and timely data
submission.
(11) Method Defined Quality Control. As
appropriate to the method's requirements,
perform analysis of Laboratory Fortified
Blanks and Laboratory Performance Checks
as specified in the method. Each method
specifies acceptance criteria for these qual-
ity control checks.
[64 FR 50612, Sept. 17, 1999. as amended at 65
FB 11382, Mar. 2, 2000; 66 FR 2302, Jan. 11,
2001; 66 FR 27215, May 16, 2001; 66 FR 46225,
Sept. 4, 2002; 67 FR 65900, Oct. 29, 2002]
8141,41 Special monitoring for so-
dium,
(a) Suppliers of water for community
public water systems shall collect and
analyze one sample per plant at the
entry point of the distribution system
for the determination of sodium con-
centration levels; samples must be col-
lected and analyzed annually for sys-
tems utilizing surface water sources in
whole or in part, and at least every
three years for systems utilizing solely
ground water sources. The minimum
number of samples required to be taken
by the system shall be based on the
number of treatment plants used by
the system, except that multiple wells
drawing raw water from a single aqui-
fer may, with the State approval, be
considered one treatment plant for de-
termining the minimum number of
samples. The supplier of water may be
required by the State to collect and
analyze water samples for sodium more
frequently in locations where the so-
dium content is variable.
(b) The supplier of water shall report
to EPA and/or the State the results of
the analyses for sodium within the
first 10 days of the month following the
month in which the sample results
were received or within the first 10
days following the end of the required
monitoring period as stipulated by the
State, whichever of these is first. If
more than annual sampling is required
the supplier shall report the average
sodium concentration within 10 days of
the month following the month in
which the analytical results of the last
sample used for the annual average was
received. The supplier of water shall
not be required to report the results to
EPA where the State has adopted this
regulation and results are reported to
the State. The supplier shall report the
results to EPA where the State has not
adopted this regulation,
(c) The supplier of water shall notify
appropriate local and State public
health officials of the sodium levels by
written notice by direct mail within
three months, A copy of each notice re-
quired to be provided by this paragraph
shall be sent to EPA and/or the State
within 10 days of its issuance. The sup-
plier of water is not required to notify
appropriate local and State public
health officials of the sodium levels
where the State provides such notices
in lieu of the supplier.
(d) Analyses for sodium shall be con-
ducted as directed in §141.23(k)(l).
[45 FR 57345, Aug. 27, 1980, as amended at 59
FR 62470, Dec. 5, 1994]
1141.42 Special monitoring for
corrosivity characteristics.
(a)-(c) [Reserved]
(d) Community water supply systems
shall identify whether the following
construction materials are present in
their distribution system and report to
the State:
Lead from piping, solder, caulking, interior
lining of distribution mains, alloys and
home plumbing.
Copper from piping and alloys, service lines,
and home plumbing.
Galvanized piping, service lines, and home
plumbing.
Ferrous piping- materials such as cast iron
and steel.
Asbestos cement pipe.
In addition, States may require identi-
fication and reporting of other mate-
rials of construction present in dis-
tribution systems that may contribute
contaminants to the drinking water,
such as:
Vinyl lined asbestos cement pipe.
Coal tar lined pipes and tanks.
[45 PR 57346, Aug. 27, 1980; 47 FR 10999, Mar.
12. 1982, as amended at 59 FR 62470, Dec. 5,
1994]
434
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Environmental Protection Agency
§141.50
§ 141.43 Prohibition on use of lead
pipes, solder, and flux.
(a) In general—(1) Prohibition. Any
pipe, solder, or flux, which is used after
June 19, 1986, in the installation or re-
pair of—
(i) Any public water system, or
(ii) Any plumbing in a residential or
nonresidential facility providing water
for human consumption which is con-
nected to a public water system shall
be lead free as defined by paragraph (d)
of this section. This paragraph (a)(l)
shall not apply to leaded joints nec-
essary for the repair of cast iron pipes,
(2) [Reserved]
(b) State enforcement—(!) Enforcement
of prohibition. The requirements of
paragraph (a)(l) of this section shall be
enforced in all States effective June 10,
1988, States shall enforce such require-
ments through State or local plumbing
codes, or such other means of enforce-
ment as the State may determine to be
appropriate.
(2) [Reserved]
(c) Penalties. If the Administrator de-
termines that a State is not enforcing
the requirements of paragraph (a) of
this section, as required pursuant to
paragraph (b) of this section, the Ad-
ministrator may withhold up to 5 per-
cent of Federal funds available to that
State for State program grants under
section 1443(a) of the Act.
(d) Definition of lead free. For pur-
poses of this section, the term lead
free:
(T) When used with respect to solders
and flux refers to solders and flux con-
taining not more than 0.2 percent lead:
(2) When used with respect to pipes
and pipe fittings refers to pipes and
pipe fittings containing not more than
8.0 percent lead; and
(3) When used with respect to plumb-
ing fittings and fixtures intended by
the manufacturer to dispense water for
human ingestion refers to fittings and
fixtures that are in compliance with
standards established in accordance
with 42 U.S.C. 300g^6(e).
[52 FR 20674, June 2. 1987, as amended at 65
PR 2003, Jan. 12, 2000]
Subpart F—Maximum Contami-
nant Level Goals and Max-
imum Residual Disinfectant
Level Goals
§ 141.50 Maximum contaminant level
goals for organic contaminants.
(a) MCLGs are zero for the following
contaminants:
(1) Benzene
(2) Vinyl chloride
(3) Carbon tetrachloride
(4) 1,2-dichloroethane
(5) Trichloroethylene
(6) Acrylamide
(7) Alachlor
(8) Chlordane
(9) Dibromoehloropropane
(10) 1,2-Dichloro propane
(11) Epichlorohydrin
(12) Ethylene dibromide
(13) Heptaehlor
(14) Heptaehlor epoxide
(15) Pentachlorophenol
(16) Polychlorinated biphenyls
(POBs)
(17) Tetrachloroethylene
(18) Toxaphene
(19) Benzo[a]pyrene
(20) Dichloromethane (methylene
chloride)
(21) Di(2-ethylhexyl)phthalate
(22) Hexachlorobenzene
(23) 2,3,7,8-TCDD (Dioxin)
(b) MCLGs for the following contami-
nants are as indicated:
(1) 1,1-Dichiofoethylene
(2) 1,1,1-Trichioroelhane
(3) para-Dichiorobenzene
(4) Aldicarb
(5) Aldicarb suifoxide
(8) Aldicarb sulfone .
(7) Atrazine
(8) Carbofuran
(9) 0-Dichlorobenzene
(10) cis-1.2-Dichloroethyiene
(11) trans-I.S-DichloroeShylene
(12J2.4-D
(13) Ethylbenzene
(14) Lindane
(15) Methoxychlor
(16) Monochiorobenzene
(17) Styrene
(18) Toluene
(19)2,4,5-TP
(20) Xylenes (total)
(21) Dalapon
(22) Di{2-ethylhexyl)adipate
(23) Dinoseb
(24) Diquat
(25) Endothall
0.007
0.20
0.075
0.001
0,001
0.001
0.003
0.04
0.6
0.07
0.1
0.0?
0.7
0.0002
0.04
0.1
0.1
1
0.05
10
0.2
.4
.007
.02
.1
435
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§141.51
(26) Endrin
(27) Glyphosate .
(28) Hexaehiorocyclopentadlen
(29) Oxamyl (Vydate)
(30) Pidorarn
(31) Simazine
(32) 1.2.4-Trichlorobenzene ....
(33) 1,1,2-Trichloroethane
-002
.7
-05
.2
.5
,004
,07
-003
[50 FR 46901. Nov. 13, 1985, as amended at 52
FB 20674, June 2, 1987; 52 FR 25716, July 8,
1987; 56 FR 3592, Jan. 30. 1991; 56 FR 30280,
July 1, 1991; 57 FR 31846. July 17, 1992]
§ 141.51 Maximum contaminant level
goals for inorganic contaminants.
(a) [Reserved]
(b) MCLGs for the following contami-
nants are as indicated:
Contaminant
Antimony
Arsenic .
Asbestos
Barium
Beryllium
Cadmium
Chromium
Copper
Cyanide (as free Cyanide)
Fluoride
Lead
Mercury
Nitrate
Nitrite
Total Nitrate+Nitrite
Selenium
Thallium
* This value for arsenic is effective January 23, 2006. Untii
then, there is no MCLG.
[50 FR 47155, No¥, 14, 1985, as amended at. 52
FR 20674, June 2, 1987; 86 FR 3593, Jan. 30,
1991: 56 FR 26548, June 7, 1991: 56 FB 30280,
July 1, 1991; 57 FR 31846, July 17, 1992: 60 FR
33932, June 29, 1995; 66 FR 7063, Jan. 22, 2Q01]
§141.52 Maximum contaminant level
goals for microbiological contami-
nants.
MCLGs for the following contami-
nants are as indicated:
MCLG (mg/l)
0.006
zero1
7 Million fibers/liter
(longer than 10 um).
2
.004
0.005
0,1
1,3
,2
4,0
zero
0.002
10 (as Nitrogen).
1 (as Nitrogen).
10 (as Nitrogen),
0,05
,0005
Contaminant
MCLG
(1) Giardia larnblia ,.. zero
(2) Viruses zero
(3) Leglonella zero
(4) Total conforms (including fecal coliforms ; zero.
and Escherichia coli}.
(5) Cryptosporidium | zero.
40 CFR Ch, I (7-1-04 Edition)
§ 141.53 Maximum contaminant level
goals for disinfection byproducts.
MOLGs for the following1 disinfection
byproducts are as indicated:
Disinfection byproduct
Bromodlchioromethane „,.„„.„, ., «,«.„..,„,. ,.
Bromate ,.,., , ,...,,.,,,..,,
Chlorite .....
Dibromochbromethane ,.,.,.,.,.,.,.,.„,..,.....,...,...,.,.,,,.
MCLG
(mg/L)
Zero
Zero
0,3
0.8
0.08
[63 FR 69465, Dec. 16, 1998, as amended at 65
FR 34405, May 30, 2000]
§ 141.54 Maximum residual disinfect-
ant level goals for disinfectants.
MRDLGs for disinfectants are as fol-
lows:
Disinfectant residual
Chlorine
Chloramines
Chlorine dioxide
[63 FR 69465, Dec. 16, 1998]
8141.55 Maximum contaminant level
goals for radiomiclides.
MCLGs for radionuclides are as indi-
cated in the following table;
Contaminant
1. Combined radium-226 and radium-228
2, Gross alpha particle activity (excluding radon
and uranium),
3. Beta particle and photon radioactivity
4, Uranium
MCLG
Zero.
Zero.
: Zero.
Zero.
[54 FR 27527, 27566, Jwie 29, 1889; 55 FR 25064,
June 19. 1990: 63 FR 69515, Dec. 16. 1998]
[65 FR 76748, Dec. 7, 2000]
Subpart G—National Primary
Drinking Water Regulations:
Maximum Contaminant Levels
and Maximum Residual Dis-
infectant Levels
§ 141.60 Effective dates.
(a) The effective dates for §141.61 are
as follows:
(1) The effective date for paragraphs
(a)(l) through (a)(8) of §141.61 is Janu-
ary 9, 1989.
(2) The effective date for paragraphs
(a)(9) throug-h (a)(18) and (c)(l) through
(c)(18) of §141.61 is July 30. 1992.
436
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Environmental Protection Agency
(3) The effective date for paragraphs
(a)(19) through (a)(21), (c)(19) through
(c)(25), and (cX27) through (c)(33) of
§141,61 is January 17,1994, The effective
date of §141.61(0X26) is August 17, 1992.
(b) The effective dates for §141.62 are
as follows:
(1) The effective date of paragraph
(b)(l) of §141.62 is October 2.1987.
(2) The effective date for paragraphs
(b)(2) and (b)(4) through (b)(10) of
§141.62 is July 30, 1992.
(3) The effective date for paragraphs
(b)(ll) through (b)(15) of 1141.62 is Janu-
ary 17, 1994.
§141.61
(4) The effective date for §141.62(b)(16)
is January 23, 2006.
[56 PR 3593, Jaa, 30, 1991, as amended at 57
FB 31846. July 17, 1992; 59 FB 34324. July 1.
1994; 66FB 7063, Jan. 22, 2001]
§ 141.61 Maximum contaminant levels
for organic contaminants.
(a) The following maximum contami-
nant levels for organic contaminants
apply to community and non-transient,
non-community water systems.
CAS No.
Contaminant
(1) 75-01-4 ...............,..,«,„.,...,.-.........,,,.,..,,..........-
(2) 71—43-2
(3) 56 23-5
(4) 107-06-2 .. .,..„„ ... ,
(5) 79-01-8 .. .........
(6) 106-46-7 ..,....,..„„.,.,........
(7) 75-35-4 ,.,.,,„,.,.„ ,
(8) 71 55-6
(9) 156-59-2 ..
(10) 78-87-5 ,
(11) 100-41-4
(12) 108-90-7
(13) 95-50-1
(14) 100-42-5
(15) 127-18-4 ,,,,,,,.,...,
(16) 108-83-3 ,...,.
(17) 156-60-5 ,.,.,.,
(18) 1330-20-7
(19> 75 09 2
(20) 120-82-1
(21) 79-00-5 .,...,,,.,..,.,...
Vinyl chloride ..,.«.,..,...,.........,.,.„...,...,.... ,.,.,.,.,.
Benzene ...,.,,,..,,,,,,,.,. ,.,.,.,,.,,, ,....,,. ...... ...........
1.2-DiehiQfoethane ,,,,,.., ...,,,,.,,,,..,,
Trichioroethylene ........ ...,..,,.,
para-Dichlorobenzene ........................... ,
1,1-DichloroethyIene , ,.,.„„.,.,...,...,. ,...,.,...,...
cis~1,2-Dichtoroethylene ,,.,.
1 ,2-Dichioropropane ,..............,.,.,.,.,.. ,...,.,,<,.,.
Ethylbenzene ,..,.,.,.,....,. ,.,.,.,.,, .
Monochlorobenzsne ....,,.. .,,,.,,,,. . . .
o-DJchtorobenzene ...,,...,......_
Styrene .. . ............
Tetrachloroethylene .......................... ............. ........ .
Toluene
trans- 1s2-D)ch!oro8thyiene .„ ,,.,,,..,,,..
Xyienes (tola!) .,.,.,..,,..,„. , .,,.
1,1,2-Trichloro- ethane ............... ...... . .. . . ,,.
MCL {mg/1)
0.002
0.005
0.005
0,005
0.005
0075
0.007
0.2
0.07
0.005
0.7
0.1
0.6
0.1
0.005
1
0.1
10
0.005
.07
.005
(b) The Administrator, pursuant to
section 1412 of the Act, hereby identi-
fies as indicated in the Table below
granular activated carbon (GAO),
packed tower aeration (PTA), or oxida-
tion (OX) as the best technology treat-
ment technique, or other means avail-
able for achieving compliance with the
maximum contaminant level for or-
ganic contaminants identified in para-
graphs (a) and (c) of this section:
BAT FOR ORGANIC CONTAMINANTS LISTED IN § 141.61 (a) AND (c)
CAS No. Contaminant i GAC
15972-60-8
116-06-3 ....
1646-88-4 ..
1646-67-3 ..
1912-24-9 ..
71-43-2
50-32-8
1563-66-2 ..
56-23-5
57-74-9
75-99-0
94-75-7
103-23-1 ....
117-81-7 ....
96-12-8
95-50-1
106-46-7 ....
] Aiachlor
! Aldicarb
. Aldicarb sulfone
j AWicarb sulfoxide
Atrazine
Benzene
6enzo[a]pyrene
Carbofuran ,-
: Cartoon tetrachloride
Chlordane
Dalapon
2.4-D
Di (2-ethylhexyl) adipate
Di (2-ethylhexyi) phthalate
Didromochloropropane (DBCP)
i o-Dichlorobenzene
I para-Dreri!orobenzene -
PTA
OX
437
-------
§141.61
40 CFR Ch, I (7-1-04 Edition)
BAT FOR ORGANIC CONTAMINANTS LISTED IN § 141.61 (a) AND (c)—Continued
CAS No.
io?-o6-2 :
75-35-1
156-59-2
156-60-5
75-09-2
78-87-5
88-85-7
85-00-7 ,. .
145-73-3
72 20-8
100-41-4
106-93-4
1071-83-6
76-44-8
1024-57-3
118-74-1
77-47-3
58-89-9
72-43-5 -
108-90-7
23135-22-0
87-86-5
1918 02 1
1336-36-3
122-34-9
100-42-5
1746-01-6
127-18-4
108-88-3
8001-35-2
93-72-1
120-82-1
71 55-6
79-00-5
79-01-6
75-01-4
1330-20-7
Contaminant j GAC PTA OX
1,2-Dichloroethane I X ! X. !
1.1-Dichloroethytene ' X ! X
cis-1.2-Dichloroethylene j X X
trans- 1.2-Dichloroethylene X X
Dichloromethane X
1 ,2-Dlchloropropane X j X
Dinoseb ! X ! .. ;
Diquat ' X : .
Endolhall X i
Ethylbenzene X [ X
Ethyiene Dibromide (EDB) X I X |
Gyiphosate , • : • X
Heptachlor j X
Heptachior epoxide X
Hexachlorobenzene i X i '
Hexacnlorocyelopensadiene X i X *
Lindane [ X I \
Methoxychlor : X ; •
Monochlorobenzene X j X
Oxamyl (Vydate) X
Pentachlorophenol i X :
Poiychlorinated biphenyls (PCS) X I
Slmazine . • X '
Styrene X X
2,3,7.8-TCDD (Dioxin) X
Tefrachloroethylene X > X
Toluene j X j X
Toxaphene X I
24,5-TP (Silvex) .... ... X
1 ,2.4-Trichlorobenzene X X
1 1,1-Trichloro9thane .... X ! X
Trichloroethylene j X j X
Vinyl chloride I X
Xyiene X X
(c) The following maximum contami-
nant levels for synthetic organic con-
taminants apply to community water
systems and non-transient,
munity water systems:
non-com-
CAS No.
(1) 1S972-60-8
(2)116-06-3 . .
(3) 1646-87-3
(4) 1646-87 4
(5) 1912-24-9
(6) 1563-66-2
(7) 57-74-9
(8) 96-12-8
(9) 94-75-7
(10) 106-93-4 . .
(11) 76-44-8
(12) 1024-57-3
(13) 58-89-9 .
(14) 72-43 5
(15) 1336-36-3
(16) 87-86-5
(17) 8001-35-2
(18) 93-72-1
(19) 50-32-8
(20) 75-99-0 .. . .
(21) 103-23-1
(22) 117-81-7
(23) 88-85-7 .
(24) 85-00-7
(25) 145-73-3
Contaminant
Alachlor
Carbofuran
2 4-D
Hepfachlor
Heptachlor epoxide
Pentachiorophenol
Toxaphene
2,4,5-TP
Di(2-ethylhexy!) adipate ... .
Di(2-ethylhexyl) phtnalate
Diquat
Endothall
MCL (mo/1)
0.002
0.003
0004
0002
0.003
0.04
0002
0.0002
007
0.00005
0.0004
0.0002
0.0002
004
00005
0.001
0.003
0.05
0.0002
0.2
04
0.006
0.007
0.02
0.1
438
-------
(Environmental Protection Agency
CAS No.
jcy
Contaminant
..... | Endrin „....„....„..,..„....„„..„..„.....„..,..„...„....
,.,., j Glyphosate ,....,,.,.,.,...„...,,.,..,.,.,.„ ,. . .............
..... I Hexacholorbenzene „.,,.,.,,,.,.„,„„,.„,..,.,.. „.,.
..... Hexachlorocyclopentadiene ............................
..„. | Oxamyi (Vydafe) „.„,„„.„..„...„„. ., „...
..-,. [ Pidoram ,.,..„,..,,,. ,.,,,
,,.., | Simazine .,,.,,,,,,,.,,,..,., „ ,.,...,.,.,
..... j 2.3.7-8-TCDD (Dioxin) ................. .. .... .........
§141.62
MCL jmg/l)
! 0.002
] 07
: 0.001
! 0.05
! 0.2
! 0.5
: 0.004
; .3*10-*
[56 FR 3593. Jan. 30, 1991, as amended at 56 FR 30280, July 1, 1991; 57 FR 31846. July 17. 1992:
59 FR 34324, July 1, 1994]
§ 141.62 Maximum contaminant
for inorganic contaminants.
(a) [Reserved]
(b) The maximum contaminant levels
for inorganic contaminants specified in
paragraphs (b) (2)-(6), (b)(10), and (b)
(lli-(18) of this section apply to com-
munity water systems and non-tran-
sient, non-community water systems.
The maximum contaminant level spec-
ified in paragraph (b)(l) of this section
only applies to community water sys-
tems. The maximum contaminant lev-
els specified in (bH7), (b)<8), and (b)(9'i
of this section apply to community
water systems: non-transient, non-
community water systems; and tran-
sient non-community water systems.
BAT FOR INORGANIC COMPOUNDS L;SFED IN
SECTION I41.62{b)
BATSs'i
Contaminant
(1* Fluoride -. .-
(2) Asbestos
(3) Barium
(4) Cadmium
(5) Chromium
i6) Mercury
(?) Nitraie
(Si Nitrite
(9) Total Nitrate and Nitrite .
(10) Selenium
(11} Antimony
(12) Beryllium
{13} Cyanide (as free Cya-
nide).
(14) (Reserved].
HS) Thallium
(16) Arsenic
? Million Fibers-liter (longer
than 10 ,um).
2
0.005
0.1
0.002
10 (as Nitrogen)
1 (as Nitrogen)
10 (as Nitrogen)
0.05
0.006
0.004
0.2
0.002
0.010
(c) The Administrator, pursuant to
section 1412 of the Act, hereby identi-
fies the following as the best tech-
nology, treatment technique, or other
means available for achieving compli-
ance with the maximum contaminant
levels for inorganic contaminants iden-
tified in paragraph (b) of this section,
except fluoride:
Asbestos .
Barium ....
Beryllium .
Cadmium
Chromium
Cyanide ..
Mercury . .
Nickel
Nitrate ....
Nitrite-
Selenium .
Thallium .,
1 BAT only i' influent Hg concentrations <1Qyg/1.
2 BAT for Chromium W only.
3 BAT tor Selenium IV only.
4 BATs for Arsenic V. Pre-oxidation may be required to oon-
vert Arsenic III to Arsenic V.
'' To obtain high removals, iron to arsenic ratio must be at
least 20:1.
Key to BATS in Table
l=Activatert Alumina
2 - Coagulation/Filtration (not BAT for sys-
tems < 500 service connections)
2=Coagulation'Filtration
3=Direct and Diatomite Filtration
4=Granular Activated Carbon
5~Ion Exchange
6 = Lime Softening (not BAT for systems
< 500 service connections)
7=Reversc Osmosis
8=Corrosion Control
9=Blectrodialysi3
10=Chlorine
ll=Ultraviolet
12 = Oxidation/Filtration
(d) The Administrator, pursuant to
section 1412 of the Act, hereby identi-
fies in the following table the afford-
able technology, treatment technique.
or other means available to systems
serving 10,000 persons or fewer for
achieving' compliance with the max-
imum contaminant level for arsenic;
439
203-160 D-15
-------
§141.63
40 CFR Ch. I (7-1-04 Edition)
SMALL SYSTEM COMPLIANCE TECHNOLOGIES
(SSCTs)1 FOR ARSENIC 2
Small system compliance
technology
Activated Alumina (central-
ized).
Activated Alumina (Point-of-
Use)4.
Coagulation/Filtration5
Coagulation-assisted Micro-
filtration.
Electrodialysis reversal6
Enhanced coagulation/filtra-
tion.
Enhanced lime softening
(pH> 10.5).
Ion Exchange
Lime Softening5
Oxidation/Filtration7
Reverse Osmosis (central-
ized)6.
Reverse Osmosis (Point-of-
Use)4.
Affordable for listed small
system categories 3
All size categories.
All size categories.
501-3,300, 3,301-10,000.
501-3,300, 3,301-10,000.
501-3,300, 3,301-10,000.
All size categories
All size categories.
All size categories.
501-3,300, 3,301-10,000.
All size categories.
501-3,300, 3,301-10,000.
All size categories.
'Section 1412(b)(4)(E)(ii) of SDWA specifies that SSCTs
must be affordable and technically feasible for small systems.
2 SSCTs for Arsenic V. Pre-oxidation may be required to
convert Arsenic III to Arsenic V.
3The Act (ibid.) specifies three categories of small systems:
(i) those serving 25 or more, but fewer than 501, (ii) those
serving more than 500, but fewer than 3,301, and (iii) those
serving more than 3,300, but fewer than 10,001.
4When POU or POE devices are used for compliance, pro-
grams to ensure proper long-term operation, maintenance,
and monitoring must be provided by the water system to en-
sure adequate performance.
5 Unlikely to be installed solely for arsenic removal. May re-
quire pH adjustment to optimal range if high removals are
needed.
6 Technologies reject a large volume of water—may not be
appropriate for areas where water quantity may be an issue.
7 To obtain high removals, iron to arsenic ratio must be at
least 20:1.
[56 FR 3594, Jan. 30, 1991, as amended at 56
FR 30280, July 1, 1991; 57 FR 31847. July 17,
1992; 59 FR 34325, July 1, 1994; 60 FR 33932.
June 29, 1995; 66 FR 7063, Jan. 22. 2001; 68 FR
14506, Mar. 25, 2003]
EFFECTIVE DATE NOTE: At 69 FR 38855, June
29, 2004, §141.62(0) was amended in the Table
"BAT FOR INORGANIC COMPOUNDS LIST-
ED IN SECTION 141.62(b)" in the entry for
"cyanide" by replacing the "10" with "13"; and
in the list "Key to BATS in Table", by adding
to the end of the list, "13 = Alkaline
Chlorination (pH > 8.5)", effective July 29,
2004.
§ 141.63 Maximum contaminant levels
(MCLs) for microbiological contami-
nants.
(a) The MCL is based on the presence
or absence of total coliforms in a sam-
ple, rather than coliform density.
(1) For a system which collects at
least 40 samples per month, if no more
than 5.0 percent of the samples col-
lected during a month are total coli-
form-positive, the system is in compli-
ance with the MCL for total coliforms.
(2) For a system which collects fewer
than 40 samples/month, if no more than
one sample collected during a month is
total coliform-positive, the system is
in compliance with the MCL for total
coliforms.
(b) Any fecal coliform-positive repeat
sample or E. coK-positive repeat sam-
ple, or any total coliform-positive re-
peat sample following a fecal coliform-
positive or E. co/i-positive routine sam-
ple constitutes a violation of the MCL
for total coliforms. For purposes of the
public notification requirements in
subpart Q, this is a violation that may
pose an acute risk to health.
(c) A public water system must deter-
mine compliance with the MCL for
total coliforms in paragraphs (a) and
(b) of this section for each month in
which it is required to monitor for
total coliforms.
(d) The Administrator, pursuant to
section 1412 of the Act, hereby identi-
fies the following as the best tech-
nology, treatment techniques, or other
means available for achieving compli-
ance with the maximum contaminant
level for total coliforms in paragraphs
(a) and (b) of this section:
(1) Protection of wells from contami-
nation by coliforms by appropriate
placement and construction;
(2) Maintenance of a disinfectant re-
sidual throughout the distribution sys-
tem;
(3) Proper maintenance of the dis-
tribution system including appropriate
pipe replacement and repair proce-
dures, main flushing programs, proper
operation and maintenance of storage
tanks and reservoirs, and continual
maintenance of positive water pressure
in all parts of the distribution system;
(4) Filtration and/or disinfection of
surface water, as described in subpart
H, or disinfection of ground water
using strong oxidants such as chlorine,
chlorine dioxide, or ozone; and
(5) For systems using ground water,
compliance with the requirements of
an EPA-approved State Wellhead Pro-
tection Program developed and imple-
mented under section 1428 of the
SDWA.
[54 FR 27566, June 29, 1989; 55 FR 25064, June
19, 1990, as amended at 65 FR 26022, May 4,
2000]
440
-------
Environmental Protection Agency
§ 141.64 Maximum contaminant levels
for disinfection byproducts.
(a) The maximum contaminant levels
(MCLs) for disinfection byproducts are
as follows:
Disinfection byproduct
Total trihalomethanes (TTHM)
Bromate
Chlorite
MCL
(mg/L)
0.080
0060
0.010
1.0
(b) Compliance dates. (1) CWSs and
NTNCWSs. Subpart H systems serving
10,000 or more persons must comply
with this section beginning January 1,
2002. Subpart H systems serving fewer
than 10,000 persons and systems using
only ground water not under the direct
influence of surface water must comply
with this section beginning January 1,
2004.
(2) A system that is installing GAG
or membrane technology to comply
with this section may apply to the
State for an extension of up to 24
months past the dates in paragraphs
(b)(l) of this section, but not beyond
December 31. 2003. In granting the ex-
tension, States must set a schedule for
compliance and may specify any in-
terim measures that the system must
bake. Failure to meet the schedule or
interim treatment requirements con-
stitutes a violation of a National Pri-
mary Drinking- Water Regulation.
(c) The Administrator, pursuant to
Section 1412 of the Act, hereby identi-
fies the following as the best tech-
nology, treatment techniques, or other
means available for achieving compli-
ance with the maximum contaminant
levels for disinfection byproducts iden-
tified in paragraph (a) of this section:
Disinfection
byproduct
Best available technology
Enhanced coagulation or enhanced softening
or GAC10, with chlorine as the primary and
residual disinfectant
HAAS Enhanced coagulation or enhanced softening
Of GAC10, with chlorine as the primary and
i residual disinfectant.
Bromate .... Control of ozone treatment process to reduce
j production of bromate.
Chlorite Control of treatment processes to reduce dis-
infectant demand and control of disinfection
treatment processes to reduce disinfectant
levels.
§141.66
[63 FR 69465. Dec. 16, 1998. as amended at 66
FR 3776, Jan. 16, 2001]
§ 141.65 Maximum residual disinfect-
ant levels.
(a) Maximum residual disinfectant
levels (MRDLs) are as follows:
Disinfectant residua!
Chlorine
Chloramines
Chlorine dioxide
S MRDL (mg/L)
4.0 (as cy.
4,0 (as cy.
0.8 (as CIO,).
(b) Compliance dates. (1) CWSs and
NTNCWSs. Subpart H systems serving
10,000 or more persons must comply
with this section beginning January 1.
2002. Subpart H systems serving fewer
than 10,000 persons and systems using
only ground water not under the direct
influence of surface water must comply
with this subpart beginning January 1.
2004.
(2) Transient NCWSs. Subpart H sys-
tems serving 10,000 or more persons and
using chlorine dioxide as a disinfectant
or oxidant must comply with the chlo-
rine dioxide MRDL beginning January
1, 2002. Subpart H systems serving-
fewer than 10,000 persons and using
chlorine dioxide as a disinfectant or
oxidant and systems using only ground
water not under the direct influence of
surface water and using chlorine diox-
ide as a disinfectant or oxidant must
comply with the chlorine dioxide
MRDL beginning January 1, 2004.
(c) The Administrator, pursuant to
Section 1412 of the Act, hereby identi-
fies the following as the best tech-
nology, treatment techniques, or other
means available for achieving compli-
ance with the maximum residual dis-
infectant levels identified in paragraph
(a) of this section: control of treatment
processes to reduce disinfectant de-
mand and control of disinfection treat-
ment processes to reduce disinfectant
levels.
[63 FR 69465, Dec. 16, 1998, as amended at 66
FR 3776, Jan. 16, 2001]
§ 141.66 Maximum contaminant levels
for radionuclides.
(a) [Reserved]
(b) MCL for combined radium-226 and
-228. The maximum contaminant level
for combined radium-226 and radium-
228 is 5 pCi/L. The combined radium-226
and radiurn-228 value is determined by
441
-------
§141.66
the addition of the results of the anal-
ysis for radium-226 and the analysis for
radium-228.
(c) MCL for gross alpha particle activ-
ity (excluding radon and uranium). The
maximum contaminant level for gross
alpha particle activity (including ra-
dium-226 but excluding radon and ura-
nium) is 15 pCi/L.
(d) MCL for beta particle and photon
radioactivity. (1) The average annual
concentration of beta particle and pho-
ton radioactivity from man-made
radionuclides in drinking- water must
not produce an annual dose equivalent
to the total body or any internal organ
greater than 4 millirem/year (mrem/
year).
(2) Except for the radionuqlides listed
in table A, the concentration of man-
made radionuclides causing 4 mrem
total body or organ dose equivalents
must be calculated on the basis of 2
liter per day drinking water intake
using the 168 hour data list in "Max-
imum Permissible Body Burdens and
Maximum Permissible Concentrations
of Radionuclides in Air and in Water
for Occupational Exposure," NBS (Na-
tional Bureau of Standards) Handbook
69 as amended August 1963, U.S. De-
partment of Commerce. This incorpo-
ration by reference was approved by
the Director of the Federal Register in
accordance with 5 U.S.C. 552(a) and 1
CPR part 51. Copies of this document
are available from the National Tech-
nical Information Service, NTIS ADA
280 282, U.S. Department of Commerce,
5285 Port Royal Road, Springfield, Vir-
ginia 22161. The toll-free number is 800-
553-6847. Copies may be inspected at
EPA's Drinking Water Docket, 401 M
Street, SW., Washington, DC 20460; or
at the National Archives and Records
Administration (NARA). For informa-
tion on the availability of this mate-
40 CFR Ch. I (7-1-04 Edition)
rial at NARA, call 202-741-6030, or go
to: http://www.archives.gov/
federal register/
code of_Jederal regulations/
ibr locations.html. If two or more
radionuclides are present, the sum of
their annual dose equivalent to the
total body or to any organ shall not ex-
ceed 4 mrem/year.
TABLE A—AVERAGE ANNUAL CONCENTRATIONS
ASSUMED To PRODUCE: A TOTAL BODY OR
ORGAN DOSE OF 4 MREM/YR
1. Radionuclide
2. Tritium
3. Strontium-90
Critical organ .
Total body
Bone Marrow .
pCi per liter
20,000
(e) MCL for uranium. The maximum
contaminant level for uranium is 30 jig/
L.
(f) Compliance dates. (1) Compliance
dates for combined radium-226 and -228,
gross alpha particle activity, gross
beta particle and photon radioactivity,
and uranium: Community water sys-
tems must comply with the MCLs list-
ed in paragraphs (b), (c), (d), and (e) of
this section beginning December 8, 2003
and compliance shall be determined in
accordance with the requirements of
§§141.25 and 141.26. Compliance with re-
porting requirements for the radio-
nuclides under appendix A to subpart O
and appendices A and B to subpart Q is
required on December 8, 2003.
(2) [Reserved]
(g) Best available technologies (BATs)
for radionuclides. The Administrator,
pursuant to section 1412 of the Act,
hereby identifies as indicated in the
following table the best technology
available for achieving compliance
with the maximum contaminant levels
for combined radium-226 and -228, ura-
nium, gross alpha particle activity, and
beta particle and photon radioactivity.
TABLE B—BAT FOR COMBINED RADiuM-226 AND RADiuM-228, URANIUM, GROSS ALPHA PARTICLE
ACTIVITY, AND BETA PARTICLE AND PHOTON RADIOACTIVITY
Contaminant
BAT
1. Combined radium-226 and radium-228
2. Uranium
3. Gross alpha particle activity (excluding Radon and Uranium)
4. Beta particle and photon radioactivity
Ion exchange, reverse osmosis, lime softening.
Ion exchange, reverse osmosis, lime softening, coagulation/fil-
tration.
Reverse osmosis.
Ion exchange, reverse osmosis.
(h) Small systems compliance technologies list for radionuclides.
442
-------
Environmental Protection Agency
§141.70
TABLE C—LIST OF SMALL SYSTEMS COMPLIANCE TECHNOLOGIES FOR RADIONUCLIDES AND
LIMITATIONS TO USE
Unit technologies
2 Point of use (POU2) IE
4 POU2 RO
6. Green sand filtration
7. Co- precipitation with Barium sulfate
8. Electrodialysis/electrodialysis rever-
sal.
oxide filtration.
Limitations
(see foot-
notes)
('')
(b)
(*•')
(b)
(d)
<<>
0)
00
(") (h)
(i)
Operator skill level required1
Basic
Basic.
Intermediate to Advanced
Basic to Intermediate
Raw water quality range and
considerations.1
filtration.
Surface waters usually require pre-
fi It ration.
Ground waters with suitable water
quality.
All ground waters.
anion concentrations may affect
regeneration frequency.
qualities.
1 National Research Council (NRC). Safe Water from Every Tap: Improving Water Service to Small Communities. National
Academy Press. Washington, D.C. 1997.
2 A POU, or "point-of-use" technology is a treatment device installed at a single tap used for the purpose of reducing contami-
nants in drinking water at that one tap. POU devices are typically installed at the kitchen tap. See the April 21, 2000 NODA for
more details.
Limitations Footnotes. Technologies for Radionuclides:
•••The regeneration solution contains high concentrations of the contaminant ions. Disposal options should be carefully consid-
ered before choosing this technology.
bWhen POU devices are used for compliance, programs for long-term operation, maintenance, and monitoring must be pro-
vided by water utility to ensure proper performance.
c Reject water disposal options should be carefully considered before choosing this technology. See other RO limitations de-
scribed in the SWTR Compliance Technologies Table.
JThe combination of variable source water quality and the complexity of the water chemistry involved may make this tech-
nology too complex for small surface water systems.
t-Removal efficiencies can vary depending on water quality.
'This technology may be very limited in application to small systems. Since the process requires static mixing, detention ba-
sins, and filtration, it is most applicable to systems with sufficiently high sulfate levels that already have a suitable filtration treat-
ment train in place.
yThis technology is most applicable to small systems that already have filtration in place.
h Handling of chemicals required during regeneration and pH adjustment may be too difficult for small systems without an ade-
quately trained operator.
'Assumes modification to a coagulation/filtration process already in place.
TABLE D—COMPLIANCE TECHNOLOGIES BY SYSTEM SIZE CATEGORY FOR RADIONUCLIDE NPDWR's
Contaminant
1. Combined radium-226 and radium-228
2. Gross alpha particle activity
3. Beta particle activity and photon activity
4. Uranium
Compliance technologies1 for system size categories
(population served)
25-500
123456789
3, 4
1, 2, 3, 4
1, 2. 4, 10, 11
501-3,300
123456789
3, 4
1, 2, 3. 4
1, 2, 3, 4, 5, 10, 11
3,300-10,000
123456789
3,4,
1, 2. 3, 4.
1, 2, 3, 4, 5, 10, 11.
Note: ' Numbers correspond to those technologies found listed in the table C of 141.66(h).
[65 FR 76748, Dec. 7. 2000]
Subpart H—Filtration and § 141.70 General requirements.
Disinfection (a) The requirements of this subpart
H constitute national primary drinking
SOURCE: 54 FR 27527, June 29. 1989, unless water regulations. These regulations
otherwise noted. establish criteria under which filtra-
tion is required as a treatment tech-
nique for public water systems supplied
by a surface water source and public
443
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§141.71
40 CFR Ch. I (7-1-04 Edition)
water systems supplied by a ground
water source under the direct Influence
of surface water. In addition, these reg-
ulations establish treatment technique
requirements in lieu of maximum con-
taminant levels for the following con-
taminants: Giardia lamblia, viruses,
heterotrophic plate count bacteria,
Legionella, and turbidity. Each public
water system with a surface water
source or a ground water source under
the direct influence of surface water
must provide treatment of that source
water that complies with these treat-
ment technique requirements. The
treatment technique requirements con-
sist of installing and properly oper-
ating water treatment processes which
reliably achieve:
(1) At least 99.9 percent (3-log) re-
moval and/or inactlvation of Giardia
lamblia cysts between a point where the
raw water is not subject to recontami-
nation by surface water runoff and a
point downstream before or at the first
customer: and
(2) At least 99.99 percent (4-log) re-
moval and'or inactivation of viruses
between a point where the raw water is
not subject to recontamination by sur-
face water runoff and a point down-
stream before or at the first customer.
(b) A public water system using a
surface water source or a ground water
source under the direct influence of
surface water is considered to be in
compliance with the requirements of
paragraph (a) of this section if:
(1) It meets the requirements for
avoiding filtration in §141.71 and the
disinfection requirements in §141.72(a):
or
(2) It meets the filtration require-
ments in §141.73 and the disinfection
requirements in §141.72(b).
(c) Each public water system using a
surface water source or a ground water
source under the direct influence of
surface water must be operated by
qualified personnel who meet the re-
quirements specified by the State.
(d) Additional requirements for systems
serving at least 10,000 people. In addition
to complying with requirements in this
subpart, systems serving at least 10,000
people must also comply with the re-
quirements in subpart P of this part.
(e) Additional requirements for systems
serving fewer than 10,000 people. In addi-
tion to complying with requirements in
this subpart, systems serving fewer
than 10,000 people must also comply
with the requirements in subpart T of
this part.
[54 PR 27527, June 29, 1989, as amended at 63
FR 69516, Dec. 16. 1998: 67 FR 1836, Jan. 14.
2002]
§ 141.71 Criteria for avoiding filtra-
tion.
A public water system that uses a
surface water source must meet all of
the conditions of paragraphs (a) and (b)
of this section, and is subject to para-
graph (c) of this section, beginning De-
cember 30, 1991, unless the State has
determined, in writing pursuant to
§1412(b)(7)(C)(iii), that filtration is re-
quired. A public water system that
uses a ground water source under the
direct influence of surface water must
meet all of the conditions of para-
graphs (a) and (b) of this section and is
subject to paragraph (c) of this section,
beginning 18 months after the State de-
termines that it is under the direct in-
fluence of surface water, or December
30, 1991, whichever is later, unless the
State has determined, in writing pursu-
ant to §1412(b)(7}(C)(iii), that filtration
is required. If the State determines in
writing pursuant to §1412(b)(7)(C)(iii)
before December 30. 1991, that filtra-
tion is required, the system must have
installed filtration and meet the cri-
teria for filtered systems specified in
§§141.72(b) and 141.73 by June 29, 1993.
Within 18 months of the failure of a
system using surface water or a ground
water source under the direct influence
of surface water to meet any one of the
requirements of paragraphs (a) and (b)
of this section or after June 29, 1993,
whichever is later, the system must
have installed filtration and meet the
criteria for filtered systems specified
in §§141.72(b) and 141.73.
(a) Source water quality conditions. (1)
The fecal coliform concentration must
be equal to or less than 20/100 ml, or the
total coliform concentration must be
equal to or less than 100/100 ml (meas-
ured as specified in §141.74 (a) (1) and
(2) and (b)(D), in representative sam-
ples of the source water immediately
prior to the first or only point of dis-
infectant application in at least 90 per-
cent of the measurements made for the
444
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Environmental Protection Agency
§141.71
6 previous months that the system
served water to the public on an ongo-
ing basis. If a system measures both
fecal and total coliforms, the fecal coli-
form criterion, but not the total coli-
form criterion, in this paragraph must
be met.
(2) The turbidity level cannot exceed
5 NTU (measured as specified in §141.74
(a)(4) and (b)(2)) in representative sam-
ples of the source water immediately
prior to the first or only point of dis-
infectant application unless: (i) the
State determines that any such event
was caused by circumstances that were
unusual and unpredictable; and (ii) as a
result of any such event, there have
not been more than two events in the
past 12 months the system served
water to the public, or more than five
events in the past 120 months the sys-
tem served water to the public, in
which the turbidity level exceeded 5
NTU. An "event" is a series of consecu-
tive days during which at least one tur-
bidity measurement each day exceeds 5
NTU.
(b) Site-specific conditions. (l)(i) The
public water system must meet the re-
quirements of §141.72(a)(l) at least 11 of
the 12 previous months that the system
served water to the public, on an ongo-
ing- basis, unless the system fails to
meet the requirements during 2 of the
12 previous months that the system
served water to the public, and the
State determines that at least one of
these failures was caused by cir-
cumstances that were unusual and un-
predictable.
(ii) The public water system must
meet the requirements of §141.72(a)(2)
at all times the system serves water to
the public.
(iii) The public water system must
meet the requirements of §141.72(a)(3)
at all times the system serves water to
the public unless the State determines
that any such failure was caused by
circumstances that were unusual and
unpredictable.
(iv) The public water system must
meet the requirements of §141.72(a)(4)
on an ongoing basis unless the State
determines that failure to meet these
requirements was not caused by a defi-
ciency in treatment oi the source
water.
(2) The public water system must
maintain a watershed control program
which minimizes the potential for con-
tamination by Giardia lamblia cysts and
viruses in the source water. The State
must determine whether the watershed
control program is adequate to meet
this goal. The adequacy of a program
to limit potential contamination by
Giardia lamblia cysts and viruses must
be based on: the comprehensiveness of
the watershed review; the effectiveness
of the system's program to monitor
and control detrimental activities oc-
curring in the watershed; and the ex-
tent to which the water system has
maximized land ownership and/or con-
trolled land use within the watershed.
At a minimum, the watershed control
program must:
(i) Characterize the watershed hy-
drology and land ownership;
(ii) Identify watershed characteris-
tics and activities which may have an
adverse effect on source water quality;
and
(iii) Monitor the occurrence of activi-
ties which may have an adverse effect
on source water quality.
The public water system must dem-
onstrate through ownership and/or
written agreements with landowners
within the watershed that it can con-
trol all human activities which may
have an adverse impact on the micro-
biological quality of the source water.
The public water system must submit
an annual report to the State that
identifies any special concerns about
the watershed and how they are being
handled; describes activities in the wa-
tershed that affect water quality; and
projects what adverse activities are ex-
pected to occur in the future and de-
scribes how the public water system
expects to address them. For systems
using a ground water source under the
direct influence of surface water, an
approved wellhead protection program
developed under section 1428 of the Safe
Drinking Water Act may be used, if the
State deems it appropriate, to meet
these requirements.
(3) The public water system mast be
subject to an annual on-site inspection
to assess the watershed control pro-
gram and disinfection treatment proc-
ess. Either the State or a party ap-
proved by the State must conduct the
445
-------
§141.72
40 CFR Ch. I (7-1-04 Edition)
cm-site inspection. The inspection must
be conducted by competent individuals
such as sanitary and civil engineers,
sanitarians, or technicians who have
experience and knowledge about the
operation and maintenance of a public
water system, and who have a sound
understanding of public health prin-
ciples and waterborne diseases. A re-
port of the on-site Inspection summa-
rizing all findings must be prepared
every year. The on-site inspection
must indicate to the State's satisfac-
tion that the watershed control pro-
gram and disinfection treatment proc-
ess are adequately designed and main-
tained. The on-site Inspection must in-
clude:
(i) A review of the effectiveness of
the watershed control program;
(ii) A review of the physical condi-
tion of the source intake and how well
it is protected;
(iii) A review of the system's equip-
ment maintenance program to ensure
there is low probability for failure of
the disinfection process;
(iv) An inspection of the disinfection
equipment for physical deterioration;
(v) A review of operating" procedures;
(vi) A review of data records to en-
sure that all required tests are being
conducted and recorded and disinfec-
tion is effectively practiced; and
(vii) Identification of any improve-
ments which are needed in the equip-
ment, system maintenance and oper-
ation, or data collection.
(4) The public water system must not
have been identified as a source of a
waterborne disease outbreak, or if it
has been so identified, the system must
have been modified sufficiently to pre-
vent another such occurrence, as deter-
mined by the State.
(5) The public water system must
comply with the maximum contami-
nant level (MCL) for total coliforms in
§141.63 at least 11 months of the 12 pre-
vious months that the system served
water to the public, on an ongoing
basis, unless the State determines that
failure to meet this requirement was
not caused by a deficiency in treat-
ment of the source water.
(6) The public water system must
comply with the requirements for
trihalomethanes in §§141.12 and 141.30
until December 31, 2001. After Decem-
ber 31, 2001, the system must comply
with the requirements for total
trihalomethanes, haloacetic acids
(five), bromate, chlorite, chlorine,
chloramines, and chlorine dioxide in
subpart L of this part.
(c) Treatment technique violations, (1)
A system that (i) fails to meet any one
of the criteria in paragraphs (a) and (b)
of this section and/or which the State
has determined that filtration is re-
quired, in writing pursuant to
§1412(b)(7)(C)(iii), and (ii) fails to in-
stall filtration by the date specified in
the introductory paragraph of this sec-
tion is in violation of a treatment tech-
nique requirement.
(2) A system that has not installed
filtration is in violation of a treatment
technique requirement if:
(1) The turbidity level (measured as
specified in §141.74(a)(4) and (b)(2)) in a
representative sample of the source
water immediately prior to the first or
only point of disinfection application
exceeds 5 NTU; or
(ii) The system is identified as a
source of a waterborne disease out-
break.
[54 PR 27527, June 29, 1989, as amended at 63
PR 69516, Deo. 16, 1998; 66 FR 3776. Jan. 16,
2001]
EFFECTIVE DATE NOTE: At 69 FR 38855, June
29, 2004, §141.71 was amended in paragraph
(a)(2) introductory text by removing' the ci-
tation "§141.74(a)(4)" and adding in its place
"§141.74(a)(l)" and in paragraph (e)(2)(i) by re-
moving the citation "§ 141.74(a)(4)" and adding
in its place "§141.74(a)(D". effective July 29,
2004.
§ 141.72 Disinfection.
A public water system that uses a
surface water source and does not pro-
vide filtration treatment must provide
the disinfection treatment specified in
paragraph (a) of this section beginning
December 30, 1991, unless the State de-
termines that filtration is required in
writing pursuant to §1412 (b)(7)(C)(iii).
A public water system that uses a
ground water source under the direct
influence of surface water and does not
provide filtration treatment must pro-
vide disinfection treatment specified in
paragraph (a) of this section beginning
December 30, 1991, or 18 months after
the State determines that the ground
water source is under the influence of
446
-------
Environmental Protection Agency
§141.72
surface water, whichever is later, un-
less the State has determined that fil-
tration is required in writing pursuant
to §1412(b)(7)(C)(iii). If the State has
determined that filtration is required,
the system must comply with any in-
terim, disinfection requirements the
State deems necessary "before filtration
is installed. A system that uses a sur-
face water source that provides filtra-
tion treatment must provide the dis-
infection treatment specified in para-
graph (b) of this section beglnnng June
29. 1993. or beginning when filtration is
installed, whichever is later. A system
that uses a ground water source under
the direct influence of surface water
and provides filtration treatment must
provide disinfection treatment as spec-
ified in paragraph (b) of this section by
June 29, 1993, or beginning when filtra-
tion is installed, whichever is later.
Failure to meet any requirement of
this section after the applicable date
specified in this introductory para-
graph Is a treatment technique viola-
tion.
(a) Disinfection requirements for public
water systems that do not provide filtra-
tion. Each public water system that
does not provide filtration treatment
must provide disinfection treatment as
follows:
(1) The disinfection treatment must
be sufficient, to ensure at least 99.9 per-
cent (3-log) inactivation of Giardia
lamblia cysts and 99.99 percent (4-log)
inactivation of viruses, every day the
system serves water to the public, ex-
cept any one day each month. Each day
a system serves water to the public.
the public water system must calculate
the CT value(s) from the system's
treatment parameters, using the proce-
dure specified in §141.74(b)<3), and de-
termine whether this valuers) is suffi-
cient to achieve the specified inactiva-
tion rates for Giardia lamblia cysts and
viruses. If a system uses a disinfectant
other than chlorine, the system may
demonstrate to the State, through the
use of a State-approved protocol for on-
site disinfection challenge studies or
other information satisfactory to the
State, that CT
-------
§141.73
40 CFR Ch. I (7-1-04 Edition)
not detected and where the HPC is >5QO/ml;
and
e=number of instances where the residual
disinfectant concentration is not measured
and HPC is >500/ml.
(ii) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory under the requisite
time and temperature conditions speci-
fied by §141.74(a)(3) and that the sys-
tem is providing adequate disinfection
in the distribution system, the require-
ments of paragraph (a)(4)(i) of this sec-
tion do not apply to that system.
(b) Disinfection requirements for public
water systems which provide filtration.
Each public water system that provides
filtration treatment must provide dis-
infection treatment as follows.
(1) The disinfection treatment must
be sufficient to ensure that the total
treatment processes of that system
achieve at least 99.9 percent (3-log) in-
activation and/or removal of Giardia
lamblia cysts and at least 99.99 percent
(4-log) inactivation and/or removal of
viruses, as determined by the State.
(2) The residual disinfectant con-
centration in the water entering the
distribution system, measured as speci-
fied in §141.74 (a)(5) and (c)(2), cannot
be less than 0.2 mgr/1 for more than 4
hours.
(3)(i) The residual disinfectant con-
centration in the distribution system,
measured as total chlorine, combined
chlorine, or chlorine dioxide, as speci-
fied in §141.74 (a)(5) and (c)(3), cannot
be undetectatale in more than 5 percent
of the samples each month, for any two
consecutive months that the system
serves water to the public. Water in the
distribution system with a
heterotrophic bacteria concentration
less than or equal to 500/ml. measured
as heterotrophic plate count (HPC) as
specified in §141.74(a)(3), is deemed to
have a detectable disinfectant residual
for purposes of determining compliance
with this requirement. Thus, the value
"V" in the following formula cannot ex-
ceed 5 percent in one month, for any
two consecutive months.
where:
a + b
a=number of instances where the residual
disinfectant concentration is measured;
b=number of instances where the residual
disinfectant concentration is not measured
but heterotrophic bacteria plate count
(HPC) is measured;
c=nttrflber of instances where the residual
disinfectant concentration is measured hut
not detected and no HPC is measured;
d=nnmber of instances where no residual dis-
infectant concentration is detected and
where the HPC is >50Q/ml; and
e=number of instances where the residual
disinfectant concentration is not measured
and HPC is >500/ml.
(ii) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory under the requisite
time and temperature conditions speci-
fied in § 141.74(a)(3) and that the system
is providing adequate disinfection in
the distribution system, the require-
ments of paragraph (b)(3)(i) of this sec-
tion do not apply.
EFFECTIVE DATE NOTE; At 69 PR 38855. June
29, 2004, §141.72 was amended in paragraph
(a)(3) by removing the citation "§141.74(a)(5)"
and adding in its place "§141.74(a)(2)"; in
paragraph (a)(4)(i) by removing the citation
"§ 141.74(a)(5)" and adding in its place
"§ 141,74(a)(2)" and by removing the citation
"§ 141.74(a)(3)" and adding in its place
"§141.74('a)(l)"; m paragraph (a)(4)(ii) by re-
moving the citation "§ 141.74(a}(3}" and adding
in its place "§141,74(a)(D"; in paragraph (b)(2)
by removing- the citation "§141.74(a)(5)" and
adding in its place "§141.74(,a)(2)"; in para-
graph (b)(3)(i) by removing the citation
"§141.74(a)(5>" and adding in its place
"|141.74(a)(2)" and by removing the citation
"§141.74(a)(3)" and adding in its place
"§141.74(a)(l)"; and in paragraph (b)(3)(ii) by
removing the citation "§ 141.74(a)(3)" and add-
ing in its place "§141.74(aKlj", effective July
29, 2004.
1141.73 Filtration.
A public water system that uses a
surface water source or a ground water
source under the direct influence of
surface water, and does not meet all of
the criteria in §141.71 (a) and (b) for
avoiding filtration, must pro%'ide treat-
ment consisting of both disinfection, as
specified in §141.72(b), and filtration
treatment which complies with the re-
quirements of paragraph (a), (b), (c),
(d), or (e) of this section by June 29,
1993, or within 18 months of the failure
to meet any one of the criteria for
448
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Environmental Protection Agency
§141.73
avoiding filtration in §141.71 (a) and
(b). whichever is later. Failure to meet
any requirement, of this section after
the date specified in this introductory
paragraph is a treatment technique
violation.
(a) Conventional filtration treatment or
direct filtration. (1) For systems using
conventional filtration or direct filtra-
tion, the turbidity level of representa-
tive samples of a system's filtered
water must be less than or equal to 0.5
NTU in at least 95 percent of the meas-
urements taken each month, measured
as specified in §141.74 (a)(4) and (0(1),
except that if the State determines
that the system is capable of achieving
at least 99.9 percent removal and/or in-
activation of Giarclia lamblia cysts at
some turbidity level higher than 0.5
NTU in at least 95 percent of the meas-
urements taken each month, the State
may substitute this higher turbidity
limit for that system. However, in no
case may the State approve a turbidity
limit that allows more than 1 NTU in
more than 5 percent of the samples
taken each month, measured as speci-
fied in §141.74 (a)(4) and (c)(l).
(2) The turbidity level of representa-
tive samples of a system's filtered
water must at no time exceed 5 NTU,
measured as specified in §141.74 (a)(4)
and (c)(l).
(3) Beginning January 1. 2002, sys-
tems serving at least 10,000 people must
meet the turbidity requirements in
§141.173(a).
(4) Beginning January 14, 2005, sys-
tems serving fewer than 10,000 people
must meet the turbidity requirements
in §§141.550 through 141.553.
(b) Slow sand filtration. (1) For sys-
tems using slow sand filtration, the
turbidity level of representative sam-
ples of a system's filtered water must
be less than or equal to 1 NTU in at
least 95 percent of the measurements
taken each month, measured as speci-
fied in §141.74 (a)(4) and (c)(l), except
that if the State determines there is no
significant interference with disinfec-
tion at a higher turbidity level, the
State may substitute this higher tur-
bidity limit for that system.
(2) The turbidity level of representa-
tive samples of a system's filtered
water must at no time exceed 5 NTU,
measured as specified in §141.74 (a){4)
and (e)(l),
(c) Diatomaceous earth filtration, (l.i
For systems using diatomaceous earth
filtration, the turbidity level of rep-
resentative samples of a system's fil-
tered water must be less than or equal
to 1 NTU in at least 95 percent of the
measurements taken each month,
measured as specified in §141,74 (a)(4)
and (c)(l).
(2) The turbidity level of representa-
tive samples of a system's filtered
water must at no time exceed 5 NTU,
measured as specified in §141.74 (aK4)
and (eMl).
(d) Other filtration technologies. A pub-
lic water system may use a filtration
technology not listed in paragraphs (a)
through (cS of this section if it dem-
onstrates to the State, using pilot
plant studies or other means, that the
alternative filtration technology, in
combination with disinfection treat-
ment that meets the requirements of
§141.72(b), consistently achieves 99.9
percent removal and/or inactivation of
Giardia lamblia cysts and 99.99 percent
removal and/or inactivation of viruses.
For a system that makes this dem-
onstration, the requirements of para-
graph (b) of this section apply. Begin-
ning January 1, 2002, systems serving
at least 10,000 people must meet the re-
quirements for other filtration tech-
nologies in |141.173(b). Beginning Janu-
ary 14. 2005, systems serving fewer than
10,000 people must meet the require-
ments for other filtration technologies
in §141.550 through 141.553.
[54 FR 27527, June 29, 1989, as amended at 63
FB 69516, Dec. 16, 1998: 66 FR 3776, Jan. 16,
2001: 67 FB 1836, Jan. 14, 2002]
EFFECTIVE DATE NOTE: At 69 FB 38855, June
29. 2004, §141.73 was amended in paragraph
(a)(l) by removing both citations
"§141,74(a)(4)" and adding- in their place
"§141.74(a)(l/'; in paragraph (a)(2) by remov-
ing the citation "§141.74(a)(4)" and adding in
its place "§141.74(a)(l)"; in paragraph- (a)(4) by
removing' the date "January 14, 2005" and add-
ing in its place "January 1, 2005"; in para-
graph (b)(l) by removing the citation
"§141.74(a)(4)" and adding in its place
"§141.74(a)(l)": in paragraph (b)(2) by remov-
ing the citation "§141.74(a)(4)" and adding- in
its place "§141,74(a)(D"; in paragraph (0(1) by
removing the citation "§141.74(a)(4)" and add-
ing in its place ''|141.74(a)(l)"; and in para-
graph (c)(2) by removing the citation
449
-------
§141.74
40 CFR Ch, I (7-1-04 Edition)
"§141.74(a}(4)" and adding in its place
"§ 141.74(a)(l)", effective July 29, 2004.
§141.74 Analytical and monitoring re-
quirements,
(a) Analytical requirements. Only the
analytical method(s) specified in this
paragraph, or otherwise approved by
EPA, may be used to demonstrate com-
pliance with §§141.71, 141.72 and 141.73.
Measurements for pH, turbidity, tem-
perature and residual disinfectant con-
centrations must be conducted by a
person approved by the State. Measure-
ment for total coliforms, fecal coli-
forms and HPC must be conducted by a
laboratory certified by the State or
EPA to do such analysis. Until labora-
tory certification criteria are devel-
oped for the analysis of fecal coliforms
and HPC, any laboratory certified for
total coliforms analysis by the State or
EPA is deemed certified for fecal coli-
forms and HPC analysis. The following
procedures shall be conducted in ac-
cordance with the publications listed
in the following section. This incorpo-
ration by reference was approved by
the Director of the Federal Register in
accordance with 5 U.S.C. 552(a) and 1
CPR part 51. Copies of the methods
published in Standard Methods for the
Examination of Water and Wastewater
may be obtained from the American
Public Health Association et al., 1015
Fifteenth Street, NW., Washington, DC
20005; copies of the Minimal Medium
ONPG-MUG Method as set forth in the
article "National Field Evaluation of a
Defined Substrate Method for the Si-
multaneous Enumeration of Total Coli-
forms and Esherichia coli from Drinking
Water: Comparison with the Standard
Multiple Tube Fermentation Method"
(Edberg et al.), Applied and Environ-
mental Microbiology, Volume 54, pp.
1595-1801, June 1988 (as amended under
Erratum, Applied and Environmental
Microbiology, Volume 54, p. 3197, De-
cember. 1988), may be obtained from
the American Water Works Association
Research Foundation, 6666 West Quincy
Avenue, Denver, Colorado, 80235; and
copies of the Indigo Method as set forth
in the article "Determination of Ozone
in Water by the Indigo Method" (Bader
and Hoigne), may be obtained from
Ozone Science & Engineering,
Pergamon Press Ltd., Fairview Park,
Elmsford, New York 10523. Copies may
be inspected at the U.S. Environmental
Protection Agency, Room EB15, 401 M
St., SW., Washington, DC 20460 or at
the National Archives and Records Ad-
ministration (NARA). For information
on the availability of this material at
NAEA, call 202-741-6030, or go to: http://
www.archives.gov/federal register/
code of federal regulations/
ibr locations.html,
(1) Public water systems must con-
duct analysis of pH and temperature in
accordance with one of the methods
listed at §141.23(k)(l). Public water sys-
tems must conduct analysis of total
coliforms, fecal coliforms,
heterotrophic bacteria, and turbidity
in accordance with one of the following
analytical methods and by using ana-
lytical test procedures contained in
Technical Notes on Drinking Water Meth-
ods, EPA-600/R-94-173, October 1994,
which is available at NTIS PB95-104766.
Citation1
Total Conform a
Fecal Coliforms2 ...
Helerotrophic bac-
teria2.
Turbidity
Total Coliform Fer-
mentation Tech-
nique *45.
Total Coliform
Membrane Filter
Technique 8,
ONPG-MUG Test7
Fecal Coliform
Procedure 8.
Fecal Coliform Fil-
ter Procedure.
Pour Plate Method
SimPlate".
Nephelometric
Method.
Nephelometric
Method.
Great Lakes In-
struments.
Hach FilterTrak ....
9221 A, B
9222 A, B
9223
9221 E
92220
9215 B
2130 B
1B0.19
Method 2
1013312
C
C
0
The procedures shall be done in accordance with the docu-
ments listed below. The incorporation by reference of the fol-
lowing documents listed in footnotes 1, 6, 7 and 9-12 was ap-
proved by the Director of Ihe Federal Register in accordance
with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the docu-
ments may be obtained from the sources listed below. Infor-
mation regarding obtaining these documents can be obtained
from the Safe Drinking Water Hotline at 8QO-42&-4791. Doc-
uments may be inspected at EPA's Drinking Wafer Docket,
1301 Constitution Avenue, NW., EPA West, Room B102.
Washington DC 20460 (Telephone: 202-566-2426); or at the
National Archives and Records Administration (NARA). For in-
formation on the availability of this material at NARA, call
202-741-6030, or go to: M4uftiww.arcrvves.gov/
tpdorat_reglfterAxxl0_dl tederal^regutations/
ibt___Jocations.html.
1 Except where noted, all methods refer to Sfartcfarr! Meth-
ods for the Examination of Water and Wastewater, 18th edi-
tion (1992), 19th edition (1995), or 20th edition (1998), Amer-
ican Public Health Association, 1015 Fifteenth Street, NW.,
Washington, DC 20005, The cited methods published in any
of these three editions may be used.
450
-------
Environmental Protection Agency
§141.74
2 The time from sample collection to initiation of analysis
may not exceed 8 hours. Systems must hold samples below
10 deg. C during transit.
3 Lactose broth, as commercially available, may be used in
lieu of lauryl tryptose broth, if the system conducts at least 25
parallel tests between this medium and lauryl tryptose broth
using the water normally tested, and this comparison dem-
onstrates that the false-positive rate and false-negative rate
for total coliform, using lactose broth, is less than 10 percent.
4 Media should cover inverted tubes at least one-half to two-
thirds after the sample is added.
5 No requirement exists to run the completed phase on 10
percent of all total coliform-positive confirmed tubes.
6 Ml agar also may be used. Preparation and use of Ml
agar is set forth in the article, "New medium for the simulta-
neous detection of total coliform and Escherichia coli in water''
by Brenner, K.P., et. al., 1993, Appl. Environ. Microbiol.
59:3534-3544. Also available from the Office of Water Re-
source Center (RC-4100T), 1200 Pennsylvania Avenue, NW.,
Washington DC 20460, EPA/600/J-99/225. Verification of
colonies is not required.
7The ONPG-MUG Test is also known as the Autoanalysis
Colilert System.
8A-1 Broth may be held up to three months in a tightly
closed screw cap tube at 4 deg. C.
s "Methods for the Determination of Inorganic Substances in
Environmental Samples", EPA/600/R-93/100, August 1993.
Available at NTIS, PB94-121811.
10GLI Method 2, "Turbidity", November 2, 1992, Great
Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee,
Wisconsin 53223.
11A description of the SimPlate method, "IDEXX SimPlate
TM HPC Test Method for Heterotrophs in Water", November
2000, can be obtained from IDEXX Laboratories, Inc., One
IDEXX Drive, Westbrook, Maine 04092, telephone (800) 321-
0207.
12 A description of the Hach FilterTrak Method 10133, "De-
termination of Turbidity by Laser Nephelometry", January
2000, Revision 2.0, can be obtained from; Hach Co., P.O.
Box 389, Loveland, Colorado 80539-0389. Phone: 800-227-
4224.
(2) Public water systems must meas-
ure residual disinfectant concentra-
tions with one of the analytical meth-
ods in the following table. Except for
the method for ozone residuals, the dis-
infectant residual methods are con-
tained in the 18th, 19th, and 20th edi-
tions of Standard Methods for the Ex-
amination of Water and Wastewater,
1992, 1995, and 1998; the cited methods
published in any of these three editions
may be used. The ozone method, 4500-
O3 B, is contained in both the 18th and
19th editions of Standard Methods for
the Examination of Water and Waste-
water, 1992, 1995; either edition may be
used. If approved by the State, residual
disinfectant concentrations for free
chlorine and combined chlorine also
may be measured by using DPD color!-
metric test kits. Free and total chlo-
rine residuals may be measured con-
tinuously by adapting a specified chlo-
rine residual method for use with a
continuous monitoring instrument pro-
vided the chemistry, accuracy, and pre-
cision remain same. Instruments used
for continuous monitoring must be
calibrated with a grab sample measure-
ment at least every five days, or with
a protocol approved by the State.
Residual
Free Chlo-
rine.
Total Chlo-
rine.
Chlorine Di-
oxide.
Ozone
Methodology
Amperometric Titration
DPD Ferrous
Titrimetric.
DPD Coiorimetric
Syringaldazine
(FACTS).
Amperometric Titration
Amperometric Titration
(low level measure-
ment).
DPD Ferrous
Titrimetric.
DPD Coiorimetric
lodometric Electrode ...
Amperometric Titration
DPD Method
Amperometric Titration
Indigo Method
Methods
4500-CI D
4500-CI F
4500-CI G
4500-CI H
4500-CI D
4500-CI E
4500-CI F
4500-CI G
4500-CI 1
4500-CIO2 C
4500-CIO2 D
4500-CICh E
4500-O, B
(b) Monitoring requirements for systems
that do not provide filtration. A public
water system that uses a surface water
source and does not provide filtration
treatment must begin monitoring, as
specified in this paragraph (b), begin-
ning December 31, 1990, unless the
State has determined that filtration is
required in writing pursuant to
§1412(b)(7)(C)(iii), in which case the
State may specify alternative moni-
toring requirements, as appropriate,
until filtration is in place. A public
water system that uses a ground water
source under the direct influence of
surface water and does not provide fil-
tration treatment must begin moni-
toring as specified in this paragraph (b)
beginning December 31, 1990, or 6
months after the State determines that
the ground water source is under the
direct influence of surface water.
whichever is later, unless the State has
determined that filtration is required
in writing pursuant to
§1412(b)(7)(C)aii), in which case the
State may specify alternative moni-
toring requirements, as appropriate.
until filtration is in place.
(1) Fecal coliform or total coliform
density measurements as required by
§141.71(a)(l) must be performed on rep-
resentative source water samples im-
mediately prior to the first or only
point of disinfectant application. The
system must sample for fecal or total
coliforms at the following minimum
frequency each week the system serves
water to the public:
451
-------
§141.74
40 CFRCh. I (7-1-04 Edition)
System size (persons served)
•=500
501 to 3 300
3,301 to 10,000
10 001 to 25000
>25,000
Samples/
week1
1
2
3
4
5
1 Must be taken on separate days.
Also, one fecal or total coliform den-
sity measurement must be made every
day the system serves water to the
public and the turbidity of the source
water exceeds 1 NTU (these samples
count towards the weekly coliform
sampling requirement) unless the State
determines that the system, for
logistical reasons outside the system's
control, cannot have the sample ana-
lyzed within 30 hours of collection.
(2) Turbidity measurements as re-
quired by §141.71(a)(2) must be per-
formed on representative grab samples
of source water immediately prior to
the first or only point of disinfectant
application every four hours (or more
frequently) that the system serves
water to the public. A public water sys-
tem may substitute continuous tur-
bidity monitoring for grab sample
monitoring if it validates the contin-
uous measurement for accuracy oil a
regular basis using a protocol approved
by the State.
(3) The total inactivation ratio for
each day that the system is in oper-
ation must be determined based on the
CTcW.9 values in tables 1.1-1.6, 2.1, and
3.1 of this section, as appropriate. The
parameters necessary to determine the
total inactivation ratio must be mon-
itored as follows:
(i) The temperature of the disinfected
water must be measured at least once
per day at each residual disinfectant
concentration sampling point.
(ii) If the system uses chlorine, the
pH of the disinfected water must be
measured at least once per day at each
chlorine residual disinfectant con-
centration sampling point.
(ill) The disinfectant contact time(s)
("T") must be determined for each day
during peak hourly flow.
(iv) The residual disinfectant con-
centration^) ("C") of the water before
or at the first customer must be meas-
ured each day during peak hourly flow.
(v) If a system uses a disinfectant
other than chlorine, the system may
demonstrate to the State, through the
use of a State-approved protocol for on-
site disinfection challenge studies or
other information satisfactory to the
State, that CT99.9 values other than
those specified in tables 2.1 and 3.1 in
this section other operational param-
eters are adequate to demonstrate that
the system is achieving the minimum
inactivation rates required by
§141.72(a)(l).
TABLE 1.1—CT VALUES (CTt,^) FOR 99.9 PER-
CENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY FREE CHLORINE AT 0.5 °C OR
LOWER 1
Resid-
ual
(mg/l)
S0.4 ..
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
2.6
2.8
3.0
pH
S6.0
137
141
145
148
152
155
157
162
165
169
172
175
178
181
6.5
163
168
172
176
180
184
189
193
197
201
205
209
213
217
7.0
195
200
205
210
215
221
226
231
236
242
247
252
257
261
7.5
237
239
246
253
259
266
273
279
286
297
298
304
310
316
8.0
277
286
295
304
313
321
329
338
346
353
361
368
375
382
8.5
329
342
354
365
376
387
397
407
417
426
435
444
452
460
S9.0
390
407
422
437
451
464
477
489
500
511
522
533
543
552
1 These CT values achieve greater than a 99.99 percent in-
activation of viruses. CT values between the indicated pH val-
ues may be determined by linear interpolation. CT values be-
tween the indicated temperatures of different tables may be
determined by linear interpolation. If no interpolation is used,
use the CTg9t) value at the lower temperature and at the high-
er pH.
TABLE 1.2—CT VALUES (CT 99.9) FOR 99.9
PERCENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY FREE CHLORINE AT 5.0 °C1
Free
resid-
ual
(mg/l)
S0.4 ..
0.6 ..
0.8 ..
1.0 ..
1.2 ..
1.4 ..
1.6 ..
1.8 ..
2.0 ..
2.2 ..
2.4 ..
2.6 ..
2.8 ..
3.0 ..
PH
S6.0
97
100
103
105
107
109
111
114
116
118
120
122
124
126
6.5
117
120
122
125
127
130
132
135
138
140
143
146
148
151
7.0
139
143
146
149
152
155
158
162
165
169
172
175
178
182
7.5
166
171
175
179
183
187
192
196
200
204
209
213
217
221
8.0
198
204
210
216
221
227
232
238
243
248
253
258
263
268
8.5
236
244
252
260
267
274
281
287
294
300
306
312
318
324
£9.0
279
291
301
312
320
329
337
345
353
361
368
375
382
389
1 These CT values achieve greater than a 99.99 percent in-
activation of viruses. CT values between the indicated pH val-
ues may be determined by linear interpolation. CT values be-
tween the indicated temperatures of different tables may be
determined by linear interpolation. If no interpolation is used,
use the CT99.9 value at the lower temperature, and at the
higher pH.
452
-------
Environmental Protection Agency
§141.74
TABLE 1.3—CT VALUES (CT WJ) FOR 99.9
PERCENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY FREE CHLORINE AT 10.0 °C1
TABLE 1.5—CT VALUES (CT99.9) FOR 99.9 PER-
CENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY FREE CHLORINE AT 20°C1
free
ual
(mg/lj
S0.4 ..
0.6 ,.
0-8 ..
1.0 ..
1.2 ..
1.4 ..
1.6 ..
1.8 ..
20 ..
2.2 .-
2.4 ..
2.6 .-
2,8 ..
i n
---6.0 6.5 7.0
73 88 104
75 90 107
78 92 110
79 94 112
80 95 114
82 98 116
83 99 119
86 : 101 : 122
87 . 104 124
89 j 105 ! 127
90 i 107 i 129
92! 110 j 131
93 111 134
QR 113 1 37
pH
7.5
125
128
131
134
137
140
144
147
150
153
157
160
163
1RA
Free
8.0 8.5 sg.o /(JjJ|j
149 177 209 £0.4
153 183 218 0.6
158 189 226 0,8
162 195 234 1-0
166 200 240 1-2
170 206 247 14
174 211 253 1-6
179 215 259 1'8
182 221 i 265 °
186 ! 225 j 271 jj'f
190 i 230 ! 276 ^'*
194 j 234 ! 281 ,„
197 239 287 g°
OA1 I *>i*Q I 000
S 6,0
36
38
39
39
40
41
42
43
44
44
45
46
47
47
6.5
44
45
46
47
48
49
50
51
52
53
54
55
56
57
7.0
52
54
55
56
57
58
59
61
62
63
65
86
67
68
pH
7.5
62
64
66
67
69
70
72
74
75
77
78
80
81
83
8,0
74
77
79
81
83
85
87
89
91
93
95
97
99
101
8,5
89
92
95
98
100
103
105
108
110
113
115
117
119
122
^ 9,0
105
109
113
117
120
123
126
129
132
135
138
141
143
146
1 These CT values achieve greater than a 99.99 percent in-
activation of viruses. CT values between the indicated pH vai-
ues may be determined by linear interpolation. CT values be-
tween the indicated temperatures of different tables may be
determined by linear interpolation. If no interpolation is used,
use the CT^.v value at the lower temperature, and at the
higher pH.
TABLE 1,4—CT VALUES (CT 99,9) FOR 99.9
PERCENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY FREE CHLORINE AT 15.0 °C1
activation of viruses CT values between the indicated pH val-
ues may be determined by linear interpolation. CT values be-
tween the indicated temperatures ol different tables may be
determined by linear interpolation. If no interpolation is used,
use the CT.».
-------
§141.74
40 CFR Ch. I (7-1-04 Edition)
TABLE 3.1—CT VALUES (CT 99.9) FOR 99.9
PERCENT INACTIVATION OF GIARDIA LAMBLIA
CYSTS BY CHLORAMINESI
Temperature
<1 °C
3,800
5°C
2,200
10 °C
1,850
15 °C
1,500
20 °C
1,100
25 °C
750
1 These values are for pH values of 6 to 9. These CT val-
ues may be assumed to achieve greater than 99.99 percent
inactivation of viruses only if chlorine is added and mixed in
the water prior to the addition of ammonia. If this condition is
not met, the system must demonstrate, based on on-site stud-
ies or other information, as approved by the State, that the
system is achieving at least 99.99 percent inactivation of vi-
ruses. CT values between the indicated temperatures may be
determined by linear interpolation. If no interpolation is used,
use the CT9,>o value at the lower temperature for determining
CTj»t, values between indicated temperatures.
(4) The total inactivation ratio must
be calculated as follows:
(i) If the system uses only one point
of disinfectant application, the system
may determine the total inactivation
ratio based on either of the following
two methods:
(A) One inactivation ratio (CTcalc/
CT99.9) is determined before or at the
first customer during peak hourly flow
and if the CTcalc/CT99.9 ^ 1.0, the 99.9
percent Giardia lamblia inactivation re-
quirement has been achieved; or
(B) Successive CTcalc/CT99.9 values,
representing sequential inactivation
ratios, are determined between the
point of disinfectant application and a
point before or at the first customer
during peak hourly flow. Under this al-
ternative, the following method must
be used to calculate the total inactiva-
tion ratio:
• CTcalc r
(1) Determine for each sequence.
CT999
,_, , CTcalc , , (V (CTcalc) "|
(2) Add the values together >
CT I CT I
I CTcalc i
(3) If £ > 1.0, the 99.9 percent Giardia
\ ^99.9 )
lamblia inactivation requirement has
been achieved.
(ii) If the system uses more than one
point of disinfectant application before
or at the first customer, the system
must determine the CT value of each
disinfection sequence immediately
prior to the next point of disinfectant
application during peak hourly flow.
The CTcalc/CT99.9 value of each se-
quence and
»-, CTcalc
CT999
must be calculated using the method
in paragraph (b)(4)(i)(B) of this section
to determine if the system is in com-
pliance with §142.72(a).
(iii) Although not required, the total
percent inactivation for a system with
one or more points of residual dis-
infectant concentration monitoring
may be calculated by solving- the fol-
lowing equation:
Percent inactivation = 100 -
100
.
where z = 3 x
V
)
(5) The residual disinfectant con-
centration of the water entering the
distribution system must be monitored
continuously, and the lowest value
must be recorded each day, except that
if there is a failure in the continuous
monitoring equipment, grab sampling
every 4 hours may be conducted in lieu
of continuous monitoring, but for no
more than 5 working days following
the failure of the equipment, and sys-
tems serving 3,300 or fewer persons may
take grab samples in lieu of providing
continuous monitoring on an ongoing
454
-------
Environmental Protection Agency
§141.74
basis at the frequencies prescribed
below:
System size by population
Samples/
day1
<500 ; 1
501 (01,000 | 2
1,001 to 2.500 | 3
2,501 to 3,300 I 4
1 The day's samples cannot be taken at the same time. The
sampling intervals are subject to Stale review and approval.
If at any time the residual disinfectant
concentration falls below 0.2 mg/1 in a
system using grab sampling" in lieu of
continuous monitoring, the system
must take a grab sample every 4 hours
until the residual concentration Is
equal to or greater than 0.2 mg/1.
(6)(i) The residual disinfectant con-
centration must be measured at least
at the same points in the distribution
system and at the same time as total
coliforms are sampled, as specified in
§141.21, except that the State may
allow a public water system which uses
both a surface water source or a ground
water source under direct influence of
surface water, and a ground water
source, to take disinfectant residual
samples at points other than the total
coliform sampling points if the State
determines that such points are more
representative of treated (disinfected)
water quality within the distribution
system. Heterotrophic bacteria, meas-
ured as heterotrophic plate count
(HPC) as specified in paragraph (a)(3) of
this section, may be measured in lieu
of residual disinfectant concentration.
(ii) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory under the requisite
time and temperature conditions speci-
fied by paragraph (a)(3) of this section
and that the system is providing ade-
quate disinfection in the distribution
system, the requirements of paragraph
(b)(6)(i) of this section do not apply to
that system,
(c) Monitoring requirements for systems
using filtration treatment. A public water
system that uses a surface water
source or a ground water source under
the influence of surface water and pro-
vides filtration treatment must mon-
itor in accordance with this paragraph
(c) beginning June 29, 1993. or when fil-
tration is installed, whichever is later.
(1) Turbidity measurements as re-
quired by §141.73 must be performed on
representative samples of the system's
filtered water every four hours (or
more frequently) that the system
serves water to the public. A public
water system may substitute contin-
uous turbidity monitoring for grab
sample monitoring' if it validates the
continuous measurement for accuracy
on a regular basis using a protocol ap-
proved by the State. For any systems
using slow sand filtration or filtration
treatment other than conventional
treatment, direct filtration, or diato-
maceous earth filtration, the State
may reduce the sampling frequency to
once per day if it determines that less
frequent monitoring is sufficient to in-
dicate effective filtration performance.
For systems serving 500 or fewer per-
sons, the State may reduce the tur-
bidity sampling frequency to once per
day, regardless of the type of filtration
treatment used, if the State deter-
mines that less frequent monitoring is
sufficient to indicate effective filtra-
tion performance.
(2) The residual disinfectant con-
centration of the water entering the
distribution system must be monitored
continuously, and the lowest value
must be recorded each day, except that
if there is a failure in the continuous
monitoring equipment, grab sampling
every 4 hours may be conducted in lieu
of continuous monitoring, but for no
more than 5 working days following
the failure of the equipment, and sys-
tems serving 3,300 or fewer persons may
take grab samples in lieu of providing
continuous monitoring on an ongoing
basis at the frequencies each day pre-
scribed below:
System size by population | SiX'?s/
+500
501 to 1,000
1,001
2,501
to 2,500
to 3,300
1
2
3
4
1 The day's samples cannot be taken at (he same time. The
sampling intervals are subject to State review and approval
If at any time the residual disinfectant
concentration falls below 0.2 mg/1 in a
system using grab sampling in lieu of
continuous monitoring, the system
must take a grab sample every 4 hours
455
-------
§141.75
40 CFR Ch. I (7-1-04 Edition)
until the residual disinfectant con-
centration is equal to or greater than
0.2 mg/1.
(3)(i) The residual disinfectant con-
centration must be measured at least
at the same points in the distribution
system and at the same time as total
coliforms are sampled, as specified in
§141.21, except that the State may
allow a public water system which uses
both a surface water source or a ground
water source under direct influence of
surface water, and a ground water
source to take disinfectant residual
samples at points other than the total
coliform sampling points if the State
determines that such points are more
representative of treated (disinfected)
water quality within the distribution
system. Heterotrophic bacteria, meas-
ured as heterotrophic plate count
(HPC) as specified in paragraph (a)(3) of
this section, may be measured in lieu
of residual disinfectant concentration.
(ii) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory under the requisite
time and temperature conditions speci-
fied by paragraph (a)(3) of this section
and that the system is providing ade-
quate disinfection in the distribution
system, the requirements of paragraph
(c)(3)(i) of this section do not apply to
that system.
[54 FR 27527, June 29, 1989, as amended at 59
FR 62470, Dec. 5, 1994; 60 FR 34086, June 29,
1995: 64 PR 67465, Dec. 1, 1999; 67 FR 65252,
Oct. 23, 67 FB 65901, Oct. 29,
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, §141.74 was amended in paragraph
(b)(4)(ii) by removing the citation "§142.72(af
and adding in its place "|141.72(a)"; in para-
graph (bXSXil) by removing the citation
"(a)(3)" and adding in its place "(a)(l)"; in
paragraph (c)(3)(i) by removing the citation
"(a)(3)" and adding in its place "(a)(l)"; and in
paragraph (c)(3)(ii) by removing the citation
"(a)(3)" and adding in its place "(a)(l)", effec-
tive July 29, 2004.
§ 141.75 Reporting and recordkeeping
requirements.
(a) A public water system that uses a
surface water source and does not pro-
vide filtration treatment most report
monthly to the State the information
specified in this paragraph (a) begin-
ning December 31, 1S90, unless the
State has determined that filtration is
required in writing pursuant to section
1412(b)(7)(C}(iii), in which case the
State may specify alternative report-
ing requirements, as appropriate, until
filtration is in place. A public water
system that uses a ground water source
under the direct influence of surface
water and does not provide filtration
treatment must report monthly to the
State the information specified in this
paragraph (a) beginning December 31,
1990, or 6 months after the State deter-
mines that the ground water source is
under the direct influence of surface
water, whichever is later, unless the
State has determined that filtration is
required in writing pursuant to
§1412(b)(7)(C)(iii), in which case the
State may specify alternative report-
ing requirements, as appropriate, until
filtration is in place.
(1) Source water quality information
must be reported to the State within 10
days after the end of each month the
system serves water to the public. In-
formation that must he reported in-
cludes:
(i) The cumulative number of months
for which results are reported,
(ii) The number of fecal and/or total
coliform samples, whichever are ana-
lyzed during the month (if a system
monitors for both, only fecal coliforms
must be reported), the dates of sample
collection, and the dates when the tur-
bidity level exceeded 1 NTU.
(iii) The number of samples during
the month that had equal to or less
than 20/100 ml fecal coliforms and/or
equal to or less than 100/100 ml total
coliforms, whichever are analyzed.
(iv) The cumulative number of fecal
or total coliform samples, whichever
are analyzed, during the previous six
months the system served water to the
public.
(v) The cumulative number of sam-
ples that had equal to or less than 20/
100 ml fecal coliforms or equal to or
less than 100/100 ml total coliforms,
whichever are analyzed, during the pre-
vious six months the system served
water to the public.
(vi) The percentage of samples that
had equal to or less than 20/100 ml fecal
conforms or equal to or less than 100/
100 ml total coliforms, whichever are
analyzed, during the previous six
456
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Environmental Protection Agency
§141.75
months the system served water to the
public.
(vii) The maximum turbidity level
measured during the month, the date(s)
of occurrence for any measurement(s)
which exceeded 5 NTU, and the date(s)
the occurrence(s) was reported to the
State.
(viii) For the first 12 months of ree-
ordkeeping, the dates and cumulative
number of events during which the tur-
bidity exceeded 5 NTU, and after one
year of recordkeeping for turbidity
measurements, the dates and cumu-
lative number of events during which
the turbidity exceeded 5 NTU in the
previous 12 months the system served
water to the public.
(ix) For the first 120 months of rec-
ordkeeping, the dates and cumulative
number of events during which the tur-
bidity exceeded 5 NTU, and after 10
years of recordkeeping for turbidity
measurements, the dates and cumu-
lative number of events during which
the turbidity exceeded 5 NTU in the
previous 120 months the system served
water to the public.
(2) Disinfection information specified
in §141.74(b) must be reported to the
State within 10 days after the end of
each month the system serves water to
the public. Information that must be
reported includes:
(i) For each day, the lowest measure-
ment of residual disinfectant con-
centration in mg/1 in water entering
the distribution system.
(ii) The date and duration of each pe-
riod when the residual disinfectant
concentration in water entering the
distribution system fell below 0.2 mg.'l
and when the State was notified of the
occurrence.
(iii) The daily residual disinfectant
concentration(s) (in mg'/T) and dis-
infectant contact time(s) (in minutes)
used for calculating the CT value(s).
(iv) If chlorine is used, the daily
measurement(s) of pH of disinfected
water following each point of chlorine
disinfection.
(v) The daily measurement(s) of
water temperature in °0 following each
point of disinfection.
(vi) The daily CTcalc and CTcalc/
CT«9..) values for each disinfectant
measurement or sequence and the sum
of all CTcalc/CT9M values ((CTcalc/
CTi».9» before or at the first customer.
(vii) The daily determination of
whether disinfection achieves adequate
Giardia cyst and virus inactivation.
i.e., whether (CTcalc/CTcw.?) is at least
1.0 or. where disinfectants other than
chlorine are used, other indicator con-
ditions that the State determines are
appropriate, are met.
(viii) The following: information on
the samples taken in the distribution
system in conjunction with total coli-
form monitoring pursuant to §141,72:
(A) Number of instances where the
residual disinfectant concentration is
measured;
(B) Number of instances where the
residual disinfectant concentration is
not measured but heterotrophic bac-
teria plate count (HPC) is measured:
(C) Number of instances where the re-
sidual disinfectant concentration is
measured but not detected and no HPC
is measured;
(D) Number of instances where the
residual disinfectant concentration is
detected and where HPO is >500/ml;
(E) Number of instances where the
residual disinfectant concentration is
not measured and HPC is >500/ml;
(F) For the current and previous
month the system served water to the
public, the value of "V" in the following
formula:
a + b
where:
a=the value in paragraph (a)(2Mviii)(A) of
this section,
b=the value in paragraph (a)(2)(viii)(B) of
this section,
c=the value in paragraph (a)(2)(viii)(G) of
tills section,
d=the value in paragraph (a)(2)(viii)(D) of
this section, aiicl
e=the value in paragraph (a)(2)(viii)(E) of
this section.
(G) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory under the requisite
time and temperature conditions speci-
fied by §141.74(a)(3) and that the sys-
tem is providing adequate disinfection
in the distribution system, the require-
ments of paragraph (a)(2)(viii) (A)-(F)
457
-------
§141.75
40 CFR Ch. 1 (7-1-04 Iditlon)
of this section do not apply to that sys-
tem.
(ix) A system need not report the
data listed in paragraphs (a)(2) (i), and
(iii)-(vl) of this section if all data listed
in paragraphs (a)(2) (i)-(viii) of this sec-
tion remain on file at the system, and
the State determines that:
(A) The system has submitted to the
State all the information required by
paragraphs (a)(2) (iXviii) of this sec-
tion for at least 12 months; and
(B) The State has determined that
the system is not required to provide
filtration treatment.
(3) No later than ten days after the
end of each Federal fiscal year (Sep-
tember 30), each system must provide
to the State a report which summa-
rizes its compliance with all watershed
control program requirements specified
in§141.71(b)(2).
(4) No later than ten days after the
end of each Federal fiscal year (Sep-
tember 30), each system must provide
to the State a report on the on-site in-
spection conducted during that year
pursuant to §141.71(b)(3), unless the on-
site inspection was conducted by the
State. If the inspection was conducted
by the State, the State must provide a
copy of its report to the public water-
system.
(5)(i) Bach system, upon discovering
that a waterborne disease outbreak po-
tentially attributable to that water
system has occurred, must report that
occurrence to the State as soon as pos-
sible, but no later than by the end of
the next business day.
(ii) If at any time the turbidity ex-
ceeds 5 NTU, the system must consult
with the primacy agency as soon as
practical, but no later than 24 hours
after the exceedance is known, in ac-
cordance with the public notification
requirements under § 141.203(b)(3).
(iii) If at any time the residual falls
below 0.2 mg/1 in the water entering the
distribution system, the system must
notify the State as soon as possible,
but no later than by the end of the next
business day. The system also must no-
tify the State by the end of the next
business day whether or not the resid-
ual was restored to at least 0.2 mg/1
within 4 hours.
(b) A public water system that uses a
surface water source or a ground water
source under the direct influence of
surface water and provides filtration
treatment must report monthly to the
State the information specified in this
paragraph (b) beginning June 29, 1993,
or when filtration is installed, which-
ever is later.
(1) Turbidity measurements as re-
quired by §141.74(c)(l) must be reported
within 10 days after the end of each
month the system serves water to the
public. Information that must be re-
ported includes:
(i) The total number of filtered water
turbidity measurements taken during
the month.
(ii) The number and percentage of fil-
tered water turbidity measurements
taken during the month which are less
than or equal to the turbidity limits
specified in §141.73 for the filtration
technology being used.
(iii) The date and value of any tur-
bidity measurements taken during the
month which exceed 5 NTU.
(2) Disinfection information specified
in §141.74(c) must be reported to the
State within 10 days after the end of
each month the system serves water to
the public. Information that must be
reported includes:
(i) For each day, the lowest measure-
ment of residual disinfectant con-
centration in mg/1 in water entering
the distribution system.
(ii) The date and duration of each pe-
riod when the residual disinfectant
concentration in water entering the
distribution system fell below 0.2 mg/1
and when the State was notified of the
occurrence.
(iii) The following information on the
samples taken in the distribution sys-
tem in conjunction with total coliform
monitoring pursuant to §141.72:
(A) Number of instances where the
residual disinfectant concentration is
measured;
(B) Number of instances where the
residual disinfectant concentration is
not measured but heterotrophic bac-
teria plate count (HPC) is measured;
(C) Number of instances where the re-
sidual disinfectant concentration is
measured but not detected and no HPC
is measured:
(D) Number of Instances where no re-
sidual disinfectant concentration is de-
tected and where HPC is >500/ml;
458
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Environmental Protection Agency
§141.76
(E) Number of instances where the
residual disinfectant concentration is
not measured and HPC is >500/ml;
(P) For the current and previous
month the system serves water to the
public, the value of "V" in the following
formula:
V =
c + d + e
xlOO
where;
a=the value in
section,
b=the value in
section,
c=the value in
section,
d=the value in
section, and
e=the value in
section.
a + b
paragraph (b)(2Miii)(A> of this
paragraph (b)(2)iiii)(B) of this
paragraph (b)(2)(iii)(C) of this
paragraph (b)(2)(iii)(D) of this
paragraph (b)(2)(iii)(B) of this
(G-) If the State determines, based on
site-specific considerations, that a sys-
tem has no means for having a sample
transported and analyzed for HPC by a
certified laboratory within the req-
uisite time and temperature conditions
specified by §141.74(a)(3) and that the
system is providing adequate disinfec-
tion in the distribution system, the re-
quirements of paragraph (b)(2)(iii) (A>-
(P) of this section do not apply.
(iv) A system need not report the
data listed in paragraph (b)(2)(i) of this
section if all data listed in paragraphs
(b)(2) (i)-(iii) of this section remain on
file at the system and the State deter-
mines that the system lias submitted
all the information required by para-
graphs (b)(2) (iV(iii) of this section for
at least 12 months.
(3X1) Each system, upon discovering'
that a waterborne disease outbreak po-
tentially attributable to that water
system has occurred, must report that
occurrence to the State as soon as pos-
sible, but no later than by the end of
the next business day.
(ii) If at any time the turbidity ex-
ceeds 5 NTTJ, the system must consult
with the primacy agency as soon as
practical, but no later than 24 hours
after the exceedance is known, in ac-
cordance with the public notification
requirements under §141.203(b)(3).
(iii) If at any time the residual falls
below 0,2 tng/1 in the water entering the
distribution system, the system must
notify the State as soon as possible.
but no later than by the end of the next
business day. The system also must no-
tify the State by the end of the next
business day whether or not the resid-
ual was restored to at least 0.2 mg/1
within 4 hours.
[54 FR 27527, June 29, 1989, as amended at 65
FR 26022, May 4, 2000]
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, §141.75 was amended in paragraph
(a)(2)(vUi)(G) by removing the citation
"§141,74(a)(3)" and adding in its place
"§141.74(a)(D", and in paragraph (b)(2)(lii)(G!
by removing the citation "§141.74(a)(3)" and
adding in its place "§141.74(a)(D". effective
July 29, 2004.
§ 141.76 Recycle provisions.
(a) Applicability. All subpart H sys-
tems that employ conventional filtra-
tion or direct filtration treatment and
that recycle spent filter backwash
water, thickener supernatant, or liq-
uids from dewatering processes must
meet the requirements in paragTaphs
(b) through (d) of this section.
(b) Reporting. A system must notify
the State in writing1 by Decemeber 8,
2003, if the system recycles spent filter
backwash water, thickener super-
natant, or liquids from dewatering
processes. This notification must in-
clude, at a minimum, the information
specified in paragraphs (b)(l) and (2) of
this section.
(1) A plant schematic showing the or-
igin of all flows which are recycled (in-
cluding, but not limited to. spent filter
backwash water, thickener super-
natant, and liquids from dewatering
processes), the hydraulic conveyance
used to transport them, and the loca-
tion where they are re-introduced back
into the treatment plant.
(2) Typical recycle flow in gallons per
minute (gpm), the highest observed
plant flow experienced in the previous
year (gpm). design flow for the treat-
ment plant (gpm), and State-approved
operating capacity for the plant where
the State has made such determina-
tions.
(c) Treatment technique requirement.
Any system that recycles spent filter
backwash water, thickener super-
natant, or liquids from dewatering
processes must return these flows
through the processes of a system's ex-
isting conventional or direct filtration
459
-------
§141,80
40 CFR Ch. 1 (7-1-04 Edition)
system as defined in §141.2 or at an al-
ternate location approved by the State
by June 8, 2004. If capital improve-
ments are required to modify the recy-
cle location to meet this requirement,
all capital improvements must be com-
pleted no later than June 8, 2006.
(A) Recordkeeping. The system must
collect and retain on file recycle flow
information specified in paragraphs
(d)(l) through (6) of this section for re-
view and evaluation by the State be-
ginning June 8, 2004.
(1) Copy of the recycle notification
and information submitted to the
State under paragraph (b) of this sec-
tion.
(2) List of all recycle flows and the
frequency with which they are re-
turned.
(3) Average and maximum backwash
flow rate through the filters and the
average and maximum duration of the
filter backwash process in minutes.
(4) Typical filter run length and a
written summary of how filter run
length is determined.
(5) The type of treatment provided
for the recycle flow.
(6) Data on the physical dimensions
of the equalization and/or treatment
units, typical and maximum hydraulic
loading rates, type of treatment chemi-
cals used and average dose and fre-
quency of use. and frequency at which
solids are removed, if applicable.
[66 FR 31103, June 8, 2001]
Subpart I—Control of Lead and
Copper
SOURCE; 56 FR 26548, June 7, 1991, unless
otherwise noted.
§ 141.80 General requirements.
(a) Applicability and effective dates, (1)
The requirements of this subpart I con-
stitute the national primary drinking
water regulations for lead and copper.
Unless otherwise indicated, each of the
provisions of this subpart applies to
community water systems and non-
transient, non-community water sys-
tems (hereinafter referred to as "water
systems" or "systems").
(2) The requirements set forth in
§§141,86 to 141.91 shall take effect on
July 7, 1991. The requirements set forth
in §§141.80 to 141.85 shall take effect on
December 7, 1992.
(b) Scope. These regulations establish
a treatment technique that includes re-
quirements for corrosion control treat-
ment, source water treatment, lead
service line replacement, and public
education. These requirements are
triggered, in some cases, by lead and
copper action levels measured in sam-
ples collected at consumers' taps.
(c) Lead and copper action levels. (1)
The lead action level is exceeded if the
concentration of lead in more than 10
percent of tap water samples collected
during any monitoring period con-
ducted in accordance with §141.86 is
greater than 0.015 mg/L (i.e., if the
"90th percentile" lead level is greater
than 0.015 mg/L).
(2) The copper action level is exceed-
ed if the concentration of copper in
more than 10 percent of tap water sam-
ples collected during any monitoring
period conducted in accordance with
§141.86 is greater than 1.3 mg/L (i.e., if
the "90th percentile" copper level is
greater than 1.3 mg/L).
(3) The 90th percentile lead and cop-
per levels shall be computed as follows:
(i) The results of all lead or copper
samples taken during a monitoring pe-
riod shall be placed in ascending order
from the sample with the lowest con-
centration to the sample with the high-
est concentration. Each sampling re-
sult shall be assigned a number, as-
cending by single integers beginning
with the number 1 for the sample with
the lowest contaminant level. The
number assigned to the sample with
the highest contaminant level shall "be
equal to the total number of samples
taken.
(ii) The number of samples taken
during the monitoring period shall be
multiplied by 0.9.
(iii) The contaminant concentration
in the numbered sample yielded by the
calculation in paragraph (c)(3)(ii) is the
90th percentile contaminant level.
(iv) For water systems serving fewer
than 100 people that collect 5 samples
per monitoring period, the 90th per-
centile is computed by taking the aver-
age of the highest and second highest
concentrations.
460
-------
Environmental Protection Agency
§141.81
(d) Corrosion control treatment require-
ments. (1) All water systems shall in-
stall and operate optimal corrosion
control treatment as defined in §141.2,
(2) Any water system that complies
with the applicable corrosion control
treatment requirements specified by
the State under §§141.81 and 141.82 shall
be deemed in compliance with the
treatment requirement contained in
paragraph (d)(l) of this section.
(e) Source water treatment require-
ments. Any system exceeding the lead
or copper action level shall implement
all applicable source water treatment
requirements specified by the State
under §141.83.
(f) Lead service line replacement re-
quirements. Any system exceeding the
lead action level after implementation
of applicable corrosion control and
source water treatment requirements
shall complete the lead service line re-
placement requirements contained in
§141.84.
(g) Public education requirements. Any
system exceeding the lead action level
shall implement the public education
requirements contained in § 141.85.
(h) Monitoring and analytical require-
ments. Tap water monitoring for lead
and copper, monitoring for water qual-
ity parameters, source water moni-
toring for lead and copper, and anal-
yses of the monitoring results under
this subpart shall be completed in com-
pliance with §§141.86, 141.87, 141,88, and
141.89.
(i) Reporting requirements. Systems
shall report to the State any informa-
tion required by the treatment provi-
sions of this subpart and § 141.90.
(j) Record-keeping requirements. Sys-
tems shall maintain records in accord-
ance with §141.91.
(k) Violation of national primary drink-
ing water regulations. Failure to comply
with the applicable requirements of
§§141.80-141.91, including requirements
established by the State pursuant to
these provisions, shall constitute a vio-
lation of the national primary drinking
water regulations for lead and/or cop-
per.
[56 FE 26548, Jane 7, 1991; 57 FB 28788, Jane
29, 1992]
§ 141.81 Applicability of corrosion con-
trol treatment steps to small, me-
dium-size and large water systems.
(a) Systems shall complete the appli-
cable corrosion control treatment re-
quirements described in §141.82 by the
deadlines established in this section.
(1) A large system {serving >50,000
persons) shall complete the corrosion
control treatment steps specified in
paragraph (d) of this section, unless it
is deemed to have optimized corrosion
control under paragraph (b)(2) or (b)(3)
of this section.
(2) A small system (serving <3300 per-
sons) and a medium-size system (serv-
ing >3,300 and <50,000 persons) shall
complete the corrosion control treat-
ment steps specified in paragraph (e) of
this section, unless it is deemed to
have optimized corrosion control under
paragraph (b)(l), (b)(2), or (b)(3) of this
section.
(b) A system is deemed to have opti-
mized corrosion control and is not re-
quired to complete the applicable cor-
rosion control treatment steps identi-
fied in this section if the system satis-
fies one of the criteria specified in
paragraphs (bKl) through (b)(3) of this
section. Any such system deemed to
have optimized corrosion control under
this paragraph, and which has treat-
ment in place, shall continue to oper-
ate and maintain optimal corrosion
control treatment and meet any re-
quirements that the State determines
appropriate to ensure optimal corro-
sion control treatment is maintained.
(1) A small or medium-size water sys-
tem is deemed to have optimized corro-
sion control if the system meets the
lead and copper action levels during
each of two consecutive six-month
monitoring periods conducted in ac-
cordance with §141.86.
(2) Any water system may be deemed
by the State to have optimized corro-
sion control treatment if the system
demonstrates to the satisfaction of the
State that it has conducted activities
equivalent to the corrosion control
steps applicable to such system under
this section. If the State makes this
determination, it shall provide the sys-
tem with written notice explaining the
basis for its decision and shall specify
the water quality control parameters
representing optimal corrosion control
461
-------
§141,81
40 CFR Ch. I (7-1-04 Edition)
in accordance with §141.82(f). Water
systems deemed to have optimized cor-
rosion control under this paragraph
shall operate in compliance with the
State-designated optimal water quality
control parameters in accordance with
§141.82(g) and continue to conduct lead
and copper tap and water quality pa-
rameter sampling in accordance with
§141.86(d)(3) and §141.87(d), respectively.
A system shall provide the State with
the following information in order to
support a determination under this
paragraph:
(i) The results of all test samples col-
lected for each of the water quality pa-
rameters in §141.82(0(3).
(ii) A report explaining" the test
methods used by the water system to
evaluate the corrosion control treat-
ments listed in §141,82(c)(l), the results
of all tests conducted, and the basis for
the system's selection of optimal cor-
rosion control treatment;
(iii) A report explaining how corro-
sion control has been installed and how
it is being maintained to Insure mini-
mal lead and copper concentrations at
consumers' taps; and
(iv) The results of tap water samples
collected in accordance with §141.86 at
least once eve, / six months for one
year after corrosion control has been
installed.
(3) Any water system is deemed to
have optimized corrosion control if it
submits results of tap water moni-
toring conducted in accordance with
§141.86 and source water monitoring
conducted in accordance with §141,88
that demonstrates for two consecutive
6-month monitoring' periods that the
difference between the 90th. percentile
tap water lead level computed under
§141,80(c)(3), and the highest source
water lead concentration is less than
the Practical Quantitation Level for
lead specified in §141.89(a)(lXii).
(i) Those systems whose highest
source water lead level is below the
Method Detection Limit may also be
deemed to have optimized corrosion
control under this paragraph if the 90th
percentile tap water lead level is less
than or equal to the Practical Quan-
titation Level for lead for two consecu-
tive 6-month monitoring periods.
(ii) Any water system deemed to have
optimized corrosion control in accord-
ance with this paragraph shall con-
tinue monitoring for lead and copper at
the tap no less frequently than once
every three calendar years using the
reduced number of sites specified in
§141.86(c) and collecting the samples at
times and locations specified in
§141.86(d)(4)(iv). Any such system that
has not conducted a round of moni-
toring pursuant to §141.86(d) since Sep-
tember 30. 1997, shall complete a round
of monitoring pursuant to this para-
graph no later than September 30, 2000.
(iii) Any water system deemed to
have optimized corrosion control pur-
suant to this paragraph, shall notify
the State in writing pursuant to
§141.90{a)(3) of any change in treatment
or the addition of a new source. The
State may require any such system to
conduct, additional monitoring or to
take other action the State deems ap-
propriate to ensure that such systems
maintain minimal levels of corrosion
in the distribution system.
(iv) As of July 12, 2001, a system is
not deemed to have optimized corro-
sion control under this paragraph, and
shall implement corrosion control
treatment pursuant to paragraph
(b)(3)(v) of this section unless it meets
the copper action level,
(v) Any system triggered into corro-
sion control because it is no longer
deemed to have optimized corrosion
control under this paragraph shall im-
plement corrosion control treatment in
accordance with the deadlines in para-
graph (e) of this section. Any such
large system shall adhere to the sched-
ule specified in that paragraph for me-
dium-size systems, with the time peri-
ods for completing each step being
triggered by the date the system is no
longer deemed to have optimized corro-
sion control under this paragraph.
(c) Any small or medium-size water
system that is required to complete the
corrosion control steps due to its ex-
ceedance of the lead or copper action
level may cease completing the treat-
ment steps whenever the system meets
both action levels during each of two
consecutive monitoring periods con-
ducted pursuant to §141.86 and submits
the results to the State. If any such
water system thereafter exceeds the
lead or copper action level during any
monitoring period, the system (or the
462
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Environmental Protection Agency
§141.81
State, as the case may be) shall recom-
mence completion of the applicable
treatment steps, beginning with the
first treatment step which was not pre-
viously completed In its entirety. The
State may require a system to repeat
treatment steps previously completed
by the system where the State deter-
mines that this is necessary to imple-
ment properly the treatment require-
ments of this section. The State shall
notify the system in writing of such a
determination and explain the basis for
its decision. The requirement for any
small- or medium-size system to imple-
ment corrosion control treatment steps
in accordance with paragraph (e) of
this section (including systems deemed
to have optimized corrosion control
under paragraph (b)(l) of this section)
is triggered whenever any small- or
medium-size system exceeds the lead
or copper action level.
(d) Treatment steps and deadlines for
large systems. Except as provided in
paragraph, (b) (2) and (3) of this section,
large systems shall complete the fol-
lowing corrosion control treatment
steps (described in the referenced por-
tions of §§141.82, 141.86, and 141.87) by
the indicated dates.
(1) Step 1: The system shall conduct
initial monitoring (§ 141.86(d)(l) and
§141.87(b)) during two consecutive six-
month monitoring periods by January
1, 1893.
(2) Step 2: The system shall complete
corrosion control studies (§141.82(cl) by
July 1, 1994.
(3) Step 3: The State shall designate
optimal corrosion control treatment
(§141.82(d)> by January 1. 1995.
(4) Step 4: The system shall install op-
timal corrosion control treatment
(§141.82(e)) by January 1. 1997.
(5) Step 5: The system shall complete
follow-up sampling (|141.86(d)(2) and
§141.87(0) by January 1, 1998.
(6) Step 6: The State shall review in-
stallation of treatment and designate
optimal water quality control param-
eters (§141,82(f)) by July 1, 1998.
(7) Step 7: The system shall operate in
compliance with the State-specified op-
timal water quality control parameters
(§141.82(g)) and continue to conduct tap
sampling (§141.86(d)(3) and §141.87(d)),
(e) Treatment Steps and deadlines for
small and medium-size systems. Except as
provided in paragraph (b) of this sec-
tion, small and medium-size systems
shall complete the following corrosion
control treatment steps (described in
the referenced portions of §§141.82,
141.86 and 141.87) by the indicated time
periods,
(1) Step 1: The system shall conduct
initial tap sampling (§141.86(d)(l) and
§141,87(b)) until the system either ex-
ceeds the lead or copper action level or
becomes eligible for reduced moni-
toring under §141.86(d)(4). A system ex-
ceeding the lead or copper action level
shall recommend optimal corrosion
control treatment (§141.82(a)) within
six months after it exceeds one of the
action levels.
(2) Step 2: Within 12 months after a
system exceeds the lead or copper ac-
tion level, the State may require the
system to perform corrosion control
studies (§141.8203)). If the State does
not require the system to perform such
studies, the State shall specify optimal
corrosion control treatment (§141.82(d))
within the following timeframes:
(i) For medium-size systems, within
18 months after such system exceeds
the lead or copper action level,
(ii) For small systems, within 24
months after such system exceeds the
lead or copper action level.
(3) Step 3: If the State requires a sys-
tem to perform corrosion control stud-
ies under step 2, the system shall com-
plete the studies (§141.82(c)) within 18
months after the State requires that
such studies be conducted.
(4) Step 4: If the system has per-
formed corrosion control studies under
step 2, the State shall designate opti-
mal corrosion control treatment
(§141.82(d)) within 6 months after com-
pletion of step 3.
(5) Step 5: The system shall install op-
timal corrosion control treatment
(§141.82(e)) within 24 months after the
State designates such treatment.
(6) Step 6: The system shall complete
follow-up sampling (§141.86(d)(2) and
§141.87(c)) within 36 months after the
State designates optimal corrosion
control treatment.
(7) Step 7: The State shall review the
system's installation of treatment and
designate optimal water quality con-
trol parameters (§141.82(f)) within 6
months after completion of step 6.
463
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§141.82
40 CFR Ch. I (7-1-04 Edition)
(8) Step 8: The system shall operate in
compliance with the State-designated
optimal water quality control param-
eters (§141.82(g)) and continue to con-
duct tap sampling (§141.86(d)(3) and
§141.87(d)).
[56 FR 26548, June 7. 1991, as amended at 59
FR 33862, June 30, 1994; 65 FR 2004, Jan. 12.
2000]
§141.82 Description of corrosion con-
trol treatment requirements.
Bach system shall complete the cor-
rosion control treatment requirements
described below which are applicable to
such system under §141.81.
(a) System recommendation regarding
corrosion control treatment. Based upon
the results of lead and copper tap mon-
itoring and water quality parameter
monitoring, small and medium-size
water systems exceeding the lead or
copper action level shall recommend
installation of one or more of the cor-
rosion control treatments listed in
paragraph (c)(l) of this section which
the system believes constitutes opti-
mal corrosion control for that system.
The State may require the system to
conduct additional water quality pa-
rameter monitoring in accordance with
§141.87(b) to assist the State in review-
ing the system's recommendation.
(b) State decision to require studies of
corrosion control treatment (applicable to
small and medium-size systems). The
State may require any small or me-
dium-size system that exceeds the lead
or copper action level to perform corro-
sion control studies under paragraph
(c) of this section to identify optimal
corrosion control treatment for the
system.
(c) Performance of corrosion control
studies. (1) Any public water system
performing corrosion control studies
shall evaluate the effectiveness of each
of the following treatments, and, if ap-
propriate, combinations of the fol-
lowing treatments to identify the opti-
mal corrosion control treatment for
that system:
(i) Alkalinity and pH adjustment;
(ii) Calcium hardness adjustment;
and
(iti) The addition of a phosphate or
silicate based corrosion inhibitor at a
concentration sufficient, to maintain
an effective residual concentration in
all test tap samples.
(2) The water system shall evaluate
each of the corrosion control treat-
ments using either pipe rig/loop tests,
metal coupon tests, partial-system
tests, or analyses based on documented
analogous treatments with other sys-
tems of similar size, water chemistry
and distribution.system configuration.
(3) The water system shall measure
the following water quality parameters
in any tests conducted under this para-
graph before and after evaluating the
corrosion control treatments listed
above:
(i) Lead;
(ii) Copper;
(ill) pH;
(iv) Alkalinity;
(v) Calcium;
(vi) Conductivity;
(vii) Orthophosphate (when an inhib-
itor containing a phosphate compound
is used);
(vili) Silicate (when an inhibitor con-
taining a silicate compound is used);
(ix) Water temperature.
(4) The water system shall identify
all chemical or physical constraints
that limit or prohibit the use of a par-
ticular corrosion control treatment
and document such constraints with at
least one of the following:
(i) Data and documentation showing
that a particular corrosion control
treatment has adversely affected other
water treatment processes when used
by another water system with com-
parable water quality characteristics;
and/or
(ii) Data and documentation dem-
onstrating that the water system has
previously attempted to evaluate a
particular corrosion control treatment
and has found that the treatment is in-
effective or adversely affects other
water quality treatment processes.
(5) The water system shall evaluate
the effect of the chemicals used for cor-
rosion control treatment on other
water quality treatment processes.
(6) On the basis of an analysis of the
data generated during each evaluation,
the water system shall recommend to
the State in writing the treatment op-
tion that the uorrosior. control studies
indicate constitutes optimal corrosion
control treatment for that svstem. The
464
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Environmental Protection Agency
§141.82
water system shall provide a rationale
for its recommendation along with all
supporting' documentation specified in
paragraphs (c) (1) through (5) of this
section,
(d) State designation of optimal corro-
sion control treatment. (1) Based upon
consideration of available information
including, where applicable, studies
performed under paragraph (c) of this
section and a system's recommended
treatment alternative, the State shall
either approve the corrosion control
treatment option recommended by the
system, or designate alternative corro-
sion control treatment(s) from among'
those listed in paragraph (c)(l) of this
section. When designating' optimal
treatment the State shall consider the
effects that additional corrosion con-
trol treatment will have on water qual-
ity parameters and on other water
quality treatment processes.
(2) The State shall notify the system
of its decision on optimal corrosion
control treatment in writing and ex-
plain the basis for this determination.
If the State requests additional infor-
mation to aid its review, the water sys-
tem shall provide the information.
(e) Installation of optimal corrosion
control, Bach system shall properly in-
stall and operate throughout its dis-
tribution system the optimal corrosion
control treatment designated by the
State under paragraph (d) of this sec-
tion.
(f) State review of treatment and speci-
fication of optimal water quality control
parameters. The State shall evaluate
the results of all lead and copper tap
samples and water quality parameter
samples submitted by the water system
and determine whether the system has
properly installed and operated the op-
timal corrosion control treatment des-
ignated by the State in paragraph (d)
of this section. Upon reviewing the re-
sults of tap water and water quality
parameter monitoring by the system.
both before and after the system in-
stalls optimal corrosion control treat-
ment, the State shall designate:
(1) A minimum value or a range of
values for pH measured at each entry
point to the distribution system;
(2) A minimum pH value, measured in
all tap samples. Such value shall be
equal to or greater than 7,0, unless the
State determines that meeting a pH
level of 7.0 is not technologically fea-
sible or is not necessary for the system
to optimize corrosion control;
(3) If a corrosion inhibitor is used, a
minimum concentration or a range of
concentrations for the inhibitor, meas-
ured at each entry point to the dis-
tribution system and in all tap sam-
ples, that the State determines is nec-
essary to form a passivating film on
the interior walls of the pipes of the
distribution system;
(4) If alkalinity is adjusted as part of
optimal corrosion control treatment, a
minimum concentration or a range of
concentrations for alkalinity, meas-
ured at each entry point to the dis-
tribution system and in all tap sam-
ples;
(5) If calcium carbonate stabilization
is used as part of corrosion control, a
minimum concentration or a range of
concentrations for calcium, measured
in all tap samples.
The values for the applicable water
quality control parameters listed
above shall be those that the State de-
termines to reflect optimal corrosion
control treatment for the system. The
State may designate values for addi-
tional water quality control param-
eters determined by the State to re-
flect optimal corrosion control for the
system. The State shall notify the sys-
tem in writing of these determinations
and explain the basis for its decisions.
(g) Continued operation and moni-
toring. All systems optimizing corro-
sion control shall continue to operate
and maintain optimal corrosion con-
trol treatment, including maintaining
water quality parameters at or above
minimum values or within ranges des-
ignated by the State under paragraph
(f) of this section, in accordance with
this paragraph for all samples collected
under §141.87(d) through (f). Compli-
ance with the requirements of this
paragraph shall be determined every
six months, as specified under
§141.87(d). A water system is out of
compliance with the requirements of
this paragraph for a six-month period if
it has excursions for any State-speci-
fied parameter on more than nine days
during the period. An excursion occurs
whenever the daily value for one or
more of the water quality parameters
465
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§141.83
40 CFR Ch. I (7-1-04 Edition)
measured at a sampling location is
below the minimum value or outside
the range designated by the State.
Daily values are calculated as follows.
States have discretion to delete results
of obvious sampling errors from this
calculation.
(1) On days when more than one
measurement for the water quality pa-
rameter is collected at the sampling lo-
cation, the daily value shall be the av-
erage of all results collected during the
day regardless of whether they are col-
lected through continuous monitoring,
grab sampling, or a combination of
both. If EPA has approved an alter-
native formula under §142.16 of this
chapter in the State's application for a
program revision submitted pursuant
to §142.12 of this chapter, the State's
formula shall be used to aggregate
multiple measurements taken at a
sampling point for the water quality
parameter in lieu of the formula in this
paragraph.
(2) On days when only one measure-
ment for the water quality parameter
is collected at the sampling location,
the daily value shall be the result of
that measurement.
(3) On days when no measurement is
collected for the water quality param-
eter at the sampling location, the daily
value shall be the daily value cal-
culated on the most recent day on
which the water quality parameter was
measured at the sample site,
(h) Modification of State treatment de-
cisions. Upon its own initiative or in re-
sponse to a request by a water system
or other interested party, a State may
modify its determination of the opti-
mal corrosion control treatment under
paragraph (d) of this section or optimal
water quality control parameters
under paragraph (f) of this section. A
request for modification by a system or
other interested party shall be in writ-
ing, explain why the modification is
appropriate, and provide supporting
documentation. The State may modify
its determination where it concludes
that such change is necessary to ensure
that the system continues to optimize
corrosion control treatment. A revised
determination shall be made in writ-
ing, set forth the new treatment re-
quirements, explain the basis for the
State's decision, and provide an imple-
mentation schedule for completing the
treatment modifications.
(i) Treatment decisions by EPA in lieu
of the State. Pursuant to the procedures
in §142.19, the EPA Regional Adminis-
trator may review treatment deter-
minations made by a State under para-
graphs (d), (f), or (h) of this section and
issue federal treatment determinations
consistent with the requirements of
those paragraphs where the Regional
Administrator finds that:
(1) A State has failed to issue a treat-
ment determination by the applicable
deadlines contained in §141.81,
(2) A State has abused its discretion
in a substantial number of cases or in
cases affecting a substantial popu-
lation, or
(3) The technical aspects of a State's
determination would be indefensible in
an expected Federal enforcement ac-
tion taken against a system.
[56 FR 26548, June 7, 1991, as amended at 65
PR 2004, Jan, 12, 2000]
§ 141.83 Source water treatment re-
quirements.
Systems shall complete the applica-
ble source water monitoring and treat-
ment requirements (described in the
referenced portions of paragraph (b) of
this section, and in §§141.86, and 141.88)
by the following deadlines.
(a) Deadlines for completing source
water treatment steps—(1) Step 1: A sys-
tem exceeding the lead or copper
action level shall complete lead and
copper source water monitoring
(§141.88(b)) and make a treatment
recommendation to the State
(§141.83(b)(D) within 6 months after ex-
ceeding the lead or copper action level.
(2) Step 2: The State shall make a
determination regarding source water
treatment (§141.83(b)(2» within 6
months after submission of monitoring
results under step 1.
(3) Step 3: If the State requires instal-
lation of source water treatment, the
system shall install the treatment
(§141,83(b){3)) within 24 months after
completion of step 2.
(4) Step 4: The system shall complete
follow-up tap water monitoring
(§141.86(d)(2) and source water moni-
toring (§141.88(c)) within 36 months
after completion of step 2.
466
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Environmental Protection Agency
§141.83
(5) Step 5: The State shall review the
system's installation and operation of
source water treatment and specify
maximum permissible source water
levels (§141.83(bX4)) within 6 months
after completion of step 4.
(6) Step 6: The system shall operate in
compliance with the State-specified
maximum permissible lead and copper
source water levels (§141.83(b)(4)) and
continue source water monitoring
(§141.88(d)).
(b) Description of source water treat-
ment requirements—(1) System treatment
recommendation. Any system which ex-
ceeds the lead or copper action level
shall recommend in writing to the
State the installation and operation of
one of the source water treatments
listed in paragraph (b)(2) of this sec-
tion. A system may recommend that
no treatment be installed "based upon a
demonstration that source water treat-
ment is not necessary to minimize lead
and copper levels at users' taps.
(2) Stale determination regarding source
water treatment. The State shall com-
plete an evaluation of the results of all
source water samples submitted by the
water system to determine whether
source water treatment is necessary to
minimize lead or copper levels in water
delivered to users" taps. If the State de-
termines that treatment is needed, the
State shall either require installation
and operation of the source water
treatment recommended by the system
(if any) or require the installation and
operation of another source water
treatment from among the following:
Ion exchange, reverse osmosis, lime
softening or coagulation/filtration. If
the State requests additional informa-
tion to aid in its review, the water sys-
tem shall provide the information by
the date specified by the State in its
request. The State shall notify the sys-
tem in writing of its determination and
set forth the basis for its decision.
(3) Installation of source water treat-
ment. Bach system shall properly in-
stall and operate the source water
treatment designated by the State
under paragraph (b)(2) of this section.
(4) State review of source water treat-
ment and specification of maximum per-
missible source water levels. The State
shall review the source water samples
taken by the water system both before
and after the system installs source
water treatment, and determine wheth-
er the system has properly installed
and operated the source water treat-
ment designated "by the State. Based
upon its review, the State shall des-
ignate the maximum permissible lead
and copper concentrations for finished
water entering the distribution system.
Such levels shall reflect the contami-
nant removal capability of the treat-
ment properly operated and main-
tained. The State shall notify the sys-
tem in writing and explain the basis for
its decision.
(5) Continued operation and mainte-
nance. Each water system shall main-
tain lead and copper levels below the
maximum permissible concentrations
designated by the State at each sam-
pling point monitored in accordance
with §141.88. The system is out of com-
pliance with this paragraph if the level
of lead or copper at any sampling point
is greater than the maximum permis-
sible concentration designated by the
State.
(6) Modification of Slate treatment deci-
sions. Upon its own initiative or in re-
sponse to a request by a water system
or other interested party, a State may
modify its determination of the source
water treatment under paragraph (b)(2)
of this section, or maximum permis-
sible lead and copper concentrations
for finished water entering the dis-
tribution system under paragraph (b){4)
of this section. A request for modifica-
tion by a system or other interested
party shall be in writing, explain why
the modification is appropriate, and
provide supporting documentation. The
State may modify its determination
where it concludes that such change is
necessary to ensure that the system
continues to minimize lead and copper
concentrations in source water. A re-
vised determination shall be made in
writing, set forth the new treatment
requirements, explain the "basis for the
State's decision, and provide an imple-
mentation schedule for completing the
treatment modifications.
(7) Treatment decisions by EPA in lieu
of the State. Pursuant to the procedures
in §142.19, the EPA Regional Adminis-
trator may review treatment deter-
minations made by a State under para-
graphs (b) (2), (4), or (6) of this section
467
-------
§141.84
40 CFR Ch. I (7-1-04 Edition)
and issue Federal treatment deter-
minations consistent with the require-
ments of those paragraphs where the
Administrator finds that:
(i) A State has failed to issue a treat-
ment determination by the applicable
deadlines contained in §141.83(a),
(ii) A state has abused its discretion
in a substantial number of cases or in
cases affecting a substantial popu-
lation, or
(iii) The technical aspects of a
State's determination would be inde-
fensible in an expected Federal enforce-
ment action taken against a system.
§ 141.84 Lead service line replacement
requirements.
(a) Systems that fail to meet the lead
action level in tap samples taken pur-
suant to §141,86(d)(2), after installing
corrosion control and/or source water
treatment (whichever sampling occurs
later), shall replace lead service lines
in accordance with the requirements of
this section. If a system is in violation
of §141.81 or §141.83 for failure to install
source water or corrosion control
treatment, the State may require the
system to commence lead service line
replacement under this section after
the date by which the system was re-
quired to conduct monitoring under
§141.86(d)(2) has passed.
(b) A water system shall replace an-
nually at least ^ percent of the initial
number of lead service lines in its dis-
tribution system. The initial number of
lead service lines is the number of lead
lines in place at the time the replace-
ment program begins. The system shall
identify the initial number of lead
service lines in its distribution system,
including an identification of the por-
tion(s) owned by the system, based on
a materials evaluation, including the
evaluation required under §141.86(a)
and relevant legal authorities (e.g.,
contracts, local ordinances) regarding
the portion owned by the system. The
first year of lead service line replace-
ment shall begin on the date the action
level was exceeded in tap sampling ref-
erenced in paragraph (a) of this sec-
tion.
(c) A system is not required to re-
place an individual lead service line if
the lead concentration in all service
line samples from that line, taken pur-
suant to §141.86(b)(3), is less than or
equal to 0.015 mg/L.
(d) A water system shall replace that
portion of the lead service line that it
owns. In cases where the system does
not own the entire lead service line.
the system shall notify the owner of
the line, or the owner's authorized
agent, that the system will replace the
portion of the service line that it owns
and shall offer to replace the owner's
portion of the line. A system is not re-
quired to bear the cost of replacing the
privately-owned portion of the line, nor
is it required to replace the privately-
owned portion where the owner chooses
not to pay the cost of replacing the pri-
vately-owned portion of the line, or
where replacing the privately-owned
portion would be precluded by State,
local or common law. A water system
that does not replace the entire length
of the service line also shall complete
the following tasks.
(1) At least 45 days prior to com-
mencing with the partial replacement
of a lead service line, the water system
shall provide notice to the resident(s)
of all buildings served by the line ex-
plaining that they may experience a
temporary increase of lead levels in
their drinking water, along with guid-
ance on measures consumers can take
to minimize their exposure to lead. The
State may allow the water system to
provide notice under the previous sen-
tence less than 45 days prior to com-
mencing partial lead service line re-
placement where such replacement is
in conjunction with emergency repairs.
In addition, the water system shall in-
form the resident(s) served by the line
that the system will, at the system's
expense, collect a sample from each
partially-replaced lead service line
that is representative of the water in
the service line for analysis of lead
content, as prescribed under
§141.86(b)(3), within 72 hours after the
completion of the partial replacement
of the service line. The system shall
collect the sample and report the re-
sults of the analysis to the owner and
the resident(s) served by the line with-
in three business days of receiving the
results. Mailed notices post-marked
within three business days of receiving
the results shall be considered "on
time."
468
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Environmental Protection Agency
§141.85
(2) The water system shall provide
the information required by paragraph
(d)(l) of this section to the residents of
individual dwellings by mail or by
other methods approved by the State.
In instances where multi-family dwell-
ings are served by the line, the water
system shall have the option to post
the information at a conspicuous loca-
tion,
(e) The State shall require a system
to replace lead service lines on a short-
er schedule than that required by this
section, taking into account the num-
ber of lead service lines in the system,
where such a shorter replacement
schedule is feasible. The State shall
make this determination in writing
and notify the system of its finding
within 6 months after the system is
triggered into lead service line replace-
ment based on monitoring referenced
in paragraph (a) of this section.
(f) Any system may cease replacing
lead service lines whenever first draw
samples collected pursuant to
§141.88(b)(2) meet the lead action level
during each of two consecutive moni-
toring" periods and the system submits
the results to the State. If first draw
tap samples collected in any such sys-
tem thereafter exceeds the lead action
level, the system shall recommence re-
placing lead service lines pursuant to
paragraph (b) of this section.
(g) To demonstrate compliance with
paragraphs (a) through (d) of this sec-
tion, a system shall report to the State
the information specified in §141.90(e).
[56 FR 26548, June 7, 1991: 87 PR 28788, June
29. 1992, as amended at 65 FR 2005. Jan. 12,
2000]
§ 141.85 Public education and supple-
mental monitoring requirements.
A water system that exceeds the lead
action level based on tap water samples
collected in accordance with §141.86
shall deliver the public education ma-
terials contained in paragraphs (a) and
(b) of this section in accordance with
the requirements in paragraph (c) of
this section.
(a) Content of written public education
materials. (1) Community water systems,
A community water system shall in-
clude the following text in all of the
printed materials it distributes
through its lead public education pro-
gram. Systems may delete information
pertaining to lead service lines, upon
approval by the State, if no lead serv-
ice lines exist anywhere in the water
system service area. Public education
language at paragraphs (a)(ll(iv)(B)(5)
and (a)(l)(iv)(D)(2) of this section may
be modified regarding building permit
record availability and consumer ac-
cess to these records, if approved by
the State. Systems may also continue
to utilize pre-printed materials that
meet the public education language re-
quirements in 40 OFB 141.85, effective
November 6, 1991, and contained in the
40 CFR, parts 100 to 149, edition revised
as of July 1. 1991. Any additional infor-
mation presented by a system shall be
consistent with the information below
and be in plain English that can be un-
derstood by lay people.
(1) Introduction. The United States
Environmental Protection Agency
(EPA) and [insert name of water sup-
plier] are concerned about lead in your
drinking water. Although most homes
have very low levels of lead in their
drinking water, some homes in the
community have lead levels above the
EPA action level of 15 parts per billion
(ppb), or 0.015 milligrams of lead per
liter of water (mg/L), Under Federal
law we are required to have a program
in place to minimize lead in your
drinking water by [insert date when
corrosion control will be completed for
your system]. This program includes
corrosion control treatment, source
water treatment, and public education.
We are also required to replace the por-
tion of each lead service line that we
own if the line contributes lead con-
centrations of more than 15 ppb after
we have completed the comprehensive
treatment program. If you have any
questions about how we are carrying
out the requirements of the lead regu-
lation please give us a call at [insert
water system's phone number]. This
brochure explains the simple steps you
can take to protect you and your fam-
ily by reducing your exposure to lead
in drinking water.
(ii) Health effects of lead. Lead is a
common metal found throughout the
environment in lead-based paint, air,
soil, household dust, food, certain
types of pottery porcelain and pewter,
and water. Lead can pose a significant
469
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§141.85
40 CFR Ch. I (7-1-04 Edition)
risk to your health if too much of it
enters your body. Lead builds up in the
body over many years and can cause
damage to the brain, red blood cells
and kidneys. The greatest risk is to
young children and pregnant women.
Amounts of lead that won't hurt adults
can slow down normal mental and
physical development of growing bod-
ies. In addition, a child at play often
comes into contact with sources of lead
contamination—like dirt and dust—
that rarely affect an adult. It is impor-
tant to wash children's hands and toys
often, and to try to make sure they
only pub food in. their mouths.
(iii) Lead in drinking water, (A) Lead
in drinking water, although rarely the
sole cause of lead poisoning, can sig-
nificantly increase a person's total lead
exposure, particularly the exposure of
infants who drink baby formulas and
concentrated juices that are mixed
with water. The EPA estimates that
drinking water can make up 20 percent
or more of a person's total exposure to
lead.
(B) Lead is unusual among drinking
water contaminants in that it seldom
occurs naturally in water supplies like
rivers and lakes. Lead enters drinking
water primarily as a result of the cor-
rosion, or wearing away, of materials
containing lead in the water distribu-
tion system and household plumbing.
These materials include lead-based sol-
der used to join copper pipe, brass and
chrome plated brass faucets, and in
some cases, pipes made of lead that
connect your house to the water main
(service lines). In 1986, Congress banned
the use of lead solder containing great-
er than 0.2% lead, and restricted the
lead content of faucets, pipes and other
plumbing materials to 8.0%.
(O) When water stands in lead pipes
or plumbing systems containing lead
for several hours or more, the lead may
dissolve into your drinking water. This
means the first water drawn from the
tap in the morning, or later in the
afternoon after returning from work or
school, can contain fairly high levels of
lead.
(iv) Steps you can take in the home to
reduce exposure to lead in drinking water.
(A) Despite our best efforts mentioned
earlier to control water corrosivity and
remove lead from the water supply,
lead levels in some homes or buildings
can be high. To find out whether you
need to take action in your own home,
have your drinking water tested to de-
termine if it contains excessive con-
centrations of lead. Testing the water
is essential because you cannot see,
taste, or smell lead in drinking water.
Some local laboratories that can pro-
vide this service are listed at the end of
this booklet. For more information on
having your water tested, please call
[insert phone number of water system].
(B) If a water test indicates that the
drinking water drawn from a tap in
your home contains lead above 15 ppb.
then you should take the following pre-
cautions:
(I) Let the water run from the tap be-
fore using it for drinking or cooking
any time the water in a faucet has
gone unused for more than six hours.
The longer water resides in your
home's plumbing the more lead it may
contain. Flushing the tap means run-
ning the cold water faucet until the
water gets noticeably colder, usually
about 15-30 seconds. If your house has a
lead service line to the water main,
you may have to flush the water for a
longer time, perhaps one minute, be-
fore drinking. Although toilet flushing
or showering flushes water through a
portion of your home's plumbing- sys-
tem, you still need to flush the water
in each faucet before using it for drink-
ing or cooking. Flushing tap water is a
simple and inexpensive measure you
can take to protect your family's
health. It usually uses less than one or
two gallons of water and costs less
than [insert a cost estimate based on
flushing two times a day for 30 days]
per month. To conserve water, fill a
couple of bottles for drinking water
after flushing the tap, and whenever
possible use the first flush water to
wash the dishes or water the plants. If
you live in a high-rise building, letting
the water flow before using it may not
work to lessen your risk from lead. The
plumbing systems have more, and
sometimes larger pipes than smaller
buildings. Ask your landlord for help in
locating the source of the lead and for
advice on reducing the lead level.
(2) Try not to cook with, or drink
water from the hot water tap. Hot
wTater can dissolve more lead more
470
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Environmental Protection Agency
§141.85
quickly than cold water. If you need
hot water, draw water from the cold
tap and heat it on the stove.
(3) Remove loose lead solder and de-
bris from the plumbing materials in-
stalled in newly constructed homes, or
homes in which the plumbing has re-
cently been replaced, by removing the
faucet strainers from all taps and run-
ning the water from 3 to 5 minutes.
Thereafter, periodically remove the
strainers and flush out any debris that
has accumulated over time.
(4) If your copper pipes are joined
with lead solder that has been installed
illegally since it was banned in 1986,
notify the plumber who did the work
and request that he or she replace the
lead solder with lead-free solder. Lead
solder looks dull gray, and when
scratched with a key looks shiny. In
addition, notify your State [insert
name of department responsible for en-
forcing the Safe Drinking Water Act in
your State] about the violation.
(5) Determine whether or not the
service line that connects your home
or apartment to the water main is
made of lead. The best way to deter-
mine if your service line is made of
lead is by either hiring a licensed
plumber to inspect the line or by con-
tacting' the plumbing contractor who
installed the line. You can identify the
plumbing contractor by checking the
city's record of building permits which
should be maintained in the files of the
[insert name of department that issues
building permits], A licensed plumber
can at the same time check to see if
your home's plumbing contains lead
solder, lead pipes, or pipe fittings that
contain lead. The public water system
that delivers water to your home
should also maintain records of the
materials located in the distribution
system. If the service line that con-
nects your dwelling to the water main
contributes more than 15 ppb to drink-
ing water, after our comprehensive
treatment program is in place, we are
required to replace the portion of the
line we own. If the line is only par-
tially owned by the [insert the name of
the city, county, or water system that
owns the line], we are required to pro-
vide the owner of the privately-owned
portion of the line with information on
how to replace the privately-owned
portion of the service line, and offer to
replace that portion of the line at the
owner's expense. If we replace only the
portion of the line that we own, we also
are required to notify you in advance
and provide you with information on
the steps you can take to minimize ex-
posure to any temporary increase in
lead levels that may result from the
partial replacement, to take a follow-
up sample at our expense from the line
within 72 hours after the partial re-
placement, and to mail or otherwise
provide you with the results of that
sample within three business days of
receiving the results. Acceptable re-
placement alternatives include copper,
steel, iron, and plastic pipes.
(6) Have an electrician check your
wiring. If grounding wires from the
electrical system are attached to your
pipes, corrosion may be greater. Check
with a licensed electrician or your
local electrical code to determine if
your wiring can be grounded elsewhere.
DO NOT attempt to change the wiring
yourself because improper grounding
can cause electrical shock and fire haz-
ards.
(0) The steps described above will re-
duce the lead concentrations in your
drinking water. However, if a water
test indicates that the drinking water
coming from your tap contains lead
concentrations in excess of 15 ppb after
flushing, or after we have completed
our actions to minimize lead levels,
then you may want to take the fol-
lowing additional measures:
(1) Purchase or lease a home treat-
ment device. Home treatment devices
are limited in that each unit treats
only the water that flows from the fau-
cet to which it is connected, and all of
the devices require periodic mainte-
nance and replacement. Devices such
as reverse osmosis systems or distillers
can effectively remove lead from your
drinking water. Some activated carbon
filters may reduce lead levels at the
tap, however all lead reduction claims
should be investigated. Be sure to
check the actual performance of a spe-
cific home treatment device before and
after installing the unit.
(2) Purchase bottled water for drink-
ing and cooking.
(D) You can consult a variety of
sources for additional information.
471
203-160 D-16
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§141.85
40 CFR Ch. I (7-1-04 Edition)
Your family doctor or pediatrician can
perform a blood test for lead and pro-
vide you with information about the
health effects of lead. State and local
government agencies that can be con-
tacted include:
(1) [insert the name of city or county
department of public utilities] at [in-
sert phone number] can provide you
with information about your commu-
nity's water supply, and a list of local
laboratories that have been certified by
EPA for testing water quality;
(2) [insert the name of city or county
department that issues building per-
mits] at [insert phone number] can pro-
vide you with information about build-
ing' permit records that should contain
the names of plumbing' contractors
that plumbed your home; and
(3) [insert the name of the State De-
partment of Public Health] at [insert
phone number] or the [insert the name
of the city or county health depart-
ment] at [insert phone number] can
provide you with information about
the health effects of lead and how you
can have your child's blood tested.
(B) The following is a list of some
State approved laboratories in your
area that you can call to have your
water tested for lead. [Insert names
and phone numbers of at least two lab-
oratories],
(2) Non-transient non-community water
systems, A non-transient non-commu-
nity water system shall either include
the text specified in paragraph (a)(l) of
this section or shall include the fol-
lowing text in all of the printed mate-
rials it distributes through its lead
public education program. Water sys-
tems may delete information per-
taining to lead service lines upon ap-
proval by the State if no lead service
lines exist anywhere in the water sys-
tem service area. Any additional infor-
mation presented by a system shall be
consistent with the information below
and be in plain English that can be un-
derstood by lay people.
(i) Introduction. The United States
Environmental Protection Agency
(EPA) and [insert name of water sup-
plier] are concerned about lead in your
drinking water. Some drinking water
samples taken from this facility have
lead levels above the EPA action level
of 15 parts per billion (ppb), or 0.015
milligrams of lead per liter of water
(mg/L). Under Federal law we are re-
quired to have a program in place to
minimize lead in your drinking water
by [insert date when corrosion control
will be completed for your system].
This program includes corrosion con-
trol treatment, source water treat-
ment, and public education. We are
also required to replace the portion of
each lead service line that we own if
the line contributes lead concentra-
tions of more than 15 ppb after we have
completed the comprehensive treat-
ment program. If you have any ques-
tions about how we are carrying out
the requirements of the lead regulation
please give us a call at [insert water
system's phone number]. This brochure
explains the simple steps you can take
to protect yourself by reducing your
exposure to lead in drinking water.
(ii) Health effects of lead. Lead is
found throughout the environment in
lead-based paint, air, soil, household
dust, food, certain types of pottery por-
celain and pewter, and water. Lead can
pose a significant risk to your health if
too much of it enters your body. Lead
builds up in the body over many years
and can cause damage to the brain, red
blood cells and kidneys. The greatest
risk is to young children and pregnant
women. Amounts of lead that won't
hurt adults can slow down normal men-
tal and physical development of grow-
ing bodies. In addition, a child at play
often comes into contact with sources
of lead contamination—like dirt and
dust—that rarely affect an adult. It is
important to wash children's hands and
toys often, and to try to make sure
they only put food in their mouths.
(iii) Lead in drinking water. (A) Lead
in drinking water, although rarely the
sole cause of lead poisoning, can sig-
nificantly increase a person's total lead
exposure, particularly the exposure of
infants who drink baby formulas and
concentrated juices that are mixed
with water. The EPA estimates that
drinking water can make up 20 percent
or more of a person's total exposure to
lead.
(B) Lead is unusual among drinking
water contaminants in that it seldom
occurs naturally in water supplies like
rivers and lakes. Lead enters drinking
472
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Environmental Protection Agency
§141.85
water primarily as a result of the cor-
rosion, or wearing away, of materials
containing lead in the water distribu-
tion system and household plumbing.
These materials include lead-based sol-
der used to join copper pipe, brass and
chrome-plated brass faucets, and in
some cases, pipes made of lead that
connect houses and buildings to water
mains (service lines). In 1986, Congress
banned the use of lead solder con-
taining greater than 0.2% lead, and re-
stricted the lead content of faucets,
pipes and other plumbing materials to
8.0%.
(0) When water stands in lead pipes
or plumbing systems containing lead
for several hours or more, the lead may
dissolve into your drinking water. This
means the first water drawn from the
tap in the morning, or later in the
afternoon if the water has not been
used all day, can contain fairly high
levels of lead.
(iv) Steps you can take to reduce expo-
sure to lead in drinking water. (A) Let
the water run from the tap before using
it for drinking or cooking any time the
water in a faucet has gone unused for
more than six hours. The longer water
resides in plumbing the more lead it
may contain. Flushing the tap means
running the cold water faucet for about
15-30 seconds. Although toilet flushing
or showering flushes water through a
portion of the plumbing system, you
still need to flush the water in each
faucet before using it for drinking or
cooking. Flushing tap water is a simple
and inexpensive measure you can take
to protect your health. It usually uses
less than one gallon of water.
(B) Do not cook with, or drink water
from the hot water tap. Hot water can
dissolve more lead more quickly than
cold water. If you need hot water, draw
water from the cold tap and then heat
it.
(O) The steps described above will re-
duce the lead concentrations in your
drinking water. However, if you are
still concerned, you may wish to use
bottled water for drinking and cooking.
(D) You can consult a variety of
sources for additional information.
Your family doctor or pediatrician can
perform a blood test for lead and pro-
vide you with information about the
health effects of lead. State and local
government agencies that can be con-
tacted include:
(1) [insert the name or title of facil-
ity official if appropriate] at [insert
phone number] can provide you with
information about your facility's water
supply; and
(2) [insert the name or title of the
State Department of Public Health] at
[insert phone number] or the [insert
the name of the city or county health
department] at [insert phone number]
can provide you with information
about the health effects of lead.
(b) Content of broadcast materials. A
water system shall include the fol-
lowing information in all public service
announcements submitted under its
lead public education program to tele-
vision and radio stations for broad-
casting:
(1) Why should everyone want to
know the facts about lead and drinking
water? Because unhealthy amounts of
lead can enter drinking water through
the plumbing in your home. That's why
I urge you to do what I did. I had my
water tested for [insert free or $ per
sample]. You can contact the [insert
the name of the city or water system]
for information on testing and on sim-
ple ways to reduce your exposure to
lead In drinking water.
(2) To have your water tested for
lead, or to get more information about
this public health concern, please call
[insert the phone number of the city or
water system].
(c) Delivery of a public education pro-
gram. (1) In communities where a sig-
nificant proportion of the population
speaks a language other than English,
public education materials shall be
communicated in the appropriate lan-
guage(s).
(2) A community water system that
exceeds the lead action level on the
basis of tap water samples collected in
accordance with §141.86, and that is not
already repeating public education
tasks pursuant to paragraph (c)(3),
(c)(7), or (c)(8), of this section, shall,
within 60 days:
(i) Insert notices in each customer's
water utility bill containing the infor-
mation in paragraph (a)(l) of this sec-
tion, along with the following alert on
the water bill itself in large print:
"SOME HOMES IN THIS COMMUNITY
473
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§141.85
40 CFR Ch. I (7-1-04 Edffion)
HAVE ELEVATED LEAD LEVELS IN
THEIB DRINKING WATER. LEAD
CAN POSE A SIGNIFICANT RISK TO
YOUR HEALTH, PLEASE READ THE
ENCLOSED NOTICE FOR FURTHER
INFORMATION," A community water
system having a billing cycle that does
not include a billing: within 60 days of
exceeding the action level, or that can-
not insert information in the water
utility bill without making major
changes to its billing system, may use
a separate mailing to deliver the infor-
mation in paragraph (a)(l) of this sec-
tion as long as the information is deliv-
ered to each customer within 60 days of
exceeding the action level. Such water
systems shall also include the "alert"
language specified in this paragraph.
(ii) Submit the information in para-
graph (a)(l) of this section to the edi-
torial departments of the major daily
and weekly newspapers circulated
throughout the community.
(iii) Deliver pamphlets and/or bro-
chures that contain the public edu-
cation materials in paragraphs (a)(l)(ii)
and (a)(l)(iv) of this section to facili-
ties and organizations, including the
following:
(A) Public schools, and/or local
school boards;
(B) City or county health depart-
ment;
(C) Women, Infants, and Children
and/or Head Start Program(s) whenever
available;
(D) Public and private hospitals and/
or clinics;
(E) Pediatricians;
(F) Family planning clinics; and
(G) Local welfare agencies.
(iv) Submit the public service an-
nouncement in paragraph (b) of this
section to at least five of the radio and
television stations with the largest au-
diences that broadcast to the commu-
nity served by the water system.
(3) A community water system shall
repeat the tasks contained in para-
graphs (c)(2) (i), (ii) and (iii) of this sec-
tion every 12 months, and the tasks
contained in paragraphs (c)(2)(iv) of
this section every 6 months for as long
as the system exceeds the lead action
level.
(4) Within 60 days after it exceeds the
lead action level (unless it already is
repeating public education tasks pursu-
ant to paragraph (c)(5) of this section),
a non-transient non-community water
system shall deliver the public edu-
cation materials specified by para-
graph (a)(l) of this section or the public
education materials specified by para-
graph (a)(2) of this section as follows:
(i) Post informational posters on lead
in drinking water in a public place or
common area in each of the buildings
served by the system; and
(ii) Distribute informational pam-
phlets and/or brochures on lead in
drinking water to each person served
by the non-transient non-community
water system. The State may allow the
system to utilize electronic trans-
mission in lieu of or combined with
printed materials as long as it achieves
at least the same coverage.
(5) A non-transient non-community
water system shall repeat the tasks
contained in paragraph (c)(4) of this
section at least once during each cal-
endar year in which the system exceeds
the lead action level.
(6) A water system may discontinue
delivery of public education materials
if the system has met the lead action
level during the most recent six-month
monitoring period conducted pursuant
to §141.86. Such a system shall recom-
mence public education in accordance
with this section if it subsequently ex-
ceeds the lead action level during any
monitoring period.
(7) A community water system may
apply to the State, in writing, (unless
the State has waived the requirement
for prior State approval) to use the
text specified in paragraph (a)(2) of this
section in lieu of the text in paragraph
(a)(l) of this section and to perform the
tasks listed in paragraphs (c)(4) and
(c)(5) of this section in lieu of the tasks
in paragraphs (c)(2) and (c)(3) of this
section if:
(i) The system is a facility, such as a
prison or a hospital, where the popu-
lation served is not capable of or is pre-
vented from making improvements to
plumbing or installing point of use
treatment devices; and
(ii) The system provides water as
part of the cost of services provided
and does not separately charge for
water consumption.
(8)(i) A community water system
serving 3,300 or fewer people may omit
474
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Environmental Protection Agency
§141.86
the task contained in paragraph
(c)(2)(iv) of this section. As long as it
distributes notices containing the in-
formation contained in paragraph (a)(l)
of this section to every household
served by the system, such systems
may further limit their public edu-
cation programs as follows:
(A) Systems serving 500 or fewer peo-
ple may forego the task contained in
paragraph (c)(2)(ii) of this section.
Such a system may limit the distribu-
tion of the public education materials
required under paragraph (c)(2)(iii) of
this section to facilities and organiza-
tions served by the system that are
most likely to be visited regularly by
pregnant women and children, unless it
is notified by the State in writing that
it must make a broader distribution.
(B) If approved by the State in writ-
ing, a system serving 501 to 3,300 people
may omit the task in paragraph
(c)(2)(ii) of this section and/or limit the
distribution of the public education
materials required under paragraph
(c)(2)(iii) of this section to facilities
and organizations served by the system
that are most likely to be visited regu-
larly by pregnant women and children.
(ii) A community water system serv-
ing 3,300 or fewer people that delivers
public education in accordance with
paragraph (c)(8)(i) of this section shall
repeat the required public education
tasks at least once during each cal-
endar year in which the system exceeds
the lead action level.
(d) Supplemental monitoring and notifi-
cation of results. A water system that
fails to meet the lead action level on
the basis of tap samples collected in
accordance with §141.86 shall offer to
sample the tap water of any customer
who requests it. The system is not re-
quired to pay for collecting or ana-
lyzing the sample, nor is the system re-
quired to collect and analyze the sam-
ple itself.
[56 PR 26548, June 7, 1991; 5T PR 28788, June
29, 1992, as amended at 65 FR 2005, Jan. 12,
2000; 69 FR 38856, June 29, 2004]
§141.86 Monitoring requirements for
lead and copper in tap water.
(a) Sample site location. (1) By the ap-
plicable date for commencement of
monitoring under paragraph (d)(l) of
this section, each water system shall
complete a materials evaluation of its
distribution system in order to identify
a pool of targeted sampling sites that
meets the requirements of this section,
and which is sufficiently large to en-
sure that the water system can collect
the number of lead and copper tap sam-
ples required in paragraph (c) of this
section. All sites from which first draw
samples are collected shall be selected
from this pool of targeted sampling
sites. Sampling sites may not include
faucets that have point-of-use or point-
of-entry treatment devices designed to
remove inorganic contaminants.
(2) A water system shall use the in-
formation on lead, copper, and galva-
nized steel that it is required to collect
under §141.42(d) of this part [special
monitoring for corrosivity characteris-
tics] when conducting a materials eval-
uation. When an evaluation of the in-
formation collected pursuant to
§141.42(d) is insufficient to locate the
requisite number of lead and copper
sampling sites that meet the targeting
criteria in paragraph (a) of this sec-
tion, the water system shall review the
sources of information listed below in
order to identify a sufficient number of
sampling sites. In addition, the system
shall seek to collect such information
where possible in the course of its nor-
mal operations (e.g., checking service
line materials when reading water me-
ters or performing maintenance activi-
ties):
(i) All plumbing codes, permits, and
records in the files of the building de-
partment(s) which indicate the plumb-
ing materials that are installed within
publicly and privately owned struc-
tures connected to the distribution sys-
tem;
(ii) All inspections and records of the
distribution system that indicate the
material composition of the service
connections that connect a structure
to the distribution system; and
(iii) All existing water quality infor-
mation, which includes the results of
all prior analyses of the system or indi-
vidual structures connected to the sys-
tem, indicating locations that may be
particularly susceptible to high lead or
copper concentrations.
(3) The sampling sites selected for a
community water system's sampling
475
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§141.86
40 CFR Ch. 1 (7-1-04 Edition)
pool ("tier 1 sampling sites") shall con-
sist of single family structures that:
(i) Contain copper pipes with lead sol-
der installed after 1982 or contain lead
pipes; and/or
(ii) Are served by a lead service line.
When multiple-family residences com-
prise at least 20 percent of the struc-
tures served by a water system, the
system may include these types of
structures in its sampling pool.
(4) Any community water system
with insufficient tier 1 sampling sites
shall complete its sampling; pool with
"tier 2 sampling sites", consisting of
buildings, including multiple-family
residences that:
(i) Contain copper pipes with lead sol-
der installed after 1982 or contain lead
pipes; and/or
(ii) Are served by a lead service line.
(5) Any community water system
with insufficient tier 1 and tier 2 sam-
pling sites shall complete its sampling
pool with "tier 3 sampling sites", con-
sisting of single family structures that
contain copper pipes with lead solder
installed before 1983. A community
water system with insufficient tier 1,
tier 2, and tier 3 sampling sites shall
complete its sampling pool with rep-
resentative sites throughout the dis-
tribution system. For the purpose of
this paragraph, a representative site is
a site in which the plumbing materials
used at that site would be commonly
found at other sites served by the
water system.
(6) The sampling sites selected for a
non-transient noncommunity water
system ("tier 1 sampling sites") shall
consist of buildings that:
(i) Contain copper pipes with lead sol-
der installed after 1982 or contain lead
pipes; and/or
(ii) Are served by a lead service line.
(7) A non-transient non-community
water system with insufficient tier 1
sites that meet the targeting criteria
in paragraph (a)(6) of this section shall
complete its sampling pool with sam-
pling- sites that contain copper pipes
with lead solder installed before 1983. If
additional sites are needed to complete
the sampling pool, the non-transient
non-community water system shall use
representative sites throughout the
distribution system. For the purpose of
this paragraph, a representative site is
a site in which the plumbing materials
used at that site would be commonly
found at other sites served by the
water system.
(8) Any water system whose distribu-
tion system contains lead service lines
shall draw 50 percent of the samples it
collects during each monitoring period
from sites that contain lead pipes, or
copper pipes with lead solder, and 50
percent of the samples from sites
served by a lead service line. A water
system that cannot identify a suffi-
cient number of sampling sites served
by a lead service line shall collect first-
draw samples from all of the sites iden-
tified as being served by such lines.
(b) Sample collection methods. (1) All
tap samples for lead and copper col-
lected in accordance with this subpart,
with the exception of lead service line
samples collected under §141.84(c) and
samples collected under paragraph
(b)(5) of this section, shall be first-draw
samples.
(2) Bach first-draw tap sample for
lead and copper shall be one liter in
volume and have stood motionless in
the plumbing system of each sampling
site for at least six hours. First-draw
samples from residential housing shall
be collected from the cold water kitch-
en tap or bathroom sink tap. First-
draw samples from a nonresidential
building shall be one liter in volume
and shall be collected at an interior tap
from which water is typically drawn
for consumption. Non-first-draw sam-
ples collected in lieu of first-draw sam-
ples pursuant to paragraph (b)(5) of
this section shall be one liter in vol-
ume and shall be collected at an inte-
rior tap from which water is typically
drawn for consumption. First-draw
samples may be collected by the sys-
tem or the system may allow residents
to collect first-draw samples after in-
structing the residents of the sampling
procedures specified in this paragraph.
To avoid problems of residents han-
dling nitric acid, acidification of first-
draw samples may be done up to 14
days after the sample is collected.
After acidification to resolubilize the
metals, the sample must stand in the
original container for the time speci-
fied in the approved EPA method be-
fore the sample can be analyzed. If a
system allows residents to perform
476
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Environmental Protection Agency
§141.86
sampling, the system may not chal-
lenge, based on alleged errors in sam-
ple collection, the accuracy of sam-
pling results.
(3) Bach service line sample shall be
one liter in volume and have stood mo-
tionless in the lead service line for at
least six hours. Lead service line sam-
ples shall be collected in one of the fol-
lowing three ways:
(i) At the tap after flushing the vol-
ume of water between the tap and the
lead service line. The volume of water
shall be calculated based on the inte-
rior diameter and length of the pipe be-
tween the tap and the lead service line;
(ii) Tapping directly into the lead
service line; or
(iii) If the sampling site is a building
constructed as a single-family resi-
dence, allowing the water to run until
there is a significant change in tem-
perature which would be indicative of
water that has been standing in the
lead service line.
(4) A water system shall collect each
first draw tap sample from the same
sampling site from which it collected a
previous sample. If, for any reason, the
water system cannot gain entry to a
sampling site in order to collect a fol-
low-up tap sample, the system may col-
lect the follow-up tap sample from an-
other sampling site in its sampling
pool as long as the new site meets the
same targeting criteria, and is within
reasonable proximity of the original
site.
(5) A non-transient non-community
water system, or a community water
system that meets the criteria of
§§141.85(c)(7)(i) and (ii), that does not
have enough taps that can supply first-
draw samples, as defined in §141.2, may
apply to the State in writing to sub-
stitute non-first-draw samples. Such
systems must collect as many first-
draw samples from appropriate taps as
possible and identify sampling times
and locations that would likely result
in the longest standing time for the re-
maining sites. The State has the dis-
cretion to waive the requirement for
prior State approval of non-first-draw
sample sites selected by the system, ei-
ther through State regulation or writ-
ten notification to the system.
(c) Number of samples. Water systems
shall collect at least one sample during
each monitoring period specified in
paragraph (d) of this section from the
number of sites listed in the first col-
umn ("standard monitoring") of the
table in this paragraph. A system con-
ducting reduced monitoring under
paragraph (d)(4) of this section shall
collect at least one sample from the
number of sites specified in the second
column ("reduced monitoring") of the
table in this paragraph during each
monitoring period specified in para-
graph (d)(4) of this section. Such re-
duced monitoring sites shall be rep-
resentative of the sites required for
standard monitoring. States may speci-
fy sampling locations when a system is
conducting reduced monitoring. The
table is as follows:
System size (number of people served)
>100,000
10001 to 100,000 .
3.301 to 10,000
501 to 3,300
101 to 500
<100
Number
of sites
(stand-
ard
toring)
100
60
40
20
10
5
Number
of sites
(reduced
moni-
toring)
50
30
20
10
5
5
(d) Timing of monitoring—(1) Initial tap
sampling,
The first six-month monitoring pe-
riod for small, medium-size and large
systems shall begin on the following
dates:
System size (to, people served}
>50,000
3,301 to 50,000
<3,300
First six-montri nnon
January 1, 1982.
July 1, 1992,
July 1, 1993,
(i) All large systems shall monitor
during two consecutive six-month peri-
ods.
(ii) All small and medium-size sys-
tems shall monitor during each six-
month monitoring period until:
(A) The system exceeds the lead or
copper action level and is therefore re-
quired to implement the corrosion con-
trol treatment requirements under
§141.81, in which case the system shall
continue monitoring in accordance
with paragraph (d)(2) of this section, or
(B) The system meets the lead and
copper action levels during two con-
secutive six-month monitoring periods,
in which case the system may reduce
477
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§141.86
40 CFR Ch. I (7-1-04 Edition)
monitoring in accordance with para-
graph (d)(4) of this section.
(2) Monitoring after installation of cor-
rosion control and source water treat-
ment, (i) Any large system which in-
stalls optimal corrosion control treat-
ment pursuant to §141.81(d)(4) shall
monitor during two consecutive six-
month monitoring periods by the date
specified in §141.81(d)(5).
(ii) Any small or medium-size system
which installs optimal corrosion con-
trol treatment pursuant to §141.81(e)(5)
shall monitor during two consecutive
six-month monitoring periods by the
date specified in § 141.81(e)(6).
(iii) Any system which installs
source water treatment pursuant to
§141,83(a)(3) shall monitor during two
consecutive six-month monitoring pe-
riods by the date specified in
§141.83(a)(4).
(3) Monitoring after State specifies
water quality parameter values for opti-
mal corrosion control. After the State
specifies the values for water quality
control parameters under §141.82(f), the
system shall monitor during each sub-
sequent six-month monitoring period,
with the first monitoring period to
begin on the date the State specifies
the optimal values under §141.82(f).
(4) Reduced monitoring, (i) A small or
medium-size water system that meets
the lead and copper action levels dur-
ing each of two consecutive six-month
monitoring periods may reduce the
number of samples In accordance with
paragraph (c) of this section, and re-
duce the frequency of sampling to once
per year,
(ii) Any water system that maintains
the range of values for the water qual-
ity control parameters reflecting opti-
mal corrosion control treatment speci-
fied by the State under §141.82(f) during
each of two consecutive six-month
monitoring periods may reduce the fre-
quency of monitoring to once per year
and reduce the number of lead and cop-
per samples in accordance with para-
graph (c) of this section if it receives
written approval from the State. The
State shall review monitoring, treat-
ment, and other relevant information
submitted by the water system in ac-
cordance with §141.90, and shall notify
the system in writing when it deter-
mines the system is eligible to com-
mence reduced monitoring pursuant to
this paragraph. The State shall review,.
and where appropriate, revise its deter-
mination when the system submits new
monitoring or treatment data, or when
other data relevant to the number and
frequency of tap sampling becomes
available.
(ill) A small or medium-size water
system that meets the lead and copper
action levels during three consecutive
years of monitoring may reduce the
frequency of monitoring for lead and
copper from annually to once every
three years. Any water system that
maintains the range of values for the
water quality control parameters re-
flecting optimal corrosion control
treatment specified by the State under
§141.82(f) during three consecutive
years of monitoring may reduce the
frequency of monitoring from annually
to once every three years if it receives
written approval from the State. The
State shall review monitoring, treat-
ment, and other relevant information
submitted by the water system in ac-
cordance with §141.90, and shall notify
the system in writing when it deter-
mines the system is eligible to reduce
the frequency of monitoring to once
every three years. The State shall re-
view, and where appropriate, revise its
determination when the system sub-
mits new monitoring or treatment
data, or when other data relevant to
the number and frequency of tap sam-
pling becomes available.
(iv) A water system that reduces the
number and frequency of sampling
shall collect these samples from rep-
resentative sites included in the pool of
targeted sampling sites identified in
paragraph (a) of this section. Systems
sampling annually or less frequently
shall conduct the lead and copper tap
sampling during the months of June,
July, August, or September unless the
State has approved a different sam-
pling period in accordance with para-
graph (d)(4)(iv)(A) of this section.
(A) The State, at its discretion, may
approve a different period for con-
ducting the lead and copper tap sam-
pling for systems collecting a reduced
number of samples. Such a period shall
be no longer than four consecutive
months and must represent a time of
normal operation where the highest
478
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Environmental Protection Agency
§141.86
levels of lead are most likely to occur.
For a non-transient non-community
water system that does not operate
during the months of June through
September, and for which the period of
normal operation where the highest
levels of lead are most likely to occur
is not known, the State shall designate
a period that represents a time of nor-
mal operation for the system.
(B) Systems monitoring annually,
that have been collecting samples dur-
ing the months of June through Sep-
tember and that receive State approval
to alter their sample collection period
under paragraph (d)(4)(iv)(A) of this
section, must collect their next round
of samples during a time period that
ends no later than 21 months after the
previous round of sampling. Systems
monitoring triennially that have been
collecting samples during the months
of June through September, and re-
ceive State approval to alter the sam-
pling collection period as per para-
graph (d)(4)(iv)(A) of this section, must
collect their next round of samples dur-
ing a time period that ends no later
than 45 months after the previous
round of sampling. Subsequent rounds
of sampling must be collected annually
or triennially, as required by this sec-
tion. Small systems with waivers,
granted pursuant to paragraph (g) of
this section, that have been collecting
samples during the months of June
through September and receive State
approval to alter their sample collec-
tion period under paragraph
(d)(4)(iv)(A) of this section must collect
their next round of samples before the
end of the 9-year period.
(v) Any water system that dem-
onstrates for two consecutive 6-month
monitoring periods that the tap water
lead level computed under §141.80(c)(3)
is less than or equal to 0.005 mg/L and
the tap water copper level computed
under §141.80(c)(3) is less than or equal
to 0.65 mg/L may reduce the number of
samples in accordance with paragraph
(c) of this section and reduce the fre-
quency of sampling to once every three
calendar years.
(vi)(A) A small or medium-size water
system subject to reduced monitoring
that exceeds the lead or copper action
level shall resume sampling in accord-
ance with paragraph (d)(3) of this sec-
tion and collect the number of samples
specified for standard monitoring
under paragraph (c) of this section.
Such a system shall also conduct water
quality parameter monitoring in ac-
cordance with §141.87(b), (c) or (d) (as
appropriate) during the monitoring pe-
riod in which it exceeded the action
level. Any such system may resume an-
nual monitoring' for lead and copper at
the tap at the reduced number of sites
specified in paragraph (c) of this sec-
tion after it has completed two subse-
quent consecutive six-month rounds of
monitoring that meet the criteria of
paragraph (d)(4)(i) of this section and/'
or may resume triennial monitoring
for lead and copper at the reduced
number of sites after it demonstrates
through subsequent rounds of moni-
toring that it meets the criteria of ei-
ther paragraph (d)(4)(lii) or (d)(4)(v) of
this section.
(B) Any water system subject to the
reduced monitoring frequency that
fails to operate at or above the min-
imum value or within the range of val-
ues for the water quality parameters
specified by the State under §141.82(f)
for more than nine days in any six-
month period specified in §141.87(d)
shall conduct tap water sampling for
lead and copper at the frequency speci-
fied in paragraph (d)(3) of this section,
collect the number of samples specified
for standard monitoring under para-
graph (c) of this section, and shall re-
sume monitoring for water quality pa-
rameters within the distribution sys-
tem in accordance with §141.87(d). Such
a system may resume reduced moni-
toring for lead and copper at the tap
and for water quality parameters with-
in the distribution system under the
following conditions:
(1) The system may resume annual
monitoring for lead and copper at the
tap at the reduced number of sites
specified in paragraph (c) of this sec-
tion after it has completed two subse-
quent six-month rounds of monitoring
that meet the criteria of paragraph
(d)(4)(ii) of this section and the system
has received written approval from the
State that it is appropriate to resume
reduced monitoring on an annual fre-
quency.
(2) The system may resume triennial
monitoring for lead and copper at the
479
-------
§141.86
40 CFR Ch.! (7-1-04 Edition)
tap at the reduced number of sites
after it demonstrates through subse-
quent rounds of monitoring that it
meets the criteria of either paragraph
(d)(4)(iii) or (d)(4)(v) of this section and
the system has received written ap-
proval from the State that it is appro-
priate to resume triennial monitoring.
(3) The system may reduce the num-
ber of water quality parameter tap
water samples required in accordance
with § 141.87(e)(l) and the frequency
with which it collects such samples in
accordance with §141.87(e)(2). Such a
system may not resume triennial mon-
itoring for water quality parameters at
the tap until it demonstrates, in ac-
cordance with the requirements of
§141.87(e)(2), that it has re-qualified for
triennial monitoring.
(vii) Any water system subject to a
reduced monitoring frequency under
paragraph (d)(4) of this section that ei-
ther adds a new source of water or
changes any water treatment shall in-
form the State in writing in accord-
ance with §141.90(a)(3). The State may
require the system to resume sampling
in accordance with paragraph (d)(3) of
this section and collect the number of
samples specified for standard moni-
toring under paragraph (c) of this sec-
tion or take other appropriate steps
such as increased water quality param-
eter monitoring or re-evaluation of its
corrosion control treatment given the
potentially different water quality con-
siderations.
(e) Additional monitoring by systems,
The results of any monitoring con-
ducted in addition to the minimum re-
quirements of this section shall be con-
sidered by the system and the State in
making' any determinations (i.e., calcu-
lating the 90th percentile lead or cop-
per level) under this subpart.
(f) Invalidation of lead or copper tap
water samples, A sample invalidated
under this paragraph does not count to-
ward determining lead or copper 90th
percentile levels under §141.80(c)(3) or
toward meeting the minimum moni-
toring requirements of paragraph (c) of
this section.
(1) The State may invalidate a lead
or copper tap water sample at least if
one of the following conditions is met.
(i) The laboratory establishes that
improper sample analysis caused erro-
neous results.
(ii) The State determines that the
sample was taken from a site that did
not meet the site selection criteria of
this section.
(iii) The sample container was dam-
aged in transit.
(iv) There is substantial reason to be-
lieve that the sample was subject to
tampering.
(2) The system must report the re-
sults of all samples to the State and all
supporting documentation for samples
the system believes should be invali-
dated.
(3) To invalidate a sample under
paragraph (f)(l) of this section, the de-
cision and the rationale for the deci-
sion must be documented in writing.
States may not invalidate a sample
solely on the grounds that a follow-up
sample result is higher or lower than
that of the original sample.
(4) The water system must collect re-
placement samples for any samples in-
validated under this section if, after
the invalidation of one or more sam-
ples, the system has too few samples to
meet the minimum requirements of
paragraph (c) of this section. Any such
replacement samples must be taken as
soon as possible, but no later than 20
days after the date the State invali-
dates the sample or by the end of the
applicable monitoring period, which-
ever occurs later. Replacement samples
taken after the end of the applicable
monitoring period shall not also be
used to meet the monitoring require-
ments of a subsequent monitoring pe-
riod. The replacement samples shall be
taken at the same locations as the in-
validated samples or, if that is not pos-
sible, at locations other than those al-
ready used for sampling during the
monitoring period.
(g) Monitoring waivers for small sys-
tems. Any small system that meets the
criteria of this paragraph may apply to
the State to reduce the frequency of
monitoring for lead and copper under
this section to once every nine years
(i.e., a "full waiver") if it meets all of
the materials criteria specified in para-
graph (g)(l) of this section and all of
the monitoring criteria specified in
paragraph (g)(2) of this section. If State
480
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Environmental Protection Agency
§141.86
regulations permit, any small system
that meets the criteria in paragraphs
(g)(l) and (2) of this section only for
lead, or only for copper, may apply to
the State for a waiver to reduce the
frequency of tap water monitoring to
once every nine years for that contami-
nant only (i.e., a, "partial waiver").
(1) Materials criteria. The system must
demonstrate that its distribution sys-
tem and service lines and all drinking
water supply plumbing, including
plumbing conveying drinking water
within all residences and buildings con-
nected to the system, are free of lead-
containing materials and/or copper-
containing materials, as those terms
are defined in this paragraph, as fol-
lows:
(i) Lead. To qualify for a full waiver,
or a waiver of the tap water moni-
toring requirements for lead (i.e., a
"lead waiver"), the water system must
provide certification and supporting
documentation to the State that the
system is free of all lead-containing
materials, as follows:
(A) It contains no plastic pipes which
contain lead plasticizers, or plastic
service lines which contain lead plasti-
cizers; and
(B) It is free of lead service lines,
lead pipes, lead soldered pipe joints,
and leaded brass or bronze alloy fit-
tings and fixtures, unless such fittings
and fixtures meet the specifications of
any standard established pursuant to 42
U.S.C. 300g-6(e) (SDWA section 1417(e)).
(ii) Copper. To qualify for a full waiv-
er, or a waiver of the tap water moni-
toring requirements for copper (i.e., a
"copper waiver"), the water system
must provide certification and sup-
porting documentation to the State
that the system contains no copper
pipes or copper service lines.
(2) Monitoring criteria for waiver
issuance. The system must have com-
pleted at least one 6-month round of
standard tap water monitoring for lead
and copper at sites approved by the
State and from the number of sites re-
quired by paragraph (c) of this section
and demonstrate that the 90th per-
centile levels for any and all rounds of
monitoring conducted since the system
became free of all lead-containing and/
or copper-containing materials, as ap-
propriate, meet the following criteria.
(i) Lead levels. To qualify for a full
waiver, or a lead waiver, the system
must demonstrate that the 90th per-
centile lead level does not exceed 0.005
mg/L.
(ii) Copper levels. To qualify for a full
waiver, or a copper waiver, the system
must demonstrate that the 90th per-
centile copper level does not exceed
0.65 mg/L.
(3) State approval of waiver application.
The State shall notify the system of its
waiver determination, in writing, set-
ting forth the basis of its decision and
any condition of the waiver. As a con-
dition of the waiver, the State may re-
quire the system to perform specific
activities (e.g., limited monitoring,
periodic outreach to customers to re-
mind them to avoid installation of ma-
terials that might void the waiver) to
avoid the risk of lead or copper con-
centration of concern in tap water. The
small system must continue moni-
toring for lead and copper at the tap as
required by paragraphs (d)(l) through
(d)(4) of this section, as appropriate.
until it receives written notification
from the State that the waiver has
been approved.
(4) Monitoring frequency for systems
with waivers, (i) A system with a full
waiver must conduct tap water moni-
toring for lead and copper in accord-
ance with paragraph (d)(4)(iv) of this
section at the reduced number of sam-
pling sites identified in paragraph (c)
of this section at least once every nine
years and provide the materials certifi-
cation specified in paragraph (g)(l) of
this section for both lead and copper to
the State along with the monitoring
results.
(ii) A system with a partial waiver
must conduct tap water monitoring for
the waived contaminant in accordance
with paragraph (d)(4)(iv) of this section
at the reduced number of sampling
sites specified in paragraph (c) of this
section at least once every nine years
and provide the materials certification
specified in paragraph (g)(l) of this sec-
tion pertaining to the waived contami-
nant along with the monitoring re-
sults. Such a system also must con-
tinue to monitor for the non-waived
contaminant in accordance with re-
quirements of paragraph (d)(l) through
(d)(4) of this section, as appropriate.
481
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§141.86
40 CFR Ch. I (7-1-04 Edition)
(iii) If a system with a full or partial
waiver adds a new source of water or
changes any water treatment, the sys-
tem must notify the State in writing in
accordance with §141.90(a)(3). The State
has the authority to require the sys-
tem to add or modify waiver conditions
(e.g., require recertification that the
system is free of lead-containing and/or
copper-containing materials, require
additional round(s) of monitoring), if it
deems such modifications are nec-
essary to address treatment or source
water changes at the system.
(iv) If a system with a full or partial
waiver becomes aware that it is no
longer free of lead-containing or cop-
per-containing materials, as appro-
priate, (e.g., as a result of new con-
struction or repairs), the system shall
notify the State in writing no later
than 60 days after becoming aware of
such a change.
(5) Continued eligibility. If the system
continues to satisfy the requirements
of paragraph (g)(4) of this section, the
waiver will be renewed automatically,
unless any of the conditions listed in
paragraph (g)(5)(i) through (g)(5)(iii) of
this section occurs. A system whose
waiver has been revoked may re-apply
for a waiver at such time as it again
meets the appropriate materials and
monitoring criteria of paragraphs (g)(l)
and (g)(2) of this section.
(i) A system with a full waiver or a
lead waiver no longer satisfies the ma-
terials criteria of paragraph (g)(l)(i) of
this section or has a 90th percentile
lead level greater than 0.005 mg/L,.
(ii) A system with a full waiver or a
copper waiver no longer satisfies the
materials criteria of paragraph
(g)(l)(ii) of this section or has a 90th
percentile copper level greater than
0.65 mg/L.
(iii) The State notifies the system, in
writing, that the waiver has been re-
voked, setting forth the basis of its de-
cision.
(6) Requirements following waiver rev-
ocation. A system whose full or partial
waiver has been revoked by the State
is subject to the corrosion control
treatment and lead and copper tap
water monitoring requirements, as fol-
lows:
(i) If the system exceeds the lead and'
or copper action level, the system must
implement corrosion control treatment
in accordance with the deadlines speci-
fied in |141.81(e), and any other appli-
cable requirements of this subpart.
(ii) If the system meets both the lead
and the copper action level, the system
must monitor for lead and copper at
the tap no less frequently than once
every three years using the reduced
number of sample sites specified in
paragraph (c) of this section.
(7) Pre-existing waivers. Small system
waivers approved by the State in writ-
ing prior to April 11, 2000 shall remain
in effect under the following condi-
tions:
(i) If the system has demonstrated
that it is both free of lead-containing
and copper-containing materials, as re-
quired by paragraph (g)(l) of this sec-
tion and that its 90th percentile lead
levels and 90th percentile copper levels
meet the criteria of paragraph (g)(2) of
this section, the waiver remains in ef-
fect so long as the system continues to
meet the waiver eligibility criteria of
paragraph (g)(5) of this section. The
first round of tap water monitoring
conducted pursuant to paragraph (g)(4)
of this section shall be completed no
later than nine years after the last
time the system has monitored for lead
and copper at the tap.
(ii) If the system has met the mate-
rials criteria of paragraph (g)(l) of this
section but has not met the monitoring
criteria of paragraph (g)(2) of this sec-
tion, the system shall conduct a round
of monitoring for lead and copper at
the tap demonstrating that it meets
the criteria of paragraph (g)(2) of this
section no later than September 30,
2000. Thereafter, the waiver shall re-
main in effect as long as the system
meets the continued eligibility criteria
of paragraph (g)(5) of this section. The
first round of tap water monitoring
conducted pursuant to paragraph (g)(4)
of this section shall be completed no
later than nine years after the round of
monitoring conducted pursuant to
paragraph (g)(2) of this section.
[56 PR 26548, June 7, 1991; 56 PR 32113, July
15, 1991; 57 PR 28788, June 29, 1992; as amend-
ed at 65 FR 2007, Jan. 12, 2000]
482
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Environmental Protection Agency
§141.87
§ 141,87 Monitoring requirements for
water quality parameters.
All large water systems, and all
small- and medium-size systems that
exceed the lead or copper action level
shall monitor water quality param-
eters in addition to lead and copper in
accordance with this section. The re-
quirements of this section are summa-
rized in the table at the end of this sec-
tion.
(a) General requirements—(1) Sample
collection methods, (i) Tap samples shall
be representative of water quality
throughout the distribution system
taking into account the number of per-
sons served, the different sources of
water, the different treatment methods
employed by the system, and seasonal
variability. Tap sampling under this
section is not required to be conducted
at taps targeted for lead and copper
sampling under §141.86(a). [Note: Sys-
tems may find it convenient to conduct
tap sampling for water quality param-
eters at sites used for coliform sam-
pling under 40 CPE 141.21.]
(ii) Samples collected at the entry
point(s) to the distribution system
shall be from locations representative
of each source after treatment. If a sys-
tem draws water from more than one
source and the sources are combined
before distribution, the system must
sample at an entry point to the dis-
tribution system during periods of nor-
mal operating conditions (i.e., when
water is representative of all sources
being used).
(2) Number of samples, (i) Systems
shall collect two tap samples for appli-
cable water quality parameters during
each monitoring period specified under
paragraphs (b) through (e) of this sec-
tion from the following number of
sites.
System size (No. people served)
t No. of sites for
!' water quality
parameters
>100.000
10,001-100.000 .
3,301 to 10,000 .
501 to 3,300
101 to 500
2100
25
10
3
2
1
1
(ii) Except as provided in paragraph
(c)(3) of this section, systems shall col-
lect two samples for each applicable
water quality parameter at each entry
point to the distribution system during
each monitoring period specified in
paragraph (b) of this section. During
each monitoring period specified in
paragraphs (c)-(e) of this section, sys-
tems shall collect one sample for each
applicable water quality parameter at
each entry point to the distribution
system.
(b) Initial sampling All large water
systems shall measure the applicable
water quality parameters as specified
below at taps and at each entry point
to the distribution system during each
six-month monitoring period specified
in §141.86(d)(l). All small and medium-
size systems shall measure the applica-
ble water quality parameters at the lo-
cations specified below during each six-
month monitoring period specified in
§141.86(d)(l) during which the system
exceeds the lead or copper action level.
(1) At taps:
(i) PH;
(ii) Alkalinity;
(iii) Orthophosphate, when an inhib-
itor containing a phosphate compound
is used;
(iv) Silica, when an inhibitor con-
taining a silicate compound is used;
(v) Calcium;
(vi) Conductivity; and
(vii) Water temperature.
(2) At each entry point to the dis-
tribution system: all of the applicable
parameters listed in paragraph (b)(l) of
this section.
(c) Monitoring after installation of cor-
rosion control. Any large system which
installs optimal corrosion control
treatment pursuant to §141.81(d)(4)
shall measure the water quality param-
eters at the locations and frequencies
specified below during each six-month
monitoring period specified in
§141.86(d)(2)(i). Any small or medium-
size system which installs optimal cor-
rosion control treatment shall conduct
such monitoring during each six-month
monitoring period specified in
§141.86(d)(2)(ii) in which the system ex-
ceeds the lead or copper action level.
(1) At taps, two samples for:
(i) pH;
(ii) Alkalinity:
(iii) Orthophosphate, when an inhib-
itor containing a phosphate compound
is used;
483
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§141.87
40 CFR Ch. I (7-1-04 Edition)
(iv) Silica, when an inhibitor con-
taining a silicate compound is used;
(v) Calcium, when calcium carbonate
stabilization is used as part of corro-
sion control.
(2) Except as provided in paragraph
(c)(3) of this section, at each entry
point to the distribution system, at
least one sample no less frequently
than every two weeks (biweekly) for;
(i) PH;
(ii) When alkalinity is adjusted as
part of optimal corrosion control, a
reading of the dosage rate of the chem-
ical used to adjust alkalinity, and the
alkalinity concentration; and
(iii) When a corrosion inhibitor is
used as part of optimal corrosion con-
trol, a reading of the dosage rate of the
inhibitor used, and the concentration
of orthophosphate or silica (whichever
is applicable),
(3) Any ground water system can
limit entry point sampling described in
paragraph (c)(2) of this section to those
entry points that are representative of
water quality and treatment condi-
tions throughout the system. If water
from untreated ground water sources
mixes with water from treated ground
water sources, the system must mon-
itor for water quality parameters both
at representative entry points receiv-
ing treatment and representative entry
points receiving no treatment. Prior to
the start of any monitoring1 under this
paragraph, the system shall provide to
the State written information identi-
fying the selected entry points and doc-
umentation, including' information on
seasonal variability, sufficient to dem-
onstrate that the sites are representa-
tive of water quality and treatment
conditions throughout the system.
(d) Monitoring after State specifies
water quality parameter values for opti-
mal corrosion control. After the State
specifies the values for applicable
water quality control parameters re-
flecting optimal corrosion control
treatment under §141.82(0. all large
systems shall measure the applicable
water quality parameters in accord-
ance with paragraph (c) of this section
and determine compliance with the re-
quirements of §141.82(gi) every six
months with the first six-month period
to begin on the date the State specifies
the optimal values under §141,82(f).
Any small or medium-size system shall
conduct such monitoring during each
six-month period specified in this para-
graph in which the system exceeds the
lead or copper action level. For any
such small and medium-size system
that is subject to a reduced monitoring
frequency pursuant to §141.86(d)(4) at
the time of the action level exceed-
ance, the end of the applicable six-
month period under this paragraph
shall coincide with the end of the ap-
plicable monitoring period under
§141.86(d)(4). Compliance with State-
designated optimal water quality pa-
rameter values shall be determined as
specified under §141.82(g).
(e) Reduced monitoring. (1) Any water
system that maintains the range of
values for the water quality param-
eters reflecting optimal corrosion con-
trol treatment during each of two con-
secutive six-month monitoring periods
under paragraph (d) of this section
shall continue monitoring at the entry
point(s) to the distribution system as
specified in paragraph (c)(2) of this sec-
tion. Such system may collect two tap
samples for applicable water quality
parameters from the following reduced
number of sites during each six-month
monitoring period.
System size (No. of people served)
>100 000
10,001 to 100 000
3,301 to 10,000
501 to 3 300
101 to 500
-=100
Reduced No.
of sites for
water quality
parameters
10
7
3
2
1
1
(2)(i) Any water system that main-
tains the range of values for the water
quality parameters reflecting optimal
corrosion control treatment specified
by the State under §141.82(f) during
three consecutive years of monitoring
may reduce the frequency with which
it collects the number of tap samples
for applicable water quality param-
eters specified in this paragraph (e)(l)
of this section from every six months
to annually. Any water system that
maintains the range of values for the
water quality parameters reflecting op-
timal corrosion control treatment
specified by the State under §141.82(f)
484
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Environmental Protection Agency
§141.87
during three consecutive years of an-
nual monitoring under this paragraph
may reduce the frequency with which
it collects the number of tap samples
for applicable water quality param-
eters specified in paragraph (e)(l) from
annually to every three years.
(ii) A water system may reduce the
frequency with which it collects tap
samples for applicable water quality
parameters specified in paragraph (e)(l)
of this section to every three years if it
demonstrates during two consecutive
monitoring' periods that Its tap water
lead level at the 90th percentile is less
than or equal to the PQL for lead speci-
fied in §141.89 (a)(l)(ii), that its tap
water copper level at the 90th per-
centile is less than or equal to 0.65 mg/
L for copper in §141.80(c)(2), and that it
also has maintained the range of values
for the water quality parameters re-
flecting optimal corrosion control
treatment specified by the State under
§141.82(f).
(3) A water system that conducts
sampling annually shall collect these
samples evenly throughout the year so
as to reflect seasonal variability.
(4) Any water system subject to the
reduced monitoring frequency that
fails to operate at or above the min-
imum value or within the range of val-
ues for the water quality parameters
specified by the State in §141.82(f) for
more than nine days in any six-month
period specified in §141.82(g) shall re-
sume distribution system tap water
sampling in accordance with the num-
ber and frequency requirements in
paragraph (d) of this section. Such a
system may resume annual monitoring
for water quality parameters at the tap
at the reduced number of sites speci-
fied in paragraph (e)(l) of this section
after it has completed two subsequent
consecutive six-month rounds of moni-
toring that meet the criteria of that
paragraph and/or may resume triennial
monitoring for water quality param-
eters at the tap at the reduced number
of sites after it demonstrates through
subsequent rounds of monitoring that
it meets the criteria of either para-
graph (e)(2)(i) or (e)(2)(il) of this sec-
tion.
(f) Additional monitoring by systems.
The results of any monitoring con-
ducted in addition to the minimum re-
quirements of this section shall be con-
sidered by the system and the State in
making any determinations (i.e., deter-
mining concentrations of water quality
parameters) under this section or
§141.82.
SUMMARY OF MONITORING REQUIREMENTS FOR WATER QUALITY PARAMETERS 1
Monitoring period
Parameters 2
Location
Frequency
initial monitoring
After installation ot con
sion control.
After State specifies param-
eter values for optimal
corrosion control.
Reduced monitoring
i pH, alkalinity, orthophosphate or sHi- : Taps and at entry points
ca3, calcium, conductivity, tempera- ; to distribution system.
ture.
pH, alkalinity, orthophosphate or sili-
ca3, calcium *.
pH, alkalinity, dosage rate and con-
centration (if alkalinity adjusted as
part of corrosion control), inhibitor i
dosage rate and inhibitor residual5, j
pH, alkalinity, orthophosphate or sili- Taps
ca3, calcium4.
Taps
Entry point(s) to distribution
system 6.
pH, alkalinity dosage rate and con-
centration (H alkalinity adjusted as
part oi corrosion control), inhibitor
dosage rate and inhibitor residual5,
pH, alkalinity, orthophosphate or sili-
ca3, caleium4.
pH, alkalinity dosage rate and con-
centration (if alkalinity adjusted as
part of corrosion control), inhibitor
dosage rate and inhibitor residu
Entry point(s) to distribution
system 6.
Taps
Entry point(s) to distribution
system6.
Every 6 months.
Every 6 months.
No less frequently than
every two weeks.
Every 6 months.
No less frequently than
every two weeks.
Every 6 months, annually 7
or every 3 years B; re-
duced number of sites.
No less frequently than
every two weeks.
1 Table is for illustrative purposes: consult the text of this section for precise regulatory requirements.
2 Small and medium-size systems have to monitor for water quality parameters only during monitoring periods in which the
system exceeds the lead or copper action level.
3 Orthophosphate rnust be measured only when an inhibitor containing a phosphate compound is used. Silica must be meas-
ured only when an inhibitor containing silicate compound is used.
4 Calcium must be measured only when calcium carbonate stabilization is used as part of corrosion control.
485
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§141.88
40 CFR Ch. I (7-1-04 Edition)
s Inhibitor dosage rates and inhibitor residual concentrations (ortho-phosphate or silica) must be measured only when an inhib-
itor is used.
6 Ground water systems may limit monitoring to representative locations throughout the system.
7 Water systems may reduce frequency of monitoring for water quality parameters at the tap from every six months to annually
if they have maintained the range of values for water quaiity parameters reflecting optimal corrosion control during 3 consecutive
years of monitoring.
8 Water systems may further reduce the frequency of monitoring for water quaiity parameters at the tap from annually to once
every 3 years if they have maintained the range of values for water quality parameters reflecting optimal corrosion control during
3 consecutive years of annual monitoring. Water systems may accelerate to triennial monitoring for water quality parameters at
the tap if they have maintained 90th percentiie lead levels less than or equal to 0.005 mg/L, 90th percentile copper levels less
than or equal to 0.65 mg/L, and the range of water quality parameters designated by the State under §14L82(f) as representing
optimal corrosion control during two consecutive six-month monitoring periods.
[56 FR 26548, June 7, 1991; 5? FB 28788, June 29, 1993, as amended at 59 FR 33862, Jane 30, 1994;
65 FB 2010, Jan. 12, 2000]
§141.88 Monitoring requirements for
lead and copper in source water.
(a) Sample location, collection methods,
and number of samples. (1) A water sys-
tem that fails to meet the lead or cop-
per action level on the basis of tap
samples collected in accordance with
§141.86 shall collect lead and copper
source water samples in accordance
with the following requirements re-
garding sample location, number of
samples, and collection methods:
(i) Groundwater systems shall take a
minimum of one sample at every entry
point to the distribution system which
is representative of each well after
treatment (hereafter called a sampling
point). The system shall take one sam-
ple at the same sampling point unless
conditions make another sampling
point more representative of each
source or treatment plant.
(ii) Surface water systems shall take
a minimum of one sample at every
entry point to the distribution system
after any application of treatment or
in the distribution system at a point
which is representative of each source
after treatment (hereafter called a
sampling point). The system shall take
each sample at the same sampling
point unless conditions make another
sampling point more representative of
each source or treatment plant,
NOTE TO PARAGRAPH (A)(l)(n): For the pur-
poses of this paragraph, surface water sys-
tems include systems with a combination of
surface and ground sources.
(ill) If a system draws water from
more than one source and the sources
are combined before distribution, the
system must sample at an entry point
to the distribution system during peri-
ods of normal operating conditions
(i.e., when water is representative of all
sources being used).
(iv) The State may reduce the total
number of samples which must be ana-
lyzed by allowing the use of
compositing. Compositing of samples
must be done by certified laboratory
personnel. Composite samples from a
maximum of five samples are allowed,
provided that if the lead concentration
in the composite sample is greater
than or equal to 0.001 mg/L or the cop-
per concentration is greater than or
equal to 0.160 mg/L, then either:
(A) A follow-up sample shall be taken
and analyzed within 14 days at each
sampling point included in the com-
posite; or
(B) If duplicates of or sufficient quan-
tities from the original samples from
each sampling point used in the com-
posite are available, the system may
use these instead of resampling.
(2) Where the results of sampling in-
dicate an exceedance of maximum per-
missible source water levels estab-
lished under §141.83(b)(4), the State
may require that one additional sample
be collected as soon as possible after
the initial sample was taken (but not
to exceed two weeks) at the same sam-
pling point. If a State-required con-
firmation sample is taken for lead or
copper, then the results of the initial
and confirmation sample shall be aver-
aged in determining compliance with
the State-specified maximum permis-
sible levels. Any sample value below
the detection limit shall be considered
to be zero. Any value above the detec-
tion limit but below the PQL shall ei-
ther be considered as the measured
value or be considered one-half the
PQL.
(b) Monitoring frequency after system
exceeds tap water action level. Any sys-
tem which exceeds the lead or copper
action level at the tap shall collect one
486
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Environmental Protection Agency
§141.89
source water sample from each entry
point to the distribution system within
six months after the exceedance.
(c) Monitoring frequency after installa-
tion of source water treatment. Any sys-
tem which installs source water treat-
ment pursuant to §141.83(a)(3) shall col-
lect an additional source water sample
from each entry point to the distribu-
tion system during two consecutive
six-month monitoring periods by the
deadline specified in §141.83(a)(4).
(d) Monitoring frequency after State
specifies maximum permissible source
water levels or determines that source
water treatment is not needed. (1) A sys-
tem shall monitor at the frequency
specified below in cases where the
State specifies maximum permissible
source water levels under §141.83(b)(4)
or determines that the system is not
required to install source water treat-
ment under §141.83(b)(2).
(i) A water system using only
groundwater shall collect samples once
during the three-year compliance pe-
riod (as that term is defined in §141.2)
in effect when the applicable State de-
termination under paragraph (d)(l) of
this section is made. Such systems
shall collect samples once during each
subsequent compliance period.
(ii) A water system using surface
water (or a combination of surface and
groundwater) shall collect samples
once during each year, the first annual
monitoring period to begin on the date
on which the applicable State deter-
mination is made under paragraph
(d)(l) of this section.
(2) A system is not required to con-
duct source water sampling for lead
and/or copper if the system meets the
action level for the specific contami-
nant in tap water samples during the
entire source water sampling period ap-
plicable to the system under paragraph
(d)(l) (i) or (ii) of this section.
(e) Reduced monitoring frequency. (1) A
water system using only ground water
may reduce the monitoring frequency
for lead and copper in source water to
once during each nine-year compliance
cycle (as that term is defined in §141.2)
if the system meets one of the fol-
lowing criteria:
(i) The system demonstrates that fin-
ished drinking water entering the dis-
tribution system has been maintained
below the maximum permissible lead
and copper concentrations specified by
the State in §141.83(b)(4) during at least
three consecutive compliance periods
under paragraph (d)(l) of this section;
or
(ii) The State has determined that
source water treatment is not needed
and the system demonstrates that, dur-
ing at least three consecutive compli-
ance periods in which sampling was
conducted under paragraph (d)(l) of
this section, the concentration of lead
in source water was less than or equal
to 0.005 mg/L and the concentration of
copper in source water was less than or
equal to 0.65 mg/L.
(2) A water system using surface
water (or a combination of surface
water and ground water) may reduce
the monitoring frequency in paragraph
(d)(l) of this section to once during
each nine-year compliance cycle (as
that term is defined in §141.2) if the
system meets one of the following cri-
teria:
(i) The system demonstrates that fin-
ished drinking water entering the dis-
tribution system has been maintained
below the maximum permissible lead
and copper concentrations specified by
the State in §141.83(b)(4) for at least
three consecutive years; or
(ii) The State has determined that
source water treatment is not needed
and the system demonstrates that, dur-
ing at least three consecutive years,
the concentration of lead in source
water was less than or equal to 0.005
mg/L and the concentration of copper
in source water was less than or equal
to 0.65 mg/L.
(3) A water system that uses a new
source of water is not eligible for re-
duced monitoring for lead and/or cop-
per until concentrations in samples
collected from the new source during
three consecutive monitoring periods
are below the maximum permissible
lead and copper concentrations speci-
fied by the State in §141.83(a)(5).
[56 PR 26548, June 7, 1991; 57 FR 28788 and
28789, June 29, 1992, as amended at 65 FR 2012,
Jan. 12, 2000]
§ 141.89 Analytical methods.
(a) Analyses for lead, copper, pH, con-
ductivity, calcium, alkalinity,
487
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§141.90
40 CFR Ch. I (7-1-04 Edition)
orthophosphate, silica, and tempera-
ture shall be conducted with the meth-
ods in §141.23(k)(l).
(1) Analyses for alkalinity, calcium,
conductivity, orthophosphate, pH, sili-
ca, and temperature may be performed
by any person acceptable to the State.
Analyses under this section for lead
and copper shall only be conducted by
laboratories that have been certified by
EPA or the State. To obtain certifi-
cation to conduct analyses for lead and
copper, laboratories must:
(i) Analyze Performance Evaluation
samples, which include lead and cop-
per, provided by or acceptable to EPA
or the State at least once a year by
each method for which the laboratory
desires certification; and
(ii) Achieve quantitative acceptance
limits as follows:
(A) For lead: ±30 percent of the actual
amount in the Performance Evaluation
sample when the actual amount is
greater than or equal to 0.005 mg/L.
The Practical Quantitation Level, or
PQL for lead is 0.005 mg/L.
(B) For Copper: ±10 percent of the ac-
tual amount in the Performance Eval-
uation sample when the actual amount
is greater than or equal to 0,050 mg/L.
The Practical Quantitation Level, or
PQL for copper is 0.050 mg/L.
(iii) Achieve the method detection
limit for lead of 0.001 mg/L according to
the procedures in appendix B of part
136 of this title. This need only be ac-
complished if the laboratory will be
processing source water composite
samples under §141.88(a)(l)(iil).
(iv) Be currently certified by EPA or
the State to perform analyses to the
specifications described in paragraph
(a)(2) of this section.
(2) States have the authority to allow
the use of previously collected moni-
toring data for purposes of monitoring,
if the data were collected and analyzed
in accordance with the requirements of
this subpart.
(3) All lead and copper levels meas-
ured between the PQL and MDL must
be either reported as measured or they
can be reported as one-half the PQL
specified for lead and copper in para-
graph (a)(l)(ii) of this section. All lev-
els below the lead and copper MDLs
must be reported as zero.
(4) All copper levels measured be-
tween the PQL and the MDL must be
either reported as measured or they
can be reported as one-half the PQL
(0.025 mg/L). All levels below the copper
MDL must be reported as zero.
(b) [Eeserved]
[56 PR 26548, June 7, 1991, as amended at 57
FR 28789, June 29, 1992; 57 FR 31847, July 17,
1992; 59 FR 33863, June 30, 1994; 59 FR 62470,
Deo. 5, 1994; 64 FR 67466, Dec. 1, 1999; 65 FR
2012, Jan. 12, 2000]
§ 141.90 Reporting requirements.
All water systems shall report all of
the following information to the State
in accordance with this section.
(a) Reporting requirements for tap
water monitoring for lead and copper and
for water quality parameter monitoring,
(1) Except as provided in paragraph
(a)(l)(viii) of this section, a water sys-
tem shall report the information speci-
fied below for all tap water samples
specified in §141.86 and for all water
quality parameter samples specified in
§141.87 within the first 10 days fol-
lowing the end of each applicable moni-
toring period specified in §141.86 and
§141.87 (i.e., every six months, annu-
ally, every 3 years, or every 9 years):
(i) The results of all tap samples for
lead and copper including the location
of each site and the criteria under
§141.86(a) (3), (4), (5), (6), and/or (7)
under which the site was selected for
the system's sampling pool;
(ii) Documentation for each tap
water lead or copper sample for which
the water system requests invalidation
pursuant to §141.86(f)(2);
(iii) [Eeserved]
(iv) The 90th percentile lead and cop-
per concentrations measured from
among all lead and copper tap water
samples collected during each moni-
toring period (calculated in accordance
with §141.80(c)(3)), unless the State cal-
culates the system's 90th percentile
lead and copper levels under paragraph
(h) of this section;
(v) With the exception of initial tap
sampling conducted pursuant to
§141.86(d)(l), the system shall designate
any site which was not sampled during
previous monitoring periods, and in-
clude an explanation of why sampling
sites have changed;
488
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Environmental Protection Agency
§141.90
Cvi) The results of all tap samples for
pH, and where applicable, alkalinity,
calcium, conductivity, temperature,
and orthophosphate or silica collected
under § 141.87 (bMe);
(vii) The results of all samples col-
lected at the entry point(s) to the dis-
tribution system for applicable water
quality parameters under §141.87 (b)-
(e);
(viii) A water system shall report the
results of all water quality parameter
samples collected under §141.87(c)
through (f) during each six-month mon-
itoring period specified in §141.87(d)
within the first 10 days following the
end of the monitoring period unless the
State has specified a more frequent re-
porting requirement,
(2) For a non-transient non-commu-
nity water system, or a community
water system meeting the criteria of
§§141.85(c)(7)(i) and (ii), that does not
have enough taps that can provide
first-draw samples, the system must ei-
ther:
(i) Provide written documentation to
the State identifying standing times
and locations for enough non-first-draw
samples to make up its sampling pool
under §141.86(b)(5) by the start of the
first applicable monitoring period
under §141.86(d) that commences after
April 11, 2000, unless the State has
waived prior State approval of non-
first-draw sample sites selected by the
system pursuant to §141.86(b)(5); or
(ii) If the State has waived prior ap-
proval of non-first-draw sample sites
selected by the system, identify, in
writing, each site that did not meet the
six-hour minimum standing time and
the length of standing time for that
particular substitute sample collected
pursuant to §141.86(b)(5) and include
this information with the lead and cop-
per tap sample results required to be
submitted pursuant to paragraph
(a)(l)(i) of this section.
(3) No later than 60 days after the ad-
dition of a new source or any change in
water treatment, unless the State re-
quires earlier notification, a water sys-
tem deemed to have optimized corro-
sion control under §141.81(b)(3), a water
system subject to reduced monitoring
pursuant to §141.88(d)(4), or a water
system subject to a monitoring waiver
pursuant to §141.86(g), shall send writ-
ten documentation to the State de-
scribing the change. In those instances
where prior State approval of the
treatment change or new source is not
required, water systems are encouraged
to provide the notification to the State
beforehand to minimize the risk the
treatment change or new source will
adversely affect optimal corrosion con-
trol.
(4) Any small system applying for a
monitoring waiver under §141.86(g), or
subject to a waiver granted pursuant to
§141.86(g)(3). shall provide the following
information to the State in writing by
the specified deadline;
(i) By the start of the first applicable
monitoring period in §141.86(d), any
small water system applying for a
monitoring waiver shall provide the
documentation required to dem-
onstrate that it meets the waiver cri-
teria of §§141.86(g)(l) and (2).
(ii) No later than nine years after the
monitoring previously conducted pur-
suant to §141.86(g)(2) or §141,86(g)(4)(i),
each small system desiring to maintain
its monitoring waiver shall provide the
information required by §§141.86(g)(4)(i)
and (ii).
(ill) No later than 60 days after it be-
comes aware that it is no longer free of
lead-containing and'or copper-con-
taining material, as appropriate, each
small system with a monitoring waiver
shall provide written notification to
the State, setting forth the cir-
cumstances resulting in the lead-con-
taining and/or copper-containing mate-
rials being introduced into the system
and what corrective action, if any, the
system plans to remove these mate-
rials.
(iv) By October 10, 2000, any small
system with a waiver granted prior to
April 11, 2000 and that has not pre-
viously met the requirements of
§141.86(g)(2) shall provide the informa-
tion required by that paragraph.
(5) Each ground water system that
limits water quality parameter moni-
toring to a subset of entry points under
§141.87(c)(3) shall provide, by the com-
mencement of such monitoring, writ-
ten correspondence to the State that
identifies the selected entry points and
489
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§141.90
40 CFR Ch. I (7-1-04 Edition)
includes information sufficient to dem-
onstrate that the sites are representa-
tive of water quality and treatment
conditions throughout the system.
(b) Source water monitoring reporting
requirements, (1) A water system shall
report the sampling results for all
source water samples collected in ac-
cordance with §141.88 within the first 10
days following the end of each source
water monitoring period (i.e., annually,
per compliance period, per compliance
cycle) specified in §141.88.
(2) With the exception of the first
round of source water sampling con-
ducted pursuant to §141.88(b), the sys-
tem shall specify any site which was
not sampled during previous moni-
toring periods, and include an expla-
nation of why the sampling point has
changed.
(c) Corrosion control treatment report-
ing requirements. By the applicable
dates under §141.81, systems shall re-
port the following information:
(1) For systems demonstrating that
they have already optimized corrosion
control, information required in
§ 141.8Kb) (2) or (3).
(2) For systems required to optimize
corrosion control, their recommenda-
tion regarding optimal corrosion con-
trol treatment under §141.82(a).
(3) For systems required to evaluate
the effectiveness of corrosion control
treatments under §141.82(0), the infor-
mation required by that paragraph.
(4) For systems required to install
optimal corrosion control designated
by the State under §141.82(d), a letter
certifying that the system has com-
pleted installing that treatment.
(d) Source water treatment reporting re-
quirements. By the applicable dates in
§141.83, systems shall provide the fol-
lowing information to the State:
(1) If required under §141.83(b)(l),
their recommendation regarding
source water treatment;
(2) For systems required to install
source water treatment under
§141.83(b)(2), a letter certifying that
the system has completed installing
the treatment designated by the State
within 24 months after the State des-
ignated the treatment.
(e) Lead service line replacement report-
ing requirements. Systems shall report
the following information to the State
to demonstrate compliance with the re-
quirements of §141.84:
(1) Within 12 months after a system
exceeds the lead action level in sam-
pling referred to in §141.84(a), the sys-
tem shall demonstrate in writing to
the State that it has conducted a mate-
rial evaluation, including the evalua-
tion in §l41.86(a), to identify the initial
number of lead service lines in its dis-
tribution system, and shall provide the
State with the system's schedule for
replacing annually at least 7 percent of
the initial number of lead service lines
in its distribution system.
(2) Within 12 months after a system
exceeds the lead action level in sam-
pling referred to in §141.84(a), and
every 12 months thereafter, the system
shall demonstrate to the State in writ-
ing that the system has either:
(i) Replaced in the previous 12
months at least 7 percent of the initial
lead service lines (or a greater number
of lines specified by the State under
§141,84(e)) in its distribution system, or
(ii) Conducted sampling which dem-
onstrates that the lead concentration
in all service line samples from an indi-
vidual line(s), tafeen pursuant to
§141.86(b)(3), is less than or equal to
0.015 mg/L. In such cases, the total
number of lines replaced and/or which
meet the criteria in §141.84(c) shall
equal at least 7 percent of the initial
number of lead lines identified under
paragraph (a) of this section (or the
percentage specified by the State under
§141.84(6)).
(3) The annual letter submitted to
the State under paragraph (e)(2) of this
section shall contain the following in-
formation:
(i) The number of lead service lines
scheduled to be replaced during the
previous year of the system's replace-
ment schedule;
(ii) The number and location of each
lead service line replaced during the
previous year of the system's replace-
ment schedule;
(iii) If measured, the water lead con-
centration and location of each lead
service line sampled, the sampling
method, and the date of sampling.
(4) Any system which collects lead
service line samples following partial
lead service line replacement required
by §141.84 shall report the results to
490
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Environmental Protection Agency
§141.91
the State within the first ten days of
the month following the month in
which the system receives the labora-
tory results, or as specified by the
State. States, at their discretion may
eliminate this requirement to report
these monitoring results. Systems
shall also report any additional infor-
mation as specified by the State, and
in a time and manner prescribed by the
State, to verify that all partial lead
service line replacement activities
have taken place.
(f) Public education program reporting
requirements. (1) Any water system that
is subject to the public education re-
quirements in §141.85 shall, within ten
days after the end of each period in
which the system is required to per-
form public education tasks in accord-
ance with §141.85(c), send written docu-
mentation to the State that contains:
(i) A demonstration that the system
has delivered the public education ma-
terials that meet the content require-
ments in §141.85(a) and (b) and the de-
livery requirements in §141.85(c); and
(ii) A list of all the newspapers, radio
stations, television stations, and facili-
ties and organizations to which the
system delivered public education ma-
terials during the period in which the
system was required to perform public
education tasks.
(2) Unless required by the State, a
system that previously has submitted
the information required by paragraph
(f)(l)(ii) of this section need not resub-
mit the information required by para-
graph (f)(l)(ii) of this section, as long
as there have been no changes in the
distribution list and the system cer-
tifies that the public education mate-
rials were distributed to the same list
submitted previously.
(g) Reporting of additional monitoring
data. Any system which collects sam-
pling data in addition to that required
by this subpart shall report the results
to the State within the first ten days
following the end of the applicable
monitoring period under §§141.86, 141.87
and 141.88 during which the samples are
collected.
(h) Reporting of 90th percentile lead
and copper concentrations where the
State calculates a system's 90th percentile
concentrations. A water system is not
required to report the 90th percentile
lead and copper concentrations meas-
ured from among all lead and copper
tap water samples collected during
each monitoring period, as required by
paragraph (a)(l)(iv) of this section if:
(1) The State has previously notified
the water system that it will calculate
the water system's 90th percentile lead
and copper concentrations, based on
the lead and copper tap results sub-
mitted pursuant to paragraph (h)(2)(i)
of this section, and has specified a date
before the end of the applicable moni-
toring period by which the system
must provide the results of lead and
copper tap water samples;
(2) The system has provided the fol-
lowing information to the State by the
date specified in paragraph (h)(l) of
this section:
(i) The results of all tap samples for
lead and copper including the location
of each site and the criteria under
§141.86(a)(3), (4), (5), (6), and/or (7) under
which the site was selected for the sys-
tem's sampling pool, pursuant to para-
graph (a)(l)(i) of this section; and
(ii) An identification of sampling
sites utilized during the current moni-
toring period that were not sampled
during previous monitoring periods,
and an explanation why sampling sites
have changed; and
(3) The State has provided the results
of the 90th percentile lead and copper
calculations, in writing, to the water
system before the end of the moni-
toring period.
[56 PR 26548, June 7, 1991; 57 PR 28789, June
29, 1992, as amended at 59 FR 33864, June 30,
1994; 65 FR 2012, Jan. 12, 2000]
§ 141.91 Recordkeeping requirements.
Any system subject to the require-
ments of this subpart shall retain on
its premises original records of all
sampling data and analyses, reports,
surveys, letters, evaluations, sched-
ules, State determinations, and any
other information required by §§141.81
through 141.88. Each water system shall
retain the records required by this sec-
tion for no fewer than 12 years.
491
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§141.100
40 CFR Ch. I (7-1-04 Edition)
Subpart J—Use of Non-Centralized
Treatment Devices
SOURCE: 52 FR 25716, July 8, 1987, unless
otherwise noted.
§ 141.100 Criteria and procedures for
public water systems using point-of-
entry devices.
(a) Public water systems may use
point-of-entry devices to comply with
maximum contaminant levels only if
they meet the requirements of this
section.
(b) It is the responsibility of the
public water system to operate and
maintain the point-of-entry treatment
system.
(c) The public water system must de-
velop and obtain State approval for a
monitoring1 plan before point-of-entry
devices are installed for compliance.
Under the plan approved by the State,
point-of-entry devices must provide
health protection equivalent to central
water treatment. "Equivalent" means
that the water would meet all national
primary drinking water regulations
and would be of acceptable quality
similar to water distributed by a well-
operated central treatment plant. In
addition to the VOCs, monitoring: must
include physical measurements and ob-
servations such as total flow treated
and mechanical condition of the treat-
ment equipment.
(d) Effective technology must be
properly applied under a plan approved
by the State and the microbiological
safety of the water must be main-
tained.
(1) The State must require adequate
certification of performance, field test-
ing, and, if not included in the certifi-
cation process, a rigorous engineering
design review of the point-of-entry de-
vices.
(2) The design and application of the
point-of-entry devices must consider
the tendency for increase in
heterotrophic bacteria concentrations
in water treated with activated carbon.
It may be necessary to use frequent
backwashing, post-contactor disinfec-
tion, and Heterotrophic Plate Count
monitoring to ensure that the micro-
biological safety of the water is not
compromised.
(e) All consumers shall be protected.
Every building connected to the sys-
tem must have a point-of-entry device
installed, maintained, and adequately
monitored. The State must be assured
that every building is subject to treat-
ment and monitoring, and that the
rights and responsibilities of the public
water system customer convey with
title upon sale of property.
[52 FR 25716, July 8, 1987; 53 FR 25111, July 1,
1988]
§ 141.101 Use of bottled water.
Public water systems shall not use
bottled water to achieve compliance
with an MCL. Bottled water may be
used on a temporary basis to avoid un-
reasonable risk to health.
[63 FR 31934, June 11, 1998]
Subpart K—Treatment Techniques
SOURCE: 56 FR 3594, Jan. 30, 1991, unless
otherwise noted.
§ 141.110 General requirements.
The requirements of subpart K of this
part constitute national primary
drinking: water regulations. These reg:-
ulations establish treatment tech-
niques in lieu of maximum contami-
nant levels for specified contaminants.
§ 141.111 Treatment techniques for ac-
rylamide and epichlorohydrin.
Each public water system must cer-
tify annually in writing to the State
(using third party or manufacturer's
certification) that when acrylamide
and epichlorohydrin are used in drink-
ing water systems, the combination (or
product) of dose and monomer level
does not exceed the levels specified as
follows:
Acrylamide=0.05% dosed at 1 ppm (or equiva-
lent)
Epichlorohydrin=0.01% dosed at 20 ppm (or
equivalent)
Certifications can rely on manufactur-
ers or third parties, as approved by the
State.
492
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Environmental Protection Agency
§141.131
Subpart L—Disinfectant Residuals,
Disinfection Byproducts, and
Disinfection Byproduct Precur-
sors
§ 141.130 General requirements.
(a) The requirements of this subpart
L constitute national primary drinking
water regulations.
(1) The regulations in this subpart es-
tablish criteria under which commu-
nity water systems (CWSs) and non-
transient, noncommunity water sys-
tems (NTNCWSs) which add a chemical
disinfectant to the water in any part of
the drinking water treatment process
must modify their practices to meet
MCLs and MRDLs in §§141.64 and 141.65.
respectively, and must meet the treat-
ment technique requirements for dis-
infection byproduct precursors in
§141.135.
(2) The regulations in this subpart es-
tablish criteria under which transient
NCWSs that use chlorine dioxide as a
disinfectant or oxidant must modify
their practices to meet the MRDL for
chlorine dioxide in §141.65.
(3) EPA has established MCLs for
TTHM and HAA5 and treatment tech-
nique requirements for disinfection by-
product precursors to limit the levels
of known and unknown disinfection by-
products which may have adverse
health effects. These disinfection by-
products may include chloroform;
bromodichloromethane;
dibromochloromethane; bromoform;
dichloroacetic acid; and trichloroacetic
acid.
(b) Compliance dates. (1) CWSs and
NTNCWSs. Unless otherwise noted, sys-
tems must comply with the require-
ments of this subpart as follows. Sub-
part H systems serving 10,000 or more
persons must comply with this subpart
beginning January 1, 2002. Subpart H
systems serving- fewer than 10,000 per-
sons and systems using only ground
water not under the direct influence of
surface water must comply with this
subpart beginning January 1, 2004.
(2) Transient NCWSs. Subpart H sys-
tems serving 10,000 or more persons and
using chlorine dioxide as a disinfectant
or oxidant must comply with any re-
quirements for chlorine dioxide in this
subpart beginning January 1, 2002. Sub-
part H systems serving fewer than
10,000 persons and using chlorine diox-
ide as a disinfectant or oxidant and
systems using only ground water not
under the direct influence of surface
water and using chlorine dioxide as a
disinfectant or oxidant must comply
with any requirements for chlorine di-
oxide in this subpart beginning Janu-
ary 1, 2004.
(c) Each CWS and NTNCWS regulated
under paragraph (a) of this section
must be operated by qualified pe>--
sonnel who meet the requirements
specified by the State and are included
in a State register of qualified opera-
tors.
(d) Control of disinfectant residuals.
Notwithstanding the MRDLs in §141.65.
systems may increase residual dis-
infectant levels in the distribution sys-
tem of chlorine or chloramines (but not
chlorine dioxide) to a level and for a
time necessary to protect public
health, to address specific micro-
biological contamination problems
caused by circumstances such as, but
not limited to, distribution line breaks,
storm run-off events, source water con-
tamination events, or cross-connection
events.
[63 FR 69466, Dec. 16, 1998, as amended at 66
FR 3776, Jan. 16, 2001]
§ 141.131 Analytical requirements.
(a) General. (1) Systems must use
only the analytical method(s~) specified
in this section, or otherwise approved
by EPA for monitoring under this sub-
part, to demonstrate compliance with
the requirements of this subpart. These
methods are effective for compliance
monitoring February 16, 1999.
(2) The following documents are in-
corporated by reference. The Director
of the Federal Register approves this
incorporation by reference in accord-
ance with 5 U.S.C. 552(a) and 1 CFR
part 51. Copies may be inspected at
EPA's Drinking Water Docket, 401 M
St., SW., Washington, DC 20460, or at
the National Archives and Records Ad-
ministration (NARA). For information
on the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal register/
code of_federal regulations/
ibr locations.html. EPA Method 552.1 is
493
-------
§141.131
40 CFR Ch. I (7-1-04 Edition)
in Methods for the Determination of Or-
ganic Compounds in Drinking Water-Sup-
plement II, USEPA, August 1992, EPA/
600/R-92/129 (available through National
Information Technical Service (NTIS),
PB92-207703). EPA Methods 502.2, 524.2,
551.1, and 552.2 are in Methods for the
Determination of Organic Compounds in
Drinking Water-Supplement III, USEPA,
August 1995, EPA/600/R-95/131. (avail-
able through NTIS, PB95^261616). EPA
Method 300.0 is in Methods for the Deter-
mination of Inorganic Substances in Envi-
ronmental Samples, USEPA, August
1993, EPA/600/R-93/100. (available
through NTIS, PB94-121811), EPA Meth-
od 300.1 is titled USEPA Method 300.1,
Determination of Inorganic Anions in
Drinking Water by Ion Chromatography,
Revision 1.0, USEPA, 1997, BPA/600/B-98/
118 (available through NTIS, PB98-
169196); also available from: Chemical
Exposure Research Branch, Micro-
biological & Chemical Exposure Assess-
ment Research Division, National Ex-
posure Research Laboratory, U.S. En-
vironmental Protection Agency, Cin-
cinnati, OH 45268, Pax Number: 513-569-
7757, Phone number: 513-569-7586.
Standard Methods 4500-C1 D, 4500-C1 E,
4500-C1 P, 4500-C1 G, 4500-C1 H, 4500-C1
I, 4500-C1O-2 D, 4500-C1O2 E, 6251 B, and
5910 B shall be followed in accordance
with Standard Methods for the Examina-
tion of Water and Wastewater, 19th Edi-
tion, American Public Health Associa-
tion, 1995; copies may be obtained from
the American Public Health Associa-
tion, 1015 Fifteenth Street, NW, Wash-
ington, DC 20005. Standard Methods
5310 B, 5310 C, and 5310 D shall be fol-
lowed in accordance with the Supple-
ment to the 19th Edition of Standard
Methods for the Examination of Water
and Wastewater, American Public
Health Association, 1996; copies may be
obtained from the American Public
Health Association, 1015 Fifteenth
Street, NW, Washington. DC 20005.
ASTM Method D 1253-86 shall be fol-
lowed in accordance with the Annual
Book of ASTM Standards, Volume 11.01,
American Society for Testing and Ma-
terials, 1996 edition; copies may be ob-
tained from the American Society for
Testing and Materials, 100 Barr Harbor
Drive, West Conshohoken, PA 19428.
(b) Disinfection byproducts. (1) Sys-
tems must measure disinfection by-
products by the methods (as modified
by the footnotes) listed in the fol-
lowing- table:
APPROVED METHODS FOR DISINFECTION BYPRODUCT COMPLIANCE MONITORING
Methodology 2
P&T/GC/EICD & PID
P&T/GC/MS
LLE/GC/ECD
LLE/GC/ECD
SPE/GC/ECD
LLE/GC/ECD
Amperornetric Trtra-
tion.
1C
1C
EPA meth-
od
3502.2
524.2
551,1
552.1
552.2
300.0
300.1
Standard method
6251 B
4500-CIO, E
Byproduct measured 1
TTHM
X
X
X
HAAS
Chlorite"
X
X
X
X
X
X
Bromate
X
1 X indicates method is approved fof measuring specified disinfection byproduct.
2P&T = purge and trap; GC = gas Chromatography; E1CD= electrolytic conductivity detector; PI
S=mass spectrometer; LLE= liquid/liquid extraction; ECD=electron capture detector; SPE=so
., = photoionization detector;
= solid phase extractor; 1C = ion
romaograpy.
3 If TTHMs are the only analyles being measured in the sample, then a PID is not required
4
(2) Analysis under this section for
disinfection byproducts must be con-
ducted by laboratories that have re-
ceived certification by EPA or the
State, except as specified under para-
graph (b)(3) of this section. To receive
certification to conduct analyses for
the contaminants in §141.64(a), the lab-
oratory must carry out annual anal-
yses of performance evaluation (PE)
samples approved by EPA or the State.
In these analyses of PE samples, the
laboratory must achieve quantitative
results within the acceptance limit on
494
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Environmental Protection Agency
§141.131
a minimum of 80% of the analytes in-
cluded in each PE sample. The accept-
ance limit is defined as the 95% con-
fidence interval calculated around the
mean of the PE study data between a
maximum and minimum acceptance
limit of +/-50% and +/-15% of the
study mean.
(3) A party approved by EPA or the
State must measure daily chlorite
samples at the entrance to the dis-
tribution system.
(c) Disinfectant residuals. (1) Systems
must measure residual disinfectant
concentrations for free chlorine, com-
bined chlorine (chloramines), and chlo-
rine dioxide by the methods listed in
the following table:
APPROVED METHODS FOR DISINFECTANT RESIDUAL COMPLIANCE MONITORING
Methodology
Amperometric Titra-
tion.
Low Level Ampero-
metric Titration.
DPD Ferrous
Titrimetric.
DPD Colorimetric ..
Syringaldazin e
(FACTS).
lodometric Elec-
trode.
DPD
Amperometric
Method II.
Standard
method
4500-CI D
4500-CI E
4500-CI F
4500-CI G
4500-CI H
4500-CI 1
4500-CIO> D
4500-CIC-2 E
ASTM method
D 1253-86
Residual Measured1
Free
chlorine
X
X
X
X
Combined
chlorine
X
X
X
Total
chlorine
X
X
X
X
X
Chlorine
dioxide
X
X
1 X indicates method is approved for measuring specified disinfectant residual.
(2) If approved by the State, systems
may also measure residual disinfectant
concentrations for chlorine,
chloramines, and chlorine dioxide by
using DPD colorimetric test kits.
(3) A party approved by EPA or the
State must measure residual disinfect-
ant concentration.
(d) Additional analytical methods. Sys-
tems required to analyze parameters
not included in paragraphs (b) and (c)
of this section must use the following
methods. A party approved by EPA or
the State must measure these param-
eters.
(1) Alkalinity. All methods allowed in
§ 141.89(a) for measuring alkalinity.
(2) Bromide. EPA Method 300.0 or EPA
Method 300.1.
(3) Total Organic Carbon (TOO).
Standard Method 5310 B (High-Tem-
perature Combustion Method) or
Standard Method 5310 C (Persulfate-Ul-
traviolet or Heated-Persulfate Oxida-
tion Method) or Standard Method 5310
D (Wet-Oxidation Method). TOO sam-
ples may not be filtered prior to anal-
ysis. TOO samples must either be ana-
lyzed or must be acidified to achieve
pH less than 2.0 by minimal addition of
phosphoric or sulfuric acid as soon as
practical after sampling, not to exceed
24 hours. Acidified TOO samples must
be analyzed within 28 days.
(4) Specific Ultraviolet Absorbance
(SUVA). SUVA is equal to the UV ab-
sorption at 254nm (TJWvt) (measured in
m-1 divided by the dissolved organic
carbon (DOC) concentration (measured
as mg/L). In order to determine SUVA,
it is necessary to separately measure
UV254 and DOC. When determining
SUVA, systems must use the methods
stipulated in paragraph (d)(4)(i) of this
section to measure DOC and the meth-
od stipulated in paragraph (d)(4)(ii) of
this section to measure UV254. SUVA
must be determined on water prior to
the addition of disinfectants/oxidants
by the system. DOC and UV254 samples
used to determine a SUVA value must
be taken at the same time and at the
same location.
(i) Dissolved Organic Carbon (DOC).
Standard Method 5310 B (High-Tem-
perature Combustion Method) or
495
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§141.132
40 CFR Ch. I (7-1-04 Edition)
Standard Method 5310 C (Persulfate-Ul-
traviolet or Heated-Persulfate Oxida-
tion Method) or Standard Method 5310
D (Wet-Oxidation Method). Prior to
analysis, DOC samples must be filtered
through a 0.45 am pore-diameter filter.
Water passed through the filter prior
to filtration of the sample must serve
as the filtered blank. This filtered
blank must be analyzed using proce-
dures identical to those used for anal-
ysis of the samples and must meet the
following criteria: DOC < 0.5 mg/L. DOC
samples must be filtered through the
0.45 am pore-diameter filter prior to
acidification. DOC samples must either
be analyzed or must be acidified to
achieve pH less than 2.0 by minimal ad-
dition of phosphoric or sulfuric acid as
soon as practical after sampling, not to
exceed 48 hours. Acidified DOC samples
must be analyzed within 28 days.
(ii) Ultraviolet Absorption at 254 nm
(UV254). Method 5910 B (Ultraviolet Ab-
sorption Method). UV absorption must
be measured at 253.7 nm (may be round-
ed off to 254 nm). Prior to analysis,
UV254 samples must be filtered through
a 0.45 am pore-diameter filter. The pH
of UV254 samples may not be adjusted.
Samples must be analyzed as soon as
practical after sampling, not to exceed
48 hours.
(5) pH. All methods allowed in
§141.23(k)(l) for measuring pH.
[63 FR 69466, Dec. 16, 1998, as amended at 66
FR 3776, Jan. 16, 2001]
§ 141.132 Monitoring requirements.
(a) General requirements. (1) Systems
must take all samples during normal
operating conditions.
(2) Systems may consider multiple
wells drawing water from a single aqui-
fer as one treatment plant for deter-
mining the minimum number of TTHM
and HAA5 samples required, with State
approval in accordance with criteria
developed under §142.16(h)(5) of this
chapter.
(3) Failure to monitor in accordance
with the monitoring plan required
under paragraph (f) of this section is a
monitoring violation.
(4) Failure to monitor will be treated
as a violation for the entire period cov-
ered by the annual average where com-
pliance is based on a running annual
average of monthly or quarterly sam-
ples or averages and the system's fail-
ure to monitor makes it impossible to
determine compliance with MCLs or
MRDLs.
(5) Systems may use only data col-
lected under the provisions of this sub-
part or subpart M of this part to qual-
ify for reduced monitoring.
(b) Monitoring requirements for dis-
infection byproducts—(1) TTHMs and
HAAS—(i) Routine monitoring. Systems
must monitor at the frequency indi-
cated in the following table:
ROUTINE MONITORING FREQUENCY FOR TTHM AND HAAS
Type of system
Minimum monitoring frequency
Sample location in the distribution system
Subpart H system serving at
least 10,000 persons.
Subpart H system serving from
500 to 9,999 persons.
Subpart H system serving fewer
than 500 persons.
System using only ground
water not under direct influ-
ence of surface water using
chemical disinfectant and
serving at least 10,000 per-
sons.
Four water samples per quar-
ter per treatment plant.
One water sample per quarter
per treatment plant.
One sample per year per
treatment plant during
month of warmest water
temperature.
One water sample per quarter
per treatment plant2.
At least 25 percent of all samples collected each quarter at
locations representing maximum residence time. Remain-
ing samples taken at locations representative of at least
average residence time in the distribution system and rep-
resenting the entire distribution system, taking into account
number of persons served, different sources of water, and
different treatment methods.1
Locations representing maximum residence time.1
Locations representing maximum residence time.1 If the
sample (or average of annual samples, if more than one
sample is taken) exceeds the MCL, the system must in-
crease monitoring to one sample per treatment plant per
quarter, taken at a point reflecting the maximum residence
time in the distribution system, until the system meets cri-
teria in paragraph (b)(1 )(iv) of this section.
Locations representing maximum residence time.1
496
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Environmental Protection Agency
§141.132
ROUTINE MONITORING FREQUENCY FOR TTHM AND HAAS—Continued
Type of system
System using only ground
water not under direct influ-
ence of surface water using
chemical disinfectant and
serving fewer than 10,000
persons.
Minimum monitoring frequency
One sample per year per
treatment plant2 during
month of warmest water
temperature.
Sample location in the distribution system
Locations representing maximum residence time.1 If the
sample (or average of annual samples, if more than one
sample is taken) exceeds the MCL, the system must in-
crease monitoring to one sample per treatment plant per
quarter, taken at a point reflecting the maximum residence
time in the distribution system, until the system meets cri-
teria in paragraph (b)(1)(iv) of this section.
11f a system elects to sample more frequently than the minimum required, at least 25 percent of all samples collected each
quarter (including those taken in excess of the required frequency) must be taken at locations that represent the maximum resi-
dence time of the water in the distribution system. The remaining samples must be taken at locations representative of at least
average residence time in the distribution system.
2 Multiple wells drawing water from a single aquifer may be considered one treatment plant for determining the minimum num-
ber of samples required, with State approval in accordance with criteria developed under § 142.16(h)(5) of this chapter.
(ii) Systems may reduce monitoring,
except as otherwise provided, in ac-
cordance with the following table:
REDUCED MONITORING FREQUENCY FOR TTHM AND HAAS
If you are a ...
Subpart H system serving at
least 10,000 persons which
has a source water annual
average TOG level, before
any treatment, <4.0 mg/L.
Subpart H system serving from
500 to 9,999 persons which
has a source water annual
average TOC level, before
any treatment, <4.0 mg/L.
System using only ground
water not under direct influ-
ence of surface water using
chemical disinfectant and
serving at least 10,000 per-
sons.
System using only ground
water not under direct influ-
ence of surface water using
chemical disinfectant and
serving fewer than 10,000
persons.
You may reduce monitoring if
you have monitored at least
one year and your . . .
TTHM annual average <0.040
mg/L and HAAS annual av-
erage <0.030 mg/L.
TTHM annual average <0.040
mg/L and HAAS annual av-
erage <0.030 mg/L.
TTHM annual average <0.040
mg/L and HAAS annual av-
erage <0.030 mg/L.
TTHM annual average <0.040
mg/L and HAAS annual av-
erage <0.030 mg/L for two
consecutive years OR
TTHM annual average
<0.020 mg/L and HAAS an-
nual average <0.015 mg/L
for one year.
To this level
One sample per treatment plant per quarter at distribution
system location reflecting maximum residence time.
One sample per treatment plant per year at distribution sys-
tem location reflecting maximum residence time during
month of warmest water temperature. NOTE: Any Subpart
H system serving fewer than 500 persons may not reduce
its monitoring to less than one sample per treatment plant
per year.
One sample per treatment plant per year at distribution sys-
tem location reflecting maximum residence time during
month of warmest water temperature
One sample per treatment plant per three year monitoring
cycle at distribution system location reflecting maximum
residence time during month of warmest water tempera-
ture, with the three-year cycle beginning on January 1 fol-
lowing quarter in which system qualifies for reduced moni-
toring.
(iii) Systems that do not meet these
levels must resume monitoring at the
frequency identified in paragraph
(b)(l)(i) of this section (minimum mon-
itoring frequency column) in the quar-
ter immediately following the moni-
toring period in which the system ex-
ceeds 0.060 mg/L or 0.045 mg/L for
TTHM or HAA5 respectively. For sys-
tems using only ground water not
under the direct influence of surface
water and serving fewer than 10,000 per-
sons, if either the TTHM annual aver-
age is >0.080 mg/L or the HAA5 annual
average is >0.060 mg/L, the system
must go to the increased monitoring
identified in paragraph (b)(l)(i) of this
section (sample location column) in
the quarter immediately following the
monitoring period in which the system
exceeds 0.080 mg/L or 0.060 mg/L for
TTHMs or HAA5 respectively.
(iv) Systems on increased monitoring
may return to routine monitoring if,
after at least one year of monitoring
their TTHM annual average is <0.060
497
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§141.132
40 CFR Ch. I (7-1-04 Edition)
mg/L and their HAA5 annual average is
<0.045 mg/L.
(v) The State may return a system to
routine monitoring at the State's dis-
cretion.
(2) Chlorite. Community and nontran-
sient noncommunity water systems
using chlorine dioxide, for disinfection
or oxidation, must conduct monitoring
for chlorite.
(i) Routine monitoring. (A) Daily moni-
toring. Systems must take daily sam-
ples at the entrance to the distribution
system. For any daily sample that ex-
ceeds the chlorite MCL, the system
must take additional samples in the
distribution system the following day
at the locations required by paragraph
(b)(2)(ii) of this section, in addition to
the sample required at the entrance to
the distribution system.
(B) Monthly monitoring. Systems must
take a three-sample set each month in
the distribution system. The system
must take one sample at each of the
following locations: near the first cus-
tomer, at a location representative of
average residence time, and at a loca-
tion reflecting maximum residence
time in the distribution system. Any
additional routine sampling must be
conducted in the same manner (as
three-sample sets, at the specified loca-
tions). The system may use the results
of additional monitoring conducted
under paragraph (b)(2)(ii) of this sec-
tion to meet the requirement for moni-
toring in this paragraph.
(ii) Additional monitoring. On each day
following a routine sample monitoring
result that exceeds the chlorite MCL at
the entrance to the distribution sys-
tem, the system is required to take
three chlorite distribution system sam-
ples at the following locations: as close
to the first customer as possible, in a
location representative of average resi-
dence time, and as close to the end of
the distribution system as possible (re-
flecting maximum residence time in
the distribution system).
(iii) Reduced monitoring. (A) Chlorite
monitoring at the entrance to the dis-
tribution system required by paragraph
(b)(2)(i)(A) of this section may not be
reduced.
(B) Chlorite monitoring in the dis-
tribution system required by paragraph
(b)(2)(i)(B) of this section may be re-
duced to one three-sample set per quar-
ter after one year of monitoring where
no individual chlorite sample taken in
the distribution system under para-
graph (b)(2)(l)(B) of this section has ex-
ceeded the chlorite MCL and the sys-
tem has not been required to conduct
monitoring under paragraph (b)(2)(ii) of
this section. The system may remain
on the reduced monitoring schedule
until either any of the three individual
chlorite samples taken quarterly in the
distribution system under paragraph
(b)(2)(i)(B) of this section exceeds the
chlorite MCL or the system is required
to conduct monitoring under paragraph
(b)(2)(ii) of this section, at which time
the system must revert to routine
monitoring.
(3) Bromate—(i) Routine monitoring.
Community and nontransient non-
community systems using ozone, for
disinfection or oxidation, must take
one sample per month for each treat-
ment plant in the system using ozone.
Systems must take samples monthly
at the entrance to the distribution sys-
tem while the ozonation system is op-
erating under normal conditions.
(ii) Reduced monitoring. Systems re-
quired to analyze for bromate may re-
duce monitoring from monthly to once
per quarter, if the system dem-
onstrates that the average source
water bromide concentration is less
than 0.05 mg/L based upon representa-
tive monthly bromide measurements
for one year. The system may remain
on reduced bromate monitoring until
the running annual average source
water bromide concentration, com-
puted quarterly, is equal to or greater
than 0.05 mg/L based upon representa-
tive monthly measurements. If the
running annual average source water
bromide concentration is >0.05 mg/L,
the system must resume routine moni-
toring required by paragraph (b)(3)(i) of
this section.
(c) Monitoring requirements for dis-
infectant residuals—(1) Chlorine and
chloramines—(i) Routine monitoring.
Community and nontransient non-
community water systems that use
chlorine or chloramines must measure
the residual disinfectant level in the
distribution system at the same point
in the distribution system and at the
498
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Environmental Protection Agency
§141.132
same time as total coliforms are sam-
pled, as specified in §141.21. Subpart H
systems may use the results of residual
disinfectant concentration sampling
conducted under §141.74(b)(6)(i) for
unfiltered systems or §141.74(c)(3)(i) for
systems which filter, in lieu of taking
separate samples.
(ii) Reduced monitoring. Monitoring
may not be reduced.
(2) Chlorine dioxide—(i) Routine moni-
toring. Community, nontransient non-
community, and transient noncommu-
nity water systems that use chlorine
dioxide for disinfection or oxidation
must take daily samples at the en-
trance to the distribution system. For
any daily sample that exceeds the
MRDL, the system must take samples
in the distribution system the fol-
lowing day at the locations required by
paragraph (c)(2)(ii) of this section, in
addition to the sample required at the
entrance to the distribution system.
(ii) Additional monitoring. On each day
following a routine sample monitoring
result that exceeds the MRDL, the sys-
tem is required to take three chlorine
dioxide distribution system samples. If
chlorine dioxide or chloramines are
used to maintain a disinfectant resid-
ual in the distribution system, or if
chlorine is used to maintain a dis-
infectant residual in the distribution
system and there are no disinfection
addition points after the entrance to
the distribution system (i.e., no boost-
er chlorination), the system must take
three samples as close to the first cus-
tomer as possible, at intervals of at
least six hours. If chlorine is used to
maintain a disinfectant residual in the
distribution system and there are one
or more disinfection addition points
after the entrance to the distribution
system (i.e., booster chlorination), the
system must take one sample at each
of the following locations: as close to
the first customer as possible, in a lo-
cation representative of average resi-
dence time, and as close to the end of
the distribution system as possible (re-
flecting maximum residence time in
the distribution system).
(iii) Reduced monitoring. Chlorine di-
oxide monitoring may not be reduced.
(d) Monitoring requirements for dis-
infection byproduct precursors (DBPP).
(1) Routine monitoring. Subpart H sys-
tems which use conventional filtration
treatment (as defined in §141.2) must
monitor each treatment plant for TOO
no later than the point of combined fil-
ter effluent turbidity monitoring and
representative of the treated water. All
systems required to monitor under this
paragraph (d)(l) must also monitor for
TOC in the source water prior to any
treatment at the same time as moni-
toring for TOC in the treated water.
These samples (source water and treat-
ed water) are referred to as paired sam-
ples. At the same time as the source
water sample is taken, all systems
must monitor for alkalinity in the
source water prior to any treatment.
Systems must take one paired sample
and one source water alkalinity sample
per month per plant at a time rep-
resentative of normal operating condi-
tions and influent water quality.
(2) Reduced monitoring. Subpart H sys-
tems with an average treated water
TOC of less than 2.0 mg/L for two con-
secutive years, or less than 1.0 mg/L for
one year, may reduce monitoring for
both TOC and alkalinity to one paired
sample and one source water alkalinity
sample per plant per quarter. The sys-
tem must revert to routine monitoring
in the month following the quarter
when the annual average treated water
TOC >2.0 mg/L.
(e) Bromide. Systems required to ana-
lyze for bromate may reduce bromate
monitoring from monthly to once per
quarter, if the system demonstrates
that the average source water bromide
concentration is less than 0.05 mg/L
based upon representative monthly
measurements for one year. The sys-
tem must continue bromide monitoring
to remain on reduced bromate moni-
toring.
(f) Monitoring plans. Each system re-
quired to monitor under this subpart
must develop and implement a moni-
toring plan. The system must maintain
the plan and make it available for in-
spection by the State and the general
public no later than 30 days following
the applicable compliance dates in
§141.130(b). All Subpart H systems serv-
ing more than 3300 people must submit
a copy of the monitoring plan to the
State no later than the date of the first
report required under §141.134. The
State may also require the plan to be
499
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§141.133
40 CFR Ch. I (7-1-04 Edition)
submitted by any other system. After
review, the State may require changes
in any plan elements. The plan must
include at least the following elements.
(1) Specific locations and schedules
for collecting samples for any param-
eters included in this subpart.
(2) How the system will calculate
compliance with MCLs, MRDLs, and
treatment techniques.
(3) If approved for monitoring as a
consecutive system, or if providing
water to a consecutive system, under
the provisions of §141.29, the sampling
plan must reflect the entire distribu-
tion system.
[63 FR 69466, Dec. 16, 1998, as amended at 66
FR 3776, Jan. 16, 2001]
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, §141.132 was amended in paragraph
(a)(5) by removing the reference to "or sub-
part M of this part", effective July 29, 2004.
§ 141.133 Compliance requirements.
(a) General requirements. (1) Where
compliance is based on a running an-
nual average of monthly or quarterly
samples or averages and the system
fails to monitor for TTHM, HAAS, or
bromate, this failure to monitor will be
treated as a monitoring violation for
the entire period covered by the annual
average. Where compliance is based on
a running annual average of monthly
or quarterly samples or averages and
the system failure to monitor makes it
impossible to determine compliance
with MRDLs for chlorine and
chloramines, this failure to monitor
will be treated as a monitoring viola-
tion for the entire period covered by
the annual average.
(2) All samples taken and analyzed
under the provisions of this subpart
must be included in determining com-
pliance, even if that number is greater
than the minimum required.
(3) If, during the first year of moni-
toring under §141.132, any individual
quarter's average will cause the run-
ning annual average of that system to
exceed the MCL, the system is out of
compliance at the end of that quarter.
(b) Disinfection byproducts—(1) TTHMs
and HAAS, (i) For systems monitoring
quarterly, compliance with MCLs in
§141.64 must be based on a running an-
nual arithmetic average, computed
quarterly, of quarterly arithmetic
averages of all samples collected by the
system as prescribed by §141.132(b)(l).
(ii) For systems monitoring less fre-
quently than quarterly, systems dem-
onstrate MCL compliance if the aver-
age of samples taken that year under
the provisions of §141.132(b)(l) does not
exceed the MCLs in §141.64. If the aver-
age of these samples exceeds the MCL,
the system must increase monitoring
to once per quarter per treatment
plant and such a system is not in viola-
tion of the MCL until it has completed
one year of quarterly monitoring, un-
less the result of fewer than four quar-
ters of monitoring will cause the run-
ning annual average to exceed the
MCL, in which case the system is in
violation at the end of that quarter.
Systems required to increase moni-
toring frequency to quarterly moni-
toring must calculate compliance by
including the sample which triggered
the increased monitoring plus the fol-
lowing three quarters of monitoring.
(iii) If the running annual arithmetic
average of quarterly averages covering
any consecutive four-quarter period ex-
ceeds the MCL, the system is in viola-
tion of the MCL and must notify the
public pursuant to §141.32 or §141.202,
whichever is effective for your system,
in addition to reporting to the State
pursuant to §141.134.
(iv) If a PWS fails to complete four
consecutive quarters of monitoring,
compliance with the MCL for the last
four-quarter compliance period must
be based on an average of the available
data.
(2) Bromate. Compliance must be
based on a running annual arithmetic
average, computed quarterly, of
monthly samples (or, for months in
which the system takes more than one
sample, the average f all samples taken
during the month) collected by the sys-
tem as prescribed by §141.132(b)(3). If
the average of samples covering any
consecutive four-quarter period ex-
ceeds the MCL, the system is in viola-
tion of the MCL and must notify the
public pursuant to subpart Q, in addi-
tion to reporting to the State pursuant
to §141.134. If a PWS fails to complete
12 consecutive months' monitoring,
compliance with the MCL for the last
four-quarter compliance period must
500
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Environmental Protection Agency
§141.133
be based on an average of the available
data.
(3) Chlorite. Compliance must be
based on an arithmetic average of each
three sample set taken in the distribu-
tion system as prescribed by
§141.132(b)(2)(l)(B) and §141.132(b)(2)(ii).
If the arithmetic average of any three
sample set exceeds the MCL, the sys-
tem is in violation of the MCL and
must notify the public pursuant to sub-
part Q, in addition to reporting to the
State pursuant to §141.134.
(c) Disinfectant residuals—(1) Chlorine
and chloramines. (i) Compliance must be
based on a running annual arithmetic
average, computed quarterly, of
monthly averages of all samples col-
lected by the system under
§141.132(c)(l). If the average covering
any consecutive four-quarter period ex-
ceeds the MRDL, the system is in vio-
lation of the MRDL and must notify
the public pursuant to subpart Q, in ad-
dition to reporting to the State pursu-
ant to §141.134.
(ii) In cases where systems switch be-
tween the use of chlorine and
chloramines for residual disinfection
during the year, compliance must be
determined by including together all
monitoring results of both chlorine and
chloramines in calculating compliance.
Reports submitted pursuant to §141.134
must clearly indicate which residual
disinfectant was analyzed for each
sample.
(2) Chlorine dioxide, (i) Acute viola-
tions. Compliance must be based on
consecutive daily samples collected by
the system under §141.132(c)(2). If any
daily sample taken at the entrance to
the distribution system exceeds the
MRDL, and on the following day one
(or more) of the three samples taken in
the distribution system exceed the
MRDL, the system is in violation of
the MRDL and must take immediate
corrective action to lower the level of
chlorine dioxide below the MRDL and
must notify the public pursuant to the
procedures for acute health risks in
subpart Q in addition to reporting to
the State pursuant to §141.134. Failure
to take samples in the distribution sys-
tem the day following an exceedance of
the chlorine dioxide MRDL at the en-
trance to the distribution system will
also be considered an MRDL violation
and the system must notify the public
of the violation in accordance with the
provisions for acute violations under
subpart Q in addition to reporting to
the State pursuant to §141.134.
(ii) Nonacute violations. Compliance
must be based on consecutive daily
samples collected by the system under
§141.132(c)(2). If any two consecutive
daily samples taken at the entrance to
the distribution system exceed the
MRDL and all distribution system
samples taken are below the MRDL,
the system is in violation of the MRDL
and must take corrective action to
lower the level of chlorine dioxide
below the MRDL at the point of sam-
pling and will notify the public pursu-
ant to the procedures for nonacute
health risks in subpart Q in addition to
reporting to the State pursuant to
§141.134. Failure to monitor at the en-
trance to the distribution system the
day following an exceedance of the
chlorine dioxide MRDL at the entrance
to the distribution system is also an
MRDL violation and the system must
notify the public of the violation in ac-
cordance with the provisions for
nonacute violations under §141.32(e)(78)
in addition to reporting to the State
pursuant to §141.134.
(d) Disinfection byproduct precursors
(DBPP). Compliance must be deter-
mined as specified by § 141.135(c). Sys-
tems may begin monitoring to deter-
mine whether Step 1 TOC removals can
be met 12 months prior to the compli-
ance date for the system. This moni-
toring is not required and failure to
monitor during this period is not a vio-
lation. However, any system that does
not monitor during this period, and
then determines in the first 12 months
after the compliance date that it is not
able to meet the Step 1 requirements in
§141.135(b)(2) and must therefore apply
for alternate minimum TOC removal
(Step 2) requirements, is not eligible
for retroactive approval of alternate
minimum TOC removal (Step 2) re-
quirements as allowed pursuant to
§141.135(b)(3) and is in violation. Sys-
tems may apply for alternate min-
imum TOC removal (Step 2) require-
ments any time after the compliance
date. For systems required to meet
Step 1 TOC removals, if the value cal-
culated under §141.135(c)(l)(iv) is less
501
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§141.134
40 CFR Ch. I (7-1-04 Edition)
than 1.00, the system is in violation of
the treatment technique requirements
and must notify the public pursuant to
§141.32, in addition to reporting to the
State pursuant to §141.134.
[63 FR 69466, Dec. 16, 1998, as amended at 65
FR 26022, May 4, 2000; 65 FR 40521, June 30,
2000; 66 FR 3777, Jan. 16, 2001]
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, §141.133 was amended by revising
paragraph (a)(3), effective July 29, 2004. For
the convenience of the user, the revised text
is set forth as follows:
§ 141.133 Compliance requirements.
(a) * * *
(3) If, during the first year of monitoring
under §141.132, any individual quarter's aver-
age will cause the running annual average of
that system to exceed the MCL for total
trihalomethanes, haloacetic acids (five), or
bromate; or the MRDL for chlorine or chlor-
amine, the system is out of compliance at
the end of that quarter.
§ 141.134 Reporting and recordkeeping
requirements.
(a) Systems required to sample quar-
terly or more frequently must report
to the State within 10 days after the
end of each quarter in which samples
were collected, notwithstanding the
provisions of §141.31. Systems required
to sample less frequently than quar-
terly must report to the State within
10 days after the end of each moni-
toring period in which samples were
collected.
(b) Disinfection byproducts. Systems
must report the information specified
in the following table:
If you are a '
You must report * * *
(1) System monitoring for TTHMs and HAAS under the require-
ments of §141.132(b) on a quarterly or more frequent basis.
(2) System monitoring for TTHMs and HAAS under the require-
ments of §141.132(b) less frequently than quarterly (but as
least annually).
(3) System monitoring for TTHMs and HAAS under the
requriements of §141.132(b) less frequently than annually.
(4) System monitoring for chlorite under the requirements of
§141.132(b).
(5) System monitoring for bromate under the requirements of
§141.132(b).
(i) The number of samples taken during the last quarter.
(ii) The location, date, and result of each sample taken during
the last quarter.
(iii) The arithmetic average of all samples taken in the last
quarter.
(iv) The annual arithmetic average of the quarterly arithmetic
averages of this section for the last four quarters.
(v) Whether, based on §141.133(b)(1), the MCL was violated.
(i) The number of samples taken during the last year.
(ii) The location, date, and result of each sample taken during
the last monitoring period.
(iii) The arithmetic average of all samples taken over the last
year.
(iv) Whether, based on §141.133(b)(1), the MCL was violated.
(i) The location, date, and result of each sample taken
(ii) Whether, based on §141.133(b)(1), the MCL was violated.
(i) The number of entry point samples taken each month for
the last 3 months.
(ii) The location, date, and result of each sample (both entry
point and distribution system) taken during the last quarter.
(iii) For each month in the reporting period, the arithmetic aver-
age of all samples taken in each three samples set taken in
the distribution system.
(iv) Whether, based on §141.133(b)(3), the MCL was violated,
in which month, and how many times it was violated each
month.
(i)The number of samples taken during the last quarter.
(ii)The location, date, and result of each sample taken during
the last quarter.
(iii) The arithmetic average of the monthly arithmetic averages
of all samples taken in the last year.
(iv) Whether, based on § 141.133(b)(2), the MCL was violated.
1The State may choose to perform calculations and determine whether the MCL was exceeded, in lieu of having the system
report that information
(c) Disinfectants. Systems must report
the information specified in the fol-
lowing table:
502
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Environmental Protection Agency
§141.134
If you are a ' *
You must report * * *
(1) System monitoring for chlorine or chloramines under the re- [ (i) The number of samples laken during each month of the last
quiremenls of §l41,132(c). quarter.
I (ii) The month arithmetic average of all samples taken in each
j month for the last 12 months,
(iii) The arithmetic average of the monthly averages for the last
12 months.
(iv) Whether, based on §141,133(c}(1), the MRD was violated
(i) The dates, result, and locations of samples taken during the
last quarter.
(ii) Whether, based on §l41,133(c)(2), the MRDL was violated.
(iii) Whether the MRDL was exceeded In any two consecutive
daily samples and whether the resulting violation was acuate
or nonacute-
(2) System monitoring for chlorine dioxide under the require-
ments of §141,132(0).
1 The State may choose to perform calculations and determine whether the MRDL was exceeded, in lieu of having She system
report that information.
(d) Disinfection byproduct precursors
and enhanced coagulation or enhanced
softening. Systems must report the in-
formation specified In the following
table:
if you are a..
You must report..
(1) System monitoring monthly or quarterly for TOC under the
requirements of §14l.132(d) and required to meet the en-
hanced coagulation or enhanced softening requirements in
§141.136(b)(2)or(3).
(2) System monitoring monthly or quarterly tor TOC under the
requirements of §141.132{d) and meeting one or more of
the alternative compliance criteria in §141.13S(aX2) or (3),
-------
§141.135
40 CFR Ch. I (7-1-04 Edition)
§ 141.135 Treatment technique for con-
trol of disinfection byproduct (DBF)
precursors.
(a) Applicability. (1) Subpart H sys-
tems using conventional filtration
treatment (as defined in §141.2 ) must
operate with enhanced coagulation or
enhanced softening to achieve the TOO
percent removal levels specified in
paragraph (b) of this section unless the
system meets at least one of the alter-
native compliance criteria listed in
paragraph (a)(2) or (a)(3) of this sec-
tion,
(2) Alternative compliance criteria for
enhanced coagulation and enhanced soft-
ening systems. Subpart H systems using
conventional filtration treatment may
use the alternative compliance criteria
in paragraphs (a)(2)(i) through (vi) of
this section to comply with this sec-
tion in lieu of complying with para-
graph (b) of this section. Systems must
still comply with monitoring require-
ments in §141.132(d).
(i) The system's source water TOO
level, measured according to
§141.131(d)(3), is less than 2.0 mg/L, cal-
culated quarterly as a running annual
average.
(ii) The system's treated water TOG
level, measured according to
§ 141.131(d)(3), is less than 2.0 mg/L, cal-
culated quarterly as a running annual
average.
(iii) The system's source water TOC
level, measured according to
§141.131(d)(3), is less than 4.0 mg/L, cal-
culated quarterly as a running annual
average; the source water alkalinity,
measured according to §141.131(d)(l), is
greater than 60 mg/L (as CaCO.0, cal-
culated quarterly as a running annual
average; and either the TTHM and
HAA5 running annual averages are no
greater than 0.040 mg/L and 0.030 mg/L,
respectively; or prior to the effective
date for compliance in §141.130(b), the
system has made a clear and irrev-
ocable financial commitment not later
than the effective date for compliance
in §141.130(b) to use of technologies
that will limit the levels of TTHMs and
HAA5 to no more than 0.040 mg/L and
0.030 mg/L, respectively. Systems must
submit evidence of a clear and irrev-
ocable financial commitment, in addi-
tion to a schedule containing mile-
stones and periodic progress reports for
installation and operation of appro-
priate technologies, to the State for
approval not later than the effective
date for compliance in §141.130(b).
These technologies must be installed
and operating not later than June 30,
2005. Failure to install and operate
these technologies by the date in the
approved schedule will constitute a
violation of National Primary Drink-
ing Water Regulations.
(iv) The TTHM and HAA5 running an-
nual averages are no greater than 0.040
mg/L and 0.030 mg/L, respectively, and
the system uses only chlorine for pri-
mary disinfection and maintenance of
a residual in the distribution system.
(v) The system's source water SUVA,
prior to any treatment and measured
monthly according to §141,131(d)(4), is
less than or equal to 2.0 L/mg-m, cal-
culated quarterly as a running annual
average.
(vi) The system's finished water
SUVA, measured monthly according to
§141,131(d)(4), is less than or equal to
2.0 L/mgr-m, calculated quarterly as a
running annual average.
(3) Additional alternative compliance
criteria for softening systems. Systems
practicing enhanced softening that
cannot achieve the TOC removals re-
quired by paragraph (b)(2) of this sec-
tion may use the alternative compli-
ance criteria in paragraphs (a)(3)(i) and
(ii) of this section in lieu of complying
with paragraph (b) of this section. Sys-
tems must still comply with moni-
toring requirements in §141.132(d).
(i) Softening that results in lowering
the treated water alkalinity to less
than 60 mg/L (as CaCO3), measured
monthly according to §141.131(d)(l) and
calculated quarterly as a running an-
nual average.
(ii) Softening that results in remov-
ing at least 10 mg/L of magnesium
hardness (as CaCOa), measured monthly
and calculated quarterly as an annual
running average.
(b) Enhanced coagulation and en-
hanced softening performance require-
ments. (1) Systems must achieve the
percent reduction of TOC specified in
paragraph (b)(2) of this section between
the source water and the combined fil-
ter effluent, unless the State approves
504
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Environmental Protection Agency
§141.135
a system's request for alternate min-
imum TOO removal (Step 2) require-
ments under paragraph (b)(3) of this
section,
(2) Required Step 1 TOO reductions,
indicated in the following table, are
based upon specified source water pa-
STEP 1 REQUIRED REMOVAL OF TOO BY ENHANCED COAGULATION AND ENHANCED SOFTENING FOR
SUBPART H SYSTEMS USING CONVENTIONAL TREATMENT '2
rameters measured in accordance with
§141.131(d). Systems practicing soft-
ening are required to meet the Step 1
TOO reductions in the far-right column
(Source water alkalinity >120 mg/L) for
the specified source water TOG:
Source-water
TOO, mg/L
>20-40
>4. 0-6.0
>8.0
Source-waler alkalinity, mg/L as CaCO .1
(in precentages)
0-60
35.0
45.0
50.0
>60-120
25.0
35.0
40.0
>120~-
15.0
25.0
30.0
1 Systems meeting at least one of the conditions in paragraph (a)(2)(i)-(vi) of this section are not required to operate with en-
hanced coagulation.
2 Softening system meeting one of the alternative compliance criteria in paragraph (aX3) of this section are not required to op-
erate with enhanced softening.
3System practicing softening must meet the TOC removal requirements in this column.
(3) Subpart H conventional treatment
systems that cannot achieve the Step 1
TOC removals required by paragraph
(b)(2) of this section due to water qual-
ity parameters or operational con-
straints must apply to the State, with-
in three months of failure to achieve
the TOC removals required by para-
graph (b)(2) of this section, for approval
of alternative minimum TOC (Step 2)
removal requirements submitted by
the system. If the State approves the
alternative minimum TOC removal
(Step 2) requirements, the State may
make those requirements retroactive
for the purposes of determining compli-
ance. Until the State approves the al-
ternate minimum TOC removal (Step
2) requirements, the system must meet
the Step 1 TOC removals contained in
paragraph (b)(2) of this section.
(4) Alternate minimum TOC removal
(Step 2) requirements. Applications made
to the State by enhanced coagulation
systems for approval of alternate min-
imum TOC removal (Step 2) require-
ments under paragraph (b)(3) of this
section must include, at a minimum,
results of bench- or pilot-scale testing
conducted under paragraph (b)(4)(i) of
this section. The submitted bench- or
pilot-scale testing must be used to de-
termine the alternate enhanced coagu-
lation level.
(i) Alternate enhanced coagulation level
is defined as coagulation at a coagulant
dose and pH as determined by the
method described in paragraphs
(b)(4)(i) through (v) of this section such
that an incremental addition of 10 mg/
L of alum (or equivalent amount of fer-
ric salt) results in a TOC removal of <
0,3 mg/L. The percent removal of TOC
at this point on the "TOC removal
versus coagulant dose" curve is then
defined as the minimum TOC removal
required for the system. Once approved
by the State, this minimum require-
ment supersedes the minimum TOC re-
moval required by the table in para-
graph (b)(2) of this section. This re-
quirement will be effective until such
time as the State approves a new value
based on the results of a new bench-
and pilot-scale test. Failure to achieve
State-set alternative minimum TOC
removal levels is a violation of Na-
tional Primary Drinking Water Regu-
lations.
(ii) Bench- or pilot-scale testing of
enhanced coagulation must be con-
ducted by using representative water
samples and adding 10 mg/L increments
of alum (or equivalent amounts of fer-
ric salt) until the pH is reduced to a
level less than or equal to the enhanced
coagulation Step 2 target pH shown in
the following table:
ENHANCED COAGULATION STEP 2 TARGET pH
Alkalinity (mg/L as CaCOj)
Target pH
0-60
>6Q-12u ...
>120-240 .
5.5
6.3
7.0
505
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§141.135
40 CFR Ch, I (7-1-04 Edition)
ENHANCED COAGULATION STEP 2 TARGET PH-
Continued
>240 ..
Alkalinity (mg/L as CaCO3)
Target pH
7.5
(ill) For waters with alkalinities of
less than 60 mg/L for which addition of
small amounts of alum or equivalent
addition of iron coagulant drives the
pH below 5.5 before significant TOG re-
moval occurs, the system must add
necessary chemicals to maintain the
pH between 5.3 and 5.7 in samples until
the TOO removal of 0.3 mg/L per 10 mg/
L alum added (or equivalant addition
of iron coagulant) is reached.
(iv) The system may operate at any
coagulant dose or pH necessary (con-
sistent with other NPDWRs) to achieve
the minimum TOO percent removal ap-
proved under paragraph (b)(3) of this
section.
(v) If the TOO removal is consistently
less than 0.3 mg/L of TOO per 10 mg/L
of incremental alum dose at all dosages
of alum (or equivalant addition of iron
coagulant), the water is deemed to con-
tain TOO not amenable to enhanced co-
agulation. The system may then apply
to the State for a waiver of enhanced
coagulation requirements.
(c) Compliance calculations. (1) Sub-
part H systems other than those identi-
fied in paragraph (a)(2) or (a)(3) of this
section must comply with require-
ments contained in paragraph (b)(2) or
(b)(3) of this section. Systems must cal-
culate compliance quarterly, beginning
after the system has collected 12
months of data, by determining an an-
nual average using the following meth-
od:
(i) Determine actual monthly TOO
percent removal, equal to:
(1—(treated water TOO/source water
TOO)) * 100
(ii) Determine the required monthly
TOO percent removal (from either the
table in paragraph (b)(2) of this section
or from paragraph (b)(3) of this sec-
tion).
(iii) Divide the value in paragraph
(c)(l)(i) of this section by the value in
paragraph (c)(l)(ii) of this section.
(iv) Add together the results of para-
graph (c)(l)(iii) of this section for the
last 12 months and divide by 12.
(v) If the value calculated in para-
graph (c)(l)(iv) of this section is less
than 1,00, the system is not in compli-
ance with the TOO percent removal re-
quirements.
(2) Systems may use the provisions in
paragraphs (c)(2)(i) through (v) of this
section in lieu of the calculations in
paragraph (c)(l)(i) through (v) of this
section to determine compliance with
TOO percent removal requirements.
(i) In any month that the system's
treated or source water TOO level,
measured according to §141.131(d)(3), is
less than 2.0 mg/L, the system may as-
sign a monthly value of 1.0 (in lieu of
the value calculated in paragraph
(e)(l)(iii) of this section) when calcu-
lating compliance under the provisions
of paragraph (c)(l) of this section.
(ii) In any month that a system prac-
ticing softening removes at least 10 mg/
L of magnesium hardness (as OaCOs),
the system may assign a monthly
value of 1.0 (In lieu of the value cal-
culated in paragraph (c)(l)(iii) of this
section) when calculating compliance
under the provisions of paragraph (o)(l)
of this section.
(iii) In any month that the system's
source water SUVA, prior to any treat-
ment and measured according to
§141.131(d)(4), is <2.0 L/mg-m, the sys-
tem may assign a monthly value of 1.0
(in lieu of the value calculated in para-
graph (c)(l)(iii) of this section) when
calculating compliance under the pro-
visions of paragraph (c)(l) of this sec-
tion.
(iv) In any month that the system's
finished water SUVA, measured accord-
ing to §141.131(d)(4), is <2.0 L/mg-m, the
system may assign a monthly value of
1.0 (in lieu of the value calculated in
paragraph (c)(l)(iii) of this section)
when calculating compliance under the
provisions of paragraph (c)(l) of this
section.
(v) In any month that a system prac-
ticing enhanced softening lowers alka-
linity below 60 mg/L (as OaOO3), the
system may assign a monthly value of
1.0 (in lieu of the value calculated in
paragraph (c)(l)(iii) of this section)
when calculating compliance under the
506
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Environmental Protection Agency
§141.152
provisions of paragraph (c)(l) of this
section,
(3) Subpart H systems using conven-
tional treatment may also comply with
the requirements of this section by
meeting the criteria in paragraph (a)(2)
or (3) of this section.
(d) Treatment technique requirements
for DBF precursors. The Administrator
identifies the following as treatment
techniques to control the level of dis-
infection byproduct precursors in
drinking water treatment and distribu-
tion systems: For Subpart H systems
using conventional treatment, en-
hanced coagulation or enhanced soft-
ening.
[63 FR 69466, Dec. 16, 1998, as amended at 66
FR 3779, Jan. 16, 2001]
Subparts M-N [Reserved]
Subpart O—Consumer
Confidence Reports
SOURCE: 63 FR 44526, Aug. 19, 1998, unless
otherwise noted.
§ 141.151 Purpose and applicability of
this subpart.
(a) This subpart establishes the min-
imum requirements for the content of
annual reports that community water
systems must deliver to their cus-
tomers. These reports must contain in-
formation on the quality of the water
delivered by the systems and charac-
terize the risks (if any) from exposure
to contaminants detected in the drink-
ing water in an accurate and under-
standable manner.
(b) Notwithstanding the provisions of
§141,3, this subpart applies only to
community water systems.
(c) For the purpose of this subpart,
customers are defined as billing units or
service connections to which water is
delivered by a community water sys-
tem.
(d) For the purpose of this subpart,
detected means: at or above the levels
prescribed by §141.23(a)(4) for inorganic
contaminants, at or above the levels
prescribed by §141.24(f)(7) for the con-
taminants listed in §141.61(a), at or
above the level prescribed by
§141.24(h)(18) for the contaminants list-
ed in § 141.61(c), and at or above the lev-
els prescribed by §141.25(c) for radio-
active contaminants.
(e) A State that has primary enforce-
ment responsibility may adopt by rule,
after notice and comment, alternative
requirements for the form and content
of the reports. The alternative require-
ments must provide the same type and
amount of information as required by
§§141.153 and 141.154, and must be de-
signed to achieve an equivalent level of
public information and education as
would be achieved under this subpart.
(f) For purpose of §§141.154 and 141.155
of this subpart, the term "primacy
agency" refers to the State or tribal
government entity that has jurisdic-
tion over, and primary enforcement re-
sponsibility for, public water systems,
even if that government does not have
interim or final primary enforcement
responsibility for this rule. Where the
State or tribe does not have primary
enforcement responsibility for public
water systems, the term "primacy
agency" refers to the appropriate EPA
regional office.
§ 141.152 Effective dates.
(a) The regulations in this subpart
shall take effect on September IB, 1998.
(b) Bach existing community water
system must deliver its first report by
October 19, 1999, its second report by
July 1, 2000, and subsequent reports by
July 1 annually thereafter. The first
report must contain data collected dur-
ing, or prior to, calendar year 1998 as
prescribed in §141.153(d)(3). Each report
thereafter must contain data collected
during, or prior to, the previous cal-
endar year.
(c) A new community water system
must deliver its first report by July 1
of the year after its first full calendar
year in operation and annually there-
after.
(d) A community water system that
sells water to another community
water system must deliver the applica-
ble information required in §141,153 to
the buyer system:
(1) No later than April 19, 1999, by
April 1, 2000, and by April 1 annually
thereafter or
(2) On a date mutually agreed upon
by the seller and the purchaser, and
specifically included in a contract be-
tween the parties.
507
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§141.153
40 CFR Ch. I (7-1-04 Edition)
§ 141.153 Content of the reports,
(a) Bach community water system
must provide to its customers an an-
nual report that contains the informa-
tion specified in this section and
§141.154.
(b) Information on the source of the
water delivered:
(1) Bach report must identify the
source(s) of the water delivered by the
community water system by providing
information on:
(i) The type of the water: e.g., surface
water, ground water; and
(ii) The commonly used name (if any)
and location of the body (or bodies) of
water.
(2) If a source water assessment has
been completed, the report must notify
consumers of the availability of this
information and the means to obtain
it. In addition, systems are encouraged
to highlight in the report significant
sources of contamination in the source
water area if they have readily avail-
able information. Where a system has
received a source water assessment
from the primacy agency, the report
must include a brief summary of the
system's susceptibility to potential
sources of contamination, using lan-
guage provided by the primacy agency
or written by the operator.
(c) Definitions. (1) Bach report must
include the following definitions:
(i) Maximum Contaminant Level Goal
or MCLG: The level of a contaminant in
drinking water below which there is no
known or expected risk to health.
MCLGs allow for a margin of safety.
(ii) Maximum Contaminant Level or
MCL: The highest level of a contami-
nant that is allowed in drinking water.
MCLs are set as close to the MCLGs as
feasible using the best available treat-
ment technology.
(2) A report for a community water
system operating under a variance or
an exemption issued under §1415 or 1416
of SDWA must include the following
definition: Variances and Exemptions:
State or EPA permission not to meet
an MCL or a treatment technique
under certain conditions,
(3) A report that contains data on
contaminants that EPA regulates
using any of the following terms must
include the applicable definitions:
(i) Treatment Technique: A required
process intended to reduce the level of
a contaminant in drinking water.
(ii) Action Level: The concentration of
a contaminant which, if exceeded, trig-
gers treatment or other requirements
which a water system must follow.
(iii) Maximum residual disinfectant
level goal or MRDLG: The level of a
drinking water disinfectant below
which there is no known or expected
risk to health, MEDLQs do not reflect
the benefits of the use of disinfectants
to control microbial contaminants.
(iv) Maximum residual disinfectant
level or MRDL: The highest level of a
disinfectant allowed in drinking water.
There is convincing evidence that addi-
tion of a disinfectant is necessary for
control of microbial contaminants.
(d) Information on detected contami-
nants.
(1) This sub-section specifies the re-
quirements for information to be in-
cluded in each report for contaminants
subject to mandatory monitoring (ex-
cept Cryptosporidium). It applies to:
(i) Contaminants subject to a MCL,
action level, maximum residual dis-
infectant level, or treatment technique
(regulated contaminants).
(ii) Contaminants for which, moni-
toring is required by §141.40 (unregu-
lated contaminants); and
(iii) Disinfection by-products or mi-
crobial contaminants for which moni-
toring is required by §§141.142 and
141.143, except as provided under para-
graph (e)(l) of this section, and which
are detected in the finished water.
(2) The data relating to these con-
taminants must be displayed in one
table or in several adjacent tables. Any
additional monitoring results which a
community water system chooses to
include in its report must be displayed
separately.
(3) The data must be derived from
data collected to comply with EPA and
State monitoring and analytical re-
quirements during calendar year Ii98
for the first report and subsequent cal-
endar years thereafter except that:
(i) Where a system is allowed to mon-
itor for regulated contaminants less
often than once a year, the table(s)
must include the date and results of
508
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Environmental Protection Agency
§141,153
the most recent sampling and the re-
port must include a brief statement in-
dicating that the data presented in the
report are from the most recent testing
done in accordance with the regula-
tions. No data older than 5 years need
be included.
(ii) Results of monitoring in compli-
ance with §§141.142 and 141.143 need
only be included for 5 years from the
date of last sample or until any of the
detected contaminants becomes regu-
lated and subject to routine moni-
toring requirements, whichever comes
first.
(4) For detected regulated contami-
nants (listed in appendix A to this sub-
part), the table(s) must contain:
(i) The MCL for that contaminant ex-
pressed as a number equal to or greater
than 1.0 (as provided in appendix A to
this subpart);
(ii) The MCLG for that contaminant
expressed in the same units as the
MCL;
(ill) If there is no MCL for a detected
contaminant, the table must indicate
that there is a treatment technique, or
specify the action level, applicable to
that contaminant, and the report must
include the definitions for treatment
technique and/or action level, as appro-
priate, specified in paragraph(c)(3) of
this section;
(iv) For contaminants subject to an
MCL, except turbidity and total coli-
forms, the highest contaminant level
used to determine compliance with an
NPDWB and the range of detected lev-
els, as follows:
(A) When compliance with the MCL
is determined annually or less fre-
quently: The highest detected level at
any sampling point and the range of
detected levels expressed in the same
units as the MCL.
(B) When compliance with the MCL is
determined by calculating a running
annual average of all samples taken at
a sampling point: the highest average
of any of the sampling points and the
range of all sampling points expressed
in the same units as the MCL.
(C) When compliance with the MCL is
determined on a system-wide basis by
calculating a running annual average
of all samples at all sampling points:
the average and range of detection ex-
pressed in the same units as the MCL.
NOTE TO PARAGRAPH (d)(4)(iv): When round-
ing of results to determine compliance with
the MCL is allowed by the regulations,
rounding should be done prior to multiplying
the results by the factor listed in appendix A
of tnis subpart.
(v) For turbidity.
(A) When it is reported pursuant to
§141.13: The highest average monthly
value.
(B) When it is reported pursuant to
the requirements of § 141.71: the highest
monthly value. The report should in-
clude an explanation of the reasons for
measuring turbidity,
(C) When it is reported pursuant to
§141.73 or §141.173 or §141.551: the high-
est single measurement and the lowest
monthly percentage of samples meet-
ing the turbidity limits specified in
§141.73 or §141.173, or §141.551 for the
filtration technology being used. The
report should include an explanation of
the reasons for measuring turbidity;
(vi) For lead and copper: the 90th per-
centile value of the most recent round
of sampling and the number of sam-
pling sites exceeding the action level;
(vii) For total coliform:
(A) The highest monthly number of
positive samples for systems collecting
fewer than 40 samples per month; or
(B) The highest monthly percentage
of positive samples for systems col-
lecting at least 40 samples per month;
(viii) For fecal coliform: The total
number of positive samples; and
(ix) The likely source(s) of detected
contaminants to the best of the opera-
tor's knowledge. Specific information
regarding contaminants may be avail-
able in sanitary surveys and source
water assessments, and should be used
when available to the operator. If the
operator lacks specific information on
the likely source, the report must in-
clude one or more of the typical
sources for that contaminant listed in
appendix A to this subpart that is most
applicable to the system.
(5) If a community water system dis-
tributes water to its customers from
multiple hydraulically independent
distribution systems that are fed by
different raw water sources, the table
should contain a separate column for
each service area and the report should
identify each separate distribution sys-
tem. Alternatively, systems could
509
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§141.153
40 CFR Ch.! (7-1-04 Edition)
produce separate reports tailored to in-
clude data for each service area.
(6) The table(s) must clearly identify
any data indicating violations of
MCLs, MRDLs, or treatment tech-
niques, and the report must contain a
clear and readily understandable expla-
nation of the violation including: the
length of the violation, the potential
adverse health effects, and actions
taken by the system to address the vio-
lation. To describe the potential health
effects, the system must use the rel-
evant language of appendix A to this
subpart.
(7) For detected unregulated con-
taminants for which monitoring is re-
quired (except Cryptosporidium), the
table(s) must contain the average and
range at which the contaminant was
detected. The report may include a
brief explanation of the reasons for
monitoring for unregulated contami-
nants.
(e) Information on Cryptosporidium,
radon, and other contaminants:
(1) If the system has performed any
monitoring for Cryptosporidium, in-
cluding monitoring performed to sat-
isfy the requirements of §141.143, which
indicates that Cryptosporidium may be
present in the source water or the fin-
ished water, the report must include:
(i) A summary of the results of the
monitoring; and
(ii) An explanation of the signifi-
cance of the results.
(2) If the system has performed any
monitoring for radon which indicates
that radon may be present in the fin-
ished water, the report must include:
(i) The results of the monitoring; and
(ii) An explanation of the signifi-
cance of the results.
(3) If the system has performed addi-
tional monitoring which indicates the
presence of other contaminants in the
finished water, EPA strongly encour-
ages systems to report any results
which may indicate a health concern.
To determine if results may indicate a
health concern, EPA recommends that
systems find out if EPA has proposed
an NPDWR or issued a health advisory
for that contaminant by calling the
Safe Drinking Water Hotline (800-426-
4791). EPA considers detects above a
proposed MCL or health advisory level
to indicate possible health concerns.
For such contaminants, EPA rec-
ommends that the report include:
(i) The results of the monitoring; and
(ii) An explanation of the signifi-
cance of the results noting the exist-
ence of a health advisory or a proposed
regulation.
(f) Compliance with NPDWE. In addi-
tion to the requirements of
§141.153(d)(6), the report must note any
violation that occurred during the year
covered by the report of a requirement
listed below, and include a clear and
readily understandable explanation of
the violation, any potential adverse
health effects, and the steps the system
has taken to correct the violation.
(1) Monitoring and reporting of com-
pliance data;
(2) Filtration and disinfection pre-
scribed by subpart H of this part. For
systems which have failed to install
adequate filtration or disinfection
equipment or processes, or have had a
failure of such equipment or processes
which constitutes a violation, the re-
port must include the following lan-
guage as part of the explanation of po-
tential adverse health effects: Inad-
equately treated water may contain
disease-causing organisms. These orga-
nisms include bacteria, viruses, and
parasites which can cause symptoms
such as nausea, cramps, diarrhea, and
associated headaches.
(3) Lead and copper control require-
ments prescribed by subpart I of this
part. For systems that fail to take one
or more actions prescribed by
§§141.80(d), 141.81, 141.82, 141.83 or 141.84,
the report must include the applicable
language of appendix A to this subpart
for lead, copper, or both.
(4) Treatment techniques for Acryl-
amide and Bpichlorohydrin prescribed
by subpart K of this part. For systems
that violate the requirements of sub-
part K of this part, the report must in-
clude the relevant language from ap-
pendix A to this subpart.
(5) Recordkeeping of compliance
data.
(6) Special monitoring requirements
prescribed by §§141.40 and 141,41; and
(7) Violation of the terms of a vari-
ance, an exemption, or an administra-
tive or judicial order.
(g) Variances and Exemptions. If a
system is operating under the terms of
510
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Environmental Protection Agency
§141.153
a variance or an exemption issued
under § 1415 or 1416 of SDWA, the report
must contain:
(1) An explanation of the reasons for
the variance or exemption;
(2) The date on which the variance or
exemption was issued;
(3) A brief status report on the steps
the system is taking to install treat-
ment, find alternative sources of water,
or otherwise comply with the terms
and schedules of the variance or ex-
emption; and
(4) A notice of any opportunity for
public input in the review, or renewal,
of the variance or exemption.
(h) Additional information:
(1) The report must contain a brief
explanation regarding contaminants
which may reasonably be expected to
be found in drinking water including
bottled water. This explanation may
include the language of paragraphs
(h)(l) (i) through (iii) or systems may
use their own comparable language.
The report also must include the lan-
guage of paragraph (h)(l)(iv) of this
section.
(i) The sources of drinking water
(both tap water and bottled water) in-
clude rivers, lakes, streams, ponds, res-
ervoirs, springs, and wells. As water
travels over the surface of the land or
through the ground, it dissolves natu-
rally-occurring minerals and, in some
cases, radioactive material, and can
pick up substances resulting from the
presence of animals or from human ac-
tivity.
(ii) Contaminants that may be
present in source water include:
(A) Microbial contaminants, such as vi-
ruses and bacteria, which may come
from sewage treatment plants, septic
systems, agricultural livestock oper-
ations, and wildlife.
(B) Inorganic contaminants, such as
salts and metals, which can be natu-
rally-occurring or result from urban
storrnwater runoff, industrial or do-
mestic wastewater discharges, oil and
gas production, mining, or farming.
(C) Pesticides and herbicides, which
may come from a variety of sources
such as agriculture, urban storrnwater
runoff, and residential uses,
(D) Organic chemical contaminants, in-
cluding synthetic and volatile organic
chemicals, which are by-products of in-
dustrial processes and petroleum pro-
duction, and can also come from gas
stations, urban storrnwater runoff, and
septic systems.
(E) Radioactive contaminants, which
can be naturally-occurring or be the re-
sult of oil and gas production and min-
ing activities.
(iii) In order to ensure that tap water
is safe to drink, EPA prescribes regula-
tions which limit the amount of cer-
tain contaminants in water provided
by public water systems. FDA regula-
tions establish limits for contaminants
in bottled water which must provide
the same protection for public health.
(iv) Drinking water, including bot-
tled water, may reasonably be expected
to contain at least small amounts of
some contaminants. The presence of
contaminants does not necessarily in-
dicate that water poses a health risk.
More information about contaminants
and potential health effects can be ob-
tained by calling the Environmental
Protection Agency's Safe Drinking
Water Hotline (800-426-4791).
(2) The report must include the tele-
phone number of the owner, operator,
or designee of the community water
system as a source of additional infor-
mation concerning the report.
(3) In communities with a large pro-
portion of non-English speaking resi-
dents, as determined by the Primacy
Agency, the report must contain infor-
mation in the appropriate language(s)
regarding the importance of the report
or contain a telephone number or ad-
dress where such residents may contact
the system to obtain a translated copy
of the report or assistance in the ap-
propriate language.
(4) The report must include informa-
tion (e.g., time and place of regularly
scheduled board meetings) about op-
portunities for public participation in
decisions that may affect the quality of
the water.
(5) The systems may include such ad-
ditional information as they deem nec-
essary for public education consistent
with, and not detracting from, the pur-
pose of the report.
[63 FB 44526, Aug. 19, 1998, as amended at 63
FB 69516, Dec. 16, 1998; 64 FB 34733, June 29,
1999; 65 PR 26022, May 4, 2000; 67 FB 1836, Jan.
14, 2002]
511
-------
§141.154
40 cm Ch. I (7-1-04 Edition)
§141,164 Required additional health
information.
(a) All reports must prominently dis-
play the following language: Some peo-
ple may be more vulnerable to con-
taminants in drinking water than the
general population. Immuno-com-
promised persons such as persons with
cancer undergoing chemotherapy, per-
sons who have undergone organ trans-
plants, people with HIV/AIDS or other
immune system disorders, some elder-
ly, and infants can be particularly at
risk from infections. These people
should seek advice about drinking
water from their health care providers.
EPA/CDC guidelines on appropriate
means to lessen the risk of infection by
Cryptosporidium and other microbial
contaminants are available from the
Safe Drinking Water Hotline (800-426-
4791).
(b) Ending in the report due by July
1, 2001, a system which detects arsenic
at levels above 0.025 mg/L, but below
the 0.05 mg/L, and beginning in the re-
port due by July 1, 2002, a system that
detects arsenic above 0.005 mg/L and up
to and including 0.010 mg/L:
(1) Must include in its report a short
informational statement about arsenic,
using language such as: While your
drinking water meets EPA's standard
for arsenic, it does contain low levels
of arsenic. EPA's standard balances the
current understanding of arsenic's pos-
sible health effects against the costs of
removing arsenic from drinking water.
EPA continues to research the health
effects of low levels of arsenic, which is
a mineral known to cause cancer in hu-
mans at high concentrations and is
linked to other health effects such as
skin damage and circulatory problems.
(2) May write its own educational
statement, but only in consultation
with the Primacy Agency.
(c) A system which detects nitrate at
levels above 5 mg/1, but below the MOL:
(1) Must include a short informa-
tional statement about the impacts of
nitrate on children using language
such as: Nitrate in drinking water at
levels above 10 ppm is a health risk for
infants of less than six months of age.
High nitrate levels in drinking water
can cause blue baby syndrome. Nitrate
levels may rise quickly for short peri-
ods of time because of rainfall or agri-
cultural activity. If you are caring for
an infant you should ask advice from
your health care provider.
(2) May write its own educational
statement, but only in consultation
with the Primacy Agency.
(d) Systems which detect lead above
the action level in more than 5%, and
up to and including 10%, of homes sam-
pled:
(1) Must include a short informa-
tional statement about the special im-
pact of lead on children using language
such as: Infants and young children are
typically more vulnerable to lead in
drinking water than the general popu-
lation. It is possible that lead levels at
your home may be higher than at other
homes in the community as a result of
materials used in your home's plumb-
Ing. If you are concerned about ele-
vated lead levels in your home's water,
you may wish to have your water test-
ed and flush your tap for 30 seconds to
2 minutes before using tap water. Addi-
tional Information is available from
the Safe Drinking Water Hotline (800-
426-4791).
(2) May write its own educational
statement, but only in consultation
with the Primacy Agency.
(e) Community water systems that
detect TTHM above 0.080 mg/1, but
below the MCL in §141.12, as an annual
average, monitored and 'calculated
under the provisions of §141.30, must
include health effects language for
TTHMs prescribed by appendix A.
(f) Beginning in the report due by
July 1, 2002, and ending January 22,
2006, a community water system that
detects arsenic above 0.010 mg/L and up
to and including 0.05 mg/L must in-
clude the arsenic health effects lan-
guage prescribed by Appendix A to
Subpart O of this part.
[63 PE 44526, Aug. 19, 1998, as amended at 63
FE 69475, Deo. 16, 1998; 64 PE 34733, June 29,
1999; 65 FE 26023, May 4, 2000; 66 PR 7064, Jan.
22, 2001; 68 FE 14506, Mar. 25, 2003]
§ 141.158 Report delivery and record-
keeping.
(a) Except as provided in paragraph
(g) of this section, each community
water system must mail or otherwise
directly deliver one copy of the report
to each customer.
512
-------
Environmental Protection Agency
§141.155
(b) The system must make a good
faith effort to reach consumers who do
not get water hills, using means rec-
ommended by the primacy agency.
EPA expects that an adequate good
faith effort will be tailored to the con-
sumers who are served by the system
but are not bill-paying customers, such
as renters or workers, A good faith ef-
fort to reach consumers would include
a mix of methods appropriate to the
particular system such as: Posting the
reports on the Internet; mailing to
postal patrons in metropolitan areas;
advertising the availability of the re-
port in the news media; publication in
a local newspaper; posting in public
places such as cafeterias or lunch
rooms of public buildings; delivery of
multiple copies for distribution by sin-
gle-biller customers such as apartment
buildings or large private employers;
delivery to community organizations.
(c) No later than the date the system
is required to distribute the report to
its customers, each community water
system must mail a copy of the report
to the primacy agency, followed within
3 months by a certification that the re-
port has been distributed to customers,
and that the information is correct and
consistent with the compliance moni-
toring data previously submitted to
the primacy agency.
(d) No later than the date the system
is required to distribute the report to
its customers, each community water
system must deliver the report to any
other agency or clearinghouse identi-
fied by the primacy agency.
(e) Bach community water system
must make its reports available to the
public upon request.
(f) Each community water system
serving 100,000 or more persons must
post its current year's report to a pub-
licly-accessible site on the Internet.
(g) The Governor of a State or his
designee, or the Tribal Leader where
the tribe has met the eligibility re-
quirements contained in §142.72 for the
purposes of waiving the mailing re-
quirement, can waive the requirement
of paragraph (a) of this section for
community water systems serving
fewer than 10,000 persons. In consulta-
tion with the tribal government, the
Regional Administrator may waive the
requirement of §141.155(a) in areas in
Indian country where no tribe has been
deemed eligible.
(1) Such systems must:
(i) Publish the reports in one or more
local newspapers serving the area in
which the system is located;
(ii) Inform the customers that the re-
ports will not be mailed, either in the
newspapers in which the reports are
published or by other means approved
by the State; and
(iii) Make the reports available to
the public upon request.
(2) Systems serving 500 or fewer per-
sons may forego the requirements of
paragraphs (g)(l)(i) and (ii) of this sec-
tion if they provide notice at least once
per year to their customers by mail,
door-to-door delivery or by posting in
an appropriate location that the report
is available upon request.
(h) Any system subject to this sub-
part must retain copies of its Con-
sumer Confidence Report for no less
than 3 years.
[63 PR 44526, Aug. 19, 1998, as amended at 65
PR 26023, May 4, 2000]
513
-------
APPENDIX A TO SUBPART O OF PART MI—REGULATED CONTAMINANTS
Ol
Contaminant (units)
Microbiological contaminants:
Total Coliform Bacteria ...
Fees! coliform and E. coli
Total orysnic cartoon
(ppm).
Traditional MCL in
mg/L
MCL: (systems
that collect £40
samples/month)
5% of monthly
samples are
positive; (sys-
tems that collect
<40 samples/
month) 1 posi-
tive monthly
sample.
0
TT
To convert for
CCR, multiply by
MCL in CCR units
MCL: (systems
that collect £40
samples/month)
5% of monthly
samples are
positive; ^sys-
tems that collect
<4G samples/
month) 1 posi-
tive monthly
sample.
0
TT
MCLG
0
0
N/A
Major sources in drinking water
Naturally present in the environ*
ment.
Human and animal fecal waste ....
Naturally present in the environ-
ment
Health effects language
.
Goliforrns are bacteria that are
naturally present in the environ-
ment and are used as an indi-
cator that other, potentially-
harmful, bacteria may be
present. Conforms were found
in more samples than allowed
and the was a warning of po-
tential problems.
Fecal coliforms and E, coir are
bacteria whose presence indi-
cates that the water may be
contaminated with human or
animal wastes. Microbes in
these wastes can cause short-
term effects, such as diarrhea,
cramps, nausea, headaches, or
other symptoms. They may
pose a special health risk for in-
fants, young children, some of
the elderly, and people with se-
verely-compromised immune
systems.
Total organic carbon (TOG) has
no health effects. However,
total organic carbon provides a
medium for the formation of dis-
infection by products. These by-
products include
trihalomethanes (THMs) and
haloacetic acids (HAAs). Drink-
ing water containing these by-
products in excess of the MCL
may lead to adverse health ef-
fects, liver or kidney problems,
or nervous system effects, and
may lead to an increased risk
of getting cancer.
3
H
•O
O
"U
TJ
o
O
3
-------
Turbidity (NTU) .
Radioactive contaminants:
Beta/photon emitters
(mrem/yr}.
Inorganic contaminants:
Antimony (ppb)
nants:
itters
pCi/L)
m (pCi/Lj
nts:
rr
4 mrem/yr
15 pCift
S pCi/L
30 ng/L
.006 , . .
1000 . .
TT
4
15
5
30
6
N/A
0
o
o
0
6
Decay of natural and man-made
deposits.
eries; fire retardants; ceramics;
electronics; solder.
Turbidity has no health effects,
However, turbidity can interfere
with disinfection and provide a
medium for mierobial growth.
Turbidity may indicate the pres-
ence of disease-causing orga-
nisms. These organisms in-
clude bacteria, viruses, and
parasites that can cause symp-
toms such as nausea, cramps,
diarrhea and associated head-
aches.
Certain minerals are radioactive
and may emit forms of radiation
known as photons and beta ra-
diation. Some people who drink
water containing beta particle
and photon radioactivity in ex-
cess of the MCL over many
years may have an increased
risk of getting cancer.
Certain minerals are radioactive
and may emit a form of radi-
ation known as alpha radiation.
Some people who drink water
containing alpha emitters in ex-
cess of the MCL over many
years may have an increased
risk of getting cancer.
Some people who drink water
containing radium-226 or -228
in excess of the MCL over
many years may have an in-
creased risk of getting cancer.
Some people who drink water
containing uranium in excess of
the MCL over many years may
have an increased risk of get-
ting cancer and kidney toxicrty.
Some people who drink water
containing antimony well in ex-
cess of the MCL over many
years could experience in-
creases in blood cholesterol
and decreases in blood sugar.
in
CT
?
>
-------
Contaminant (units)
Arsenic (ppb)
Asbestos (MFL)
Chloramines (ppm)
Traditional MCL in
mg/L
1 0.010
7 MFL
2
004
010
.005
MRDU4
To convert for
OCR, multiply by
1000
1000
1000
1000 .
MCL in OCR units
MO
?
2
4
10
5
MRDL=4 ...............
MCLG
10
7
2 .......................
4
0 .. . .
5
MRDL£3=4 ...........
Major sources in drinking water
Erosion of natural deposits; Run-
off from orchards; Runoff from
glass and electronics produc-
tion wastes.
mains; Erosion of natural de-
posits.
Discharge of drilling wastes- Dis-
charge from metal refineries;
Erosion of natural deposits.
and coal-burning factories; Dis-
charge from electrical, aero-
space, and defense industries.
infection.
Erosion of natural deposits;
Discharge from metal refineries;
Runoff from waste batteries
and paints.
Water additive used to control mi-
crobes.
Health effects language
containing arsenic In excess of
the MCL over many years
could experience skin damage
or problems with their cir-
culatory system, and may have
an increased risk of getting
cancer.
containing asbestos in excess
of the MCL over many years
may have an increased risk of
developing benign intestinal
polyps.
containing barium in excess of
the MCL over many years
cou!d experience an increase in
their blood pressure.
containing beryllium well in ex-
cess of the MCL over many
years could develop intestinal
lesions
containing bromate in excess of
the MCL over many years may
have an increased risk of get-
ting cancer.
containing cadmium in excess
of the MCL over many years
could experience kidney dam-
age.
taining chloramines well in ex-
cess of the MRDL could experi-
ence irritating effects to their
eyes and nose. Some people
who drink water containing
chloramines well in excess of
the MRDL could experience
stomach discomfort or anemia.
Or
•
o
Tl
JO
o
XI
I
-------
Chlorine (ppm)
Chlorine dioxide (ppb)
MROL=4
MROL=.8 1000
Chlorite (ppm) ................. t 1
MBDL=4 MRDLG=4 ....
MRDL=800 .
MRDLG=800
0.8.
Cn
Chromium (ppb)
Copper (ppm) AL=1.3
AL=1,3 ...
i 1.3.
Water additive used to control mi- j
crobes.
Water additive used to control
mieorbes.
By-product of drinking water dis-
infection.
Discharge from steel and pulp
mills; Erosion of natural depos-
its.
Corrosion of household plumbing
systems; Erosion of natural de-
posits.
Some people who use water con-
taining chlorine well in excess
of the MRDL could experience
irritating effects to their eyes
and nose. Some people who
drink water containing chlorine
well in excess of the MRDL
could experience stomach dis-
comfort.
Some infants and young children
who drink water chlorine diox-
ide in excess of the MRDL
could experience nervous sys-
tem effects. Similar effects may
occur in fetuses of pregnant
women who drink water con-
taining chlorine dioxide in ex-
cess of the MHDL Some peo-
ple may experience anemia.
Some infants and young children
who drink water containing
chlorite in excess of the MCI
could experience nervous sys-
tem effects. Similar effects may
occur in fetuses of pregnant
women who drink water con-
taining chlorite in excess of the
MCL. Some people may experi-
ence anemia.
Some people who use water con-
taining chromium well in excess
of the MCL over many years
could experience allergic der-
matitis.
Copper is an essential nutrient,
but some people who drink
water containing copper in ex-
cess of the action level over a
relatively short amount of time
could experience gastro-
intestinal distress. Some people
who drink water containing cop-
per in excess of the action level
over many years could suffer
liver or kidney damage. People
with Wilson's disease should
consult their personal doctor.
I
O
*
P
-------
cn
i-1
00
Contaminant (units)
Fluoride (pprti)
Nitrate (ppm)
Traditional MCL in
mg/L
2 ...
4
AL= 01 5
002
10
To convert for
OCR, multiply by
1000
1000
1000
MCL in OCR units
200
4
AL=15
2
10
MCLG
200 . ...
4
o
2
10
Major sources in drinking water
tones; Discharge from plastic
and fertilizer factories.
additive which promotes strong
teeth; Discharge from fertilizer
and aluminum factories.
systems; Erosion of natural de-
posits.
charge from refineries and fac-
tories; Runoff from landfills;
Runoff from cropland.
ing from septic tanks, sew age;
Erosion of natural deposits.
Health effects language
containing cyanide well in ex-
cess of the MCL over many
years could experience nerve
damage or problems with their
thyroid.
containing fluoride in excess of
the MCL over many years
could get bone disease, includ-
ing pain and tenderness of the
bones. Fluoride in drinking
water at half the MCL or more
may cause mottling of chil-
dren's teeth, usually in children
less than nine years old. Mot-
tling, also known as dental fluo-
rosis, may include brown stain-
ing and/or pitting of the teeth,
and occurs only in developing
teeth before they erupt from the
gums.
water containing lead in excess
of the action level could experi-
ence delays in their physical or
menial development Children
could show slight deficits in at-
tention span and learning abili-
ties. Adults who drink this water
over many years could develop
kidney problems or high blood
pressure.
containing inorganic mercury
well in excess of the MCL over
many years could experience
kidney damage.
months who drink water con-
taining nitrate In excess of the
MCL could become seriously ill
and, if untreated, may die.
Symptoms include shortness of
breath and blue baby syn-
drome.
2
£
c
CT
O
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o
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-------
Environmental Protection Agency
Pt. 141,Subpt. O, App. A
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CJi
to
o
Contaminant (units)
{nanograms/1).
Chlordane (ppb) ..,.,.,.,.,,..
Traditional MCL in
mg/L
002 ..... . .......
.003 ,.,,,..
0002 . .....
04
.002
2
To convert for
CCR, multiply by
1000 .
1000 .
1 000 000
1000
1000 .
1000
MCL in CCR units
2 ...,,..,..„.,.,. ...
3
200 . .
40
2 ... . .....,.,.
200
MCLG
0 ...„.,... ..............
3 , ...........
0 . .......
40
0 ............ . .. ......
200
Major sources in drinking water
row craps.
row crops.
storage tanks and distribution
lines.
rice and alfalfa.
rights of way.
Health effects language
containing aiachlor in excess of
the MCL over many years
could have problems with their
eyes, liver, kidneys, or spleen,
or experience anemia, and may
have an increased risk of get-
ting cancer.
containing atrazine well in ex-
cess of the MCL over many
years could experience prob-
lems with their cardiovascular
system or reproductive difficul-
ties.
containing benzo(a)pyrene in
excess of the MCL over many
years may experience repro-
ductive difficulties and may
have an increased risk of get-
ting cancer.
containing carbofuran in excess
of the MCL over many years
could experience problems with
their blood, or nervous or repro-
ductive systems.
containing chlordane in excess
of the MCL over many years
could experience problems with
their liver or nervous system,
and may have an increased risk
of getting cancer.
containing dalapon well in ex-
cess of the MCL over many
years could experience minor
kidney changes.
to
&
"2.
o
o
Tl
TO
O
S
-------
Cn
to
Di(2-ethyihexyl) adipate
(PPb)
Di(2-ethylhexyl) pMhalate
(PPb).
(PPt).
Diquat {ppb)
Dioxin [2,3,7,8-TCDDl
(ppq).
Endothall (ppb!
.4
,006
0002
007
,02
.00000003
1
.002
1000
1000
1 000000
1000
1000 . .
1 000 000 000
1000
1000
400
6
200
7
20 .
30
100
2
400
0
Q
7
20
0
100
2
. j Discharge from chemical factories
Discharge from rubber and chem-
ical factories.
Runoff/leaching from soil fumigant
used on soybeans, cotton,
pineapples, and orchards.
Runoff from herbicide used on
soybeans and vegetables.
Runoff from herbicide use ,...„-..
Emissions from waste incineration
and other combustion; Dis-
charge from chemical factories.
Runoff from herbiciele use .....,.,,,.,
Residue of banned insecticide ,„.,
Some people who drink water
containing di(2-ethylhexyl) adi-
pate well in excess of the MCL
over many years could experi-
ence toxic effects such as
weight loss, liver enlargement
or possible reproductive difficul-
ties.
Some people who drink water
containing di{2-ethylhexvl)
phthatate well in excess of the
MCL over many years may
have problems with their liver,
or experience reproductive dif-
ficulties, and may have an in-
creased risk of getting cancer.
Some people who drink water
containing DBCP in excess of
the MCL over many years
could experience reproductive
problems and may have an in-
creased risk of getting cancer.
Some people who drink water
containing dinoseb well in ex-
cess of the MCL over many
years could experience repro-
ductive difficulties.
Some people who drink water
containing diquat in excess of
the MCL over many years
could get cataracts,
j Some people who drink water
containing dioxin in excess of
the MCL over many years
could experience reproductive
difficulties and may have an in-
creased risk of getting cancer.
Some people who drink water
containing endoihall in excess
of the yCL over many years
could experience problems with
their stomach or intestines.
j Some people who drink water
containing endrin sn excess of
the MCL over many years
could experience liver prob-
lems.
1.
o
-------
Cn
to
CO
Contaminant (unite)
Traditional MCL in
mg/L
jj
00005
7
0004
0002
001
To convert for
OCR, multiply by
1 000,000 ...
1000
1 000 000
1 000 000
1000
MCL in CCR units
TT ,
50
700
400
200
MCLG
o -..,...,-,.,............„.
0 , , ............. ....
TOO , ...................
o
0
0 ....
Major sources in drinking water
Discharge from industrial chem-
ical factories; An impurity of
some water treatment chemi-
cals.
eries.
Runoff from herbicide use ,...,.,„.,.
and agricultural chemieai fac-
tories.
Heafth effects language
Some people who drink water
containing high levels of
epichlorohydrin over a long pe-
riod of time could experience
stomach problems, and may
have an increased risk of get-
ting cancer.
Some people who drink water
containing ethylene dibromide
in excess of the MGL over
many years could experience
problems with their liver, stom-
ach, reproductive system, or
kidneys, and may have an in-
creased risk of getting cancer.
Some people who drink water
containing glyphosate in excess
of the MCL over many years
couid experience problems with
their kidneys or reproductive
difficulties.
containing heptachlor in excess
of the MCL over many years
could experience liver damage
and may have an increased risk
of getting cancer.
containing heptachlor epoxide
in excess of the MCL over
many years could experience
liver damage, and may have an
increased risk of getting cancer.
containing hexachlorobenzene
in excess of the MCL over
many years couid experience
problems with their liver or kid-
neys, or adverse reproductive
effects, and may have an in-
creased risk of getting cancer.
3
£
tr
TJ
"O
TJ
o
"ti
JO
O
a
*
-------
Cn
to
CO
Hexachlorocyclopenta-
diene (ppb).
Methoxychlor (ppb)
Oxamyl [Vydafe] (ppb) ....
PCBs [Polychlorlnated
biphenylsj (ppt).
Pentachlorophenol (ppb)
Picloram (ppb)
Simazine (ppb)
.05
0002
.04
2
.0005
.001
.5
.004
1000
1 000 000
1000
1000
1,000,000
1000
1000
1000
50
200
40
200
500
1
500
4
50
200
40
200
0
0 .
500
4
used on cattle, lumber, gardens.
used on fruits, vegetables, al-
falfa, livestock.
Runoff/leaching from insecticide
used on apples, potatoes and
tomatoes.
Runoff from landfills; Discharge of
waste chemicals.
factories.
Some people who drink water
containing hexachlorocyciopen-
tadiene well in excess of the
MCL over many years could ex-
perience proWems with their
kidneys or stomach.
Some people who drink water
containing lindane in excess of
the MCL over many years
could experience problems with
their kidneys or liver.
Some people who drink water
containing methoxychlor in ex-
cess of the MCL over many
years could experience repro-
ductive difficulties.
Some people who drink water
containing oxamyl in excess of
the MCL over many years
could experience slight nervous
system effects.
Some people who drink water
containing PCBs in excess of
the MCL over many years
could experience changes in
their skin, problems with their
thymus gland, immune defi-
ciencies, or reproductive or
nervous system difficulties, and
may have an increased risk of
getting cancer.
Some people who drink water
containing pentachiorophenol in
excess of the MCL over many
years couid experience prob-
lems with their liver or kidneys,
and may have an increased risk
of getting cancer.
Some people who drink water
containing picioram in excess
of the MCL over many years
could experience problems with
their liver.
Some people who drink water
containing simazine in excess
of the MCL over many years
could experience problems with
their blood.
i.
o
0)
i
"O
I
£
o
I
-------
Cn
CO
Contaminant (units)
Volatile organic contaminants:
(ppt».
o-Dichiorobenz©ne (ppb)
Traditional MCL in
mg/L
003
005
005
1
075
005
To convert for
OCR, multiply by
1000
1000
1000
1000
1000
1000
1000
MCL in CCR units
3
5
5
100
600
75
5
MCLG
0
0
0
1QG ,,„.„.,....„.„„,.,
600 .......................
75
0 -, ,„,..,....,..., >.,„„
Major sources in drinking water
Runoff/leaching from insecticide
used on cotton and cattle.
ing from gas storage tanks and
landfnls
and other industrial activities-
Discharge from chemica! and ag-
ricultural chemical factories.
Discharge from industrial chem-
ical factories.
leal factories.
Discharge from industrial chem-
ical factories-
Health effects language
Some people who drink water
containing toxaphene in excess
of the MCL over many years
could have problems with their
kidneys, liver, or thyroid, and
may have an increased risk of
getting cancer.
Some people who drink water
containing benzene in excess
of the MCL over many years
could experience anemia or a
decrease in blood platelets, and
may have an increased risk oJ
getting cancer.
containing carbon tetrachloride
in excess of the MCL over
many years could experience
problems with their liver and
may have an increased risk of
getting cancer.
Some people who drink water
containing chlorobenzene in ex-
cess of the MCL over many
years could experience prob-
lems with their liver or kidneys,
Some people who drink water
containing o-dtchlorobenzene
well in excess of the MCL over
many years could experience
problems with their fiver, kid-
neys, or circulatory systems.
containing p-dichlorobenzene in
excess of the MCL over many
years could experience anemia,
damage to their liver, kidneys,
or spleen, or changes in their
blood.
Some people who drink water
containing 1 ,2-dichloroethane In
excess of the MCL over many
years may have an increased
risk of getting cancer.
>
o
"H
O
i
I
m
a
-------
,1 -Dichloroethyiene ,007
(ppb).
cis-1,2-Dienioroethylene
(ppb).
trans-1,2-
Dichioroethylene {ppb}.
Dichloromethane (ppb) .... I ,005
1000 „.,„.,.,.,.,..
1000 .
70
1000
Oi
to
Cn
1,2-Dichloropropane
(ppb).
Ethylbenzene (ppb)
Haloacetic Acids (HAA) ,060
(ppb). |
Siyrene (ppb) ...,.....,.,.,.,., .1 ..
j 1000
! 1000
1000 ,........,„...,....
1000 ,.„.,.......,.......
70.
700
700.
Discharge from industrial chem-
ical factories.
Discharge from industrial chem-
ical factories.
Discharge from industrial chem-
ical factories.
Discharge from pharmaceutical
and chemical factories.
Discharge from industrial chem-
ical factories.
Discharge from petroleum refin-
eries.
By-product of drinking water dis-
infection.
Discharge from rubber and piastic
factories; Leaching from land-
fills,
Some people who drink water
containing 1,1-dichloroethylene
in excess of the MCL over
many years could experience
problems with their liver.
Some people who drink water
containing cis-1,2-
dichloroethylene in excess of
the MCL over many years
could experience problems with
their liver.
Some people who drink water
containing trans-1,2-
dichloroethylene well in excess
of the MCL over many years
could experience problems with
their liver.
Some people who drink water
containing dichloromethane in
excess of the MCL over many
years could have liver problems
and may have an increased risk
of getting cancer.
Some people who drink water
containing 1,2-dichloropropane
in excess of the MCL over
many years may have an in-
creased nsk of getting cancer.
Some people who drink water
containing ethylbenzene weli in
excess of the MCL over many
years could experience prob-
lems with their liver or kidneys.
Some people who drink water
containing haloacetic acids in
excess of the MCL over many
years may have an increased
risk of getting cancer-
Some people who drink water
containing styrene weH in ex-
cess of the MCL over many
years could have problems with
their liver, kidneys, or cir-
culatory system.
3
5
t?
a
"5.
"a
TJ
-------
to
O5
Contaminant (units)
(ppb).
(ppt>).
(ppb).
TTHMs {Total
trihatomethanesj (ppb).
Traditional MCL in
mg/L
00$ ,.,
07
2
005 . .
005
0 10/080
To convert for
CCR, multiply by
1000 .............
1000 .. .. . ... ....
1000
1000
1000
1000
MCL in CCR units
5 ,, ,.„„,,.,.,„„..,....
70 . ............ ..
2QQ
5
5
100/80 .. ....
MCLG
0 .................... ,.
70 .. , , ,...,.,.. ... .
200
3
0
N/A ,. ... . . ...... .
Major sources in drinking water
Discharge from factories and dry
cleaners.
factories.
sites and other factories.
ical factories.
sites and other factories.
infection.
Health effects language
Some people who drink water
containing tetrachioroethylene
in excess of the MCL over
many years could have prob-
lems with their liver, and may
have an increased risk of get-
ting cancer.
Some people who drink water
containing 1 ,2,4-
trichtorobenzene well in excess
of the MCL over many years
could experience changes in
their adrenal glands.
containing 1,1,1-trichloroethane
in excess of the MCL over
many years could experience
problems with their liver, nerv-
ous system, or circulatory sys-
tem.
Some people who drink water
containing 1,1,2-trichioroethane
well in excess of the MCL over
many years could have prob-
lems with their liver, kidneys, or
immune systems.
containing trichloroethylene in
excess of the MCL over many
years could experience prob-
lems with their liver and may
have an increased risk of get-
ting cancer.
containing trihaiomethanes in
excess of the MCL over many
years may experience problems
with their liver, kidneys, or cen-
tral nervous systems, and may
have an increased risk of get-
ting cancer.
2
£
-------
Vinyl Chloride (ppb)
002 .
10
1000
2
10
o
10
forfes.
charge from plastics factories.
lories; Discharge from chemical
factories
containing toluene well in ex-
cess of the MCL over many
years could have problems with
their nervous system, kidneys,
or liver.
containing vinyl chloride in ex-
cess of the MCL over many
years may have an increased
risk of getting cancer.
containing xyienes in excess of
the MCL over many years
coukJ experience damage to
their nervous system.
1 These arsenic values are effective January 23, 2006. Until then, the MCL is 0.05 rng/L and there is no MCLG.
Key:
AL=Action Level
MCL=Maximum Contaminant Level
MCLG=Maxlmurn Contaminant Level Goal
MFL=mlllion fibers per liter
MRDL=Maximum Residual Disinfectant Level
MRDLG=Maximum Residual Disinfectant Level Goal
Cn mrem/year=miilirems per year (a measure of radiation absorbed by the body)
00 N/A=Not Applicable
—^ NTU=Nephelpmetrtc Turbidity Units (a measure of water clarity)
pCi/l=picocuri@s per liter (a measure of radioactivity)
ppm=parts p«r million, or milligrams per liter (mgfl)
ppb=0arts per billion, or micrograms per liter (jig/l)
ppt=parts per trillion, or nanograms per liter
ppq=parts per quadrillion, or picograms per liter
TT=Treatment technique
[65 PR 26024, May 4, 2000, as amended at 65 PR 76749, Deo. 7, 2000; 66 FR 7064, Jan. 22, 2001; 67 FR 70855, Nov. 27, 2002; 67 FR 73011, Deo.
9, 2002; 68 FR 14506, Mar. 25, 2003]
I
I
CO
I
O
7
>
-------
§141.170
40 CFR Ch. I (7-1-04 Edition)
Subpart P—Enhanced Filtration
and Disinfection—Systems
Serving 10,000 or More Peo-
ple
SOURCE: 63 FR 69516, Dec. 16, 1998, unless
otherwise noted.
§ 141.170 General requirements.
(a) The requirements of this subpart
P constitute national primary drinking
water regulations. These regulations
establish requirements for filtration
and disinfection that are in addition to
criteria under which filtration and dis-
infection are required under subpart H
of this part. The requirements of this
subpart are applicable to subpart H
systems serving at least 10,000 people,
beginning January 1, 2002 unless other-
wise specified in this subpart. The reg-
ulations in this subpart establish or ex-
tend treatment technique requirements
in lieu of maximum contaminant levels
for the following contaminants: Giardia
lamblia, viruses, heterotrophic plate
count bacteria, Legionella,
Cryptosporidium, and turbidity. Each
subpart H system serving at least 10,000
people must provide treatment of its
source water that complies with these
treatment technique requirements and
are in addition to those identified in
§141.70. The treatment technique re-
quirements consist of installing and
properly operating water treatment
processes which reliably achieve:
(1) At least 99 percent (2-log) removal
of Cryptosporidium between a point
where the raw water is not subject to
recontamination by surface water run-
off and a point downstream before or at
the first customer for filtered systems,
or Cryptosporidium control under the
watershed control plan for unfiltered
systems.
(2) Compliance with the profiling and
benchmark requirements under the
provisions of §141.172.
(b) A public water system subject to
the requirements of this subpart is con-
sidered to be in compliance with the re-
quirements of paragraph (a) of this sec-
tion if:
(1) It meets the requirements for
avoiding filtration in §§141.71 and
141.171 and the disinfection require-
ments in §§141.72 and 141.172; or
(2) It meets the applicable filtration
requirements in either §141.73 or
§141.173 and the disinfection require-
ments in §§141.72 and 141.172.
(c) Systems are not permitted to
begin construction of uncovered fin-
ished water storage facilities beginning
February 16, 1999.
(d) Subpart H systems that did not
conduct optional monitoring under
§141.172 because they served fewer than
10,000 persons when such monitoring
was required, but serve more than
10,000 persons prior to January 14, 2005
must comply with §§141.170, 141.171,
141.173, 141.174, and 141.175. These sys-
tems must also consult with the State
to establish a disinfection benchmark.
A system that decides to make a sig-
nificant change to its disinfection
practice, as described in §141.172(c)(l)(i)
through (iv) must consult with the
State prior to making such change.
[63 FR 69516, Dec. 16, 1998, as amended at 66
FR 3779, Jan. 16, 2001; 67 FR 1836, Jan. 14,
2002]
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, §141.170 was amended in paragraph
(d) by removing the date "January 14, 2005"
and adding in its place "January 1, 2005", ef-
fective July 29, 2004.
§141.171 Criteria for avoiding filtra-
tion.
In addition to the requirements of
§141.71, a public water system subject
to the requirements of this subpart
that does not provide filtration must
meet all of the conditions of para-
graphs (a) and (b) of this section.
(a) Site-specific conditions. In addition
to site-specific conditions in §141.71(b),
systems must maintain the watershed
control program under §141.71(b)(2) to
minimize the potential for contamina-
tion by Cryptosporidium oocysts in the
source water. The watershed control
program must, for Cryptosporidium:
(1) Identify watershed characteristics
and activities which may have an ad-
verse effect on source water quality;
and
(2) Monitor the occurrence of activi-
ties which may have an adverse effect
on source water quality.
(b) During the onsite inspection con-
ducted under the provisions of
§141.71(b)(3), the State must determine
528
-------
Environmental Protection Agency
§141.172
whether the watershed control pro-
gram established under §141.71(b)(2) is
adequate to limit potential contamina-
tion by Cryptosporidium oocysts. The
adequacy of the program must be based
on the comprehensiveness of the water-
shed review; the effectiveness of the
system's program to monitor and con-
trol detrimental activities occurring in
the watershed; and the extent to which
the water system has maximized land
ownership and/or controlled land use
within the watershed.
§141.172 Disinfection profiling and
benchmarking.
(a) Determination of systems required to
profile. A public water system subject
to the requirements of this subpart
must determine its TTHM annual aver-
age using the procedure in paragraph
(a)(l) of this section and its HAA5 an-
nual average using the procedure in
paragraph (a)(2) of this section. The an-
nual average is the arithmetic average
of the quarterly averages of four con-
secutive quarters of monitoring.
(1) The TTHM annual average must
be the annual average during the same
period as is used for the HAAS annual
average.
(i) Those systems that collected data
under the provisions of subpart M (In-
formation Collection Rule) must use
the results of the samples collected
during the last four quarters of re-
quired monitoring under § 141.142.
(ii) Those systems that use "grand-
fathered" HAA5 occurrence data that
meet the provisions of paragraph
(a)(2)(ii) of this section must use TTHM
data collected at the same time under
the provisions of §§141.12 and 141.30.
(ill) Those systems that use HAAS oc-
currence data that meet the provisions
of paragraph (a)(2)(iii)(A) of this sec-
tion must use TTHM data collected at
the same time under the provisions of
§§141.12 and 141.30.
(2) The HAAS annual average must be
the annual average during the same pe-
riod as is used for the TTHM annual
average.
(i) Those systems that collected data
under the provisions of subpart M (In-
formation Collection Rule) must use
the results of the samples collected
during the last four quarters of re-
quired monitoring under §141.142.
(ii) Those systems that have col-
lected four quarters of HAAS occur-
rence data that meets the routine mon-
itoring sample number and location re-
quirements for TTHM in §§141.12 and
141.30 and handling and analytical
method requirements of §141.142(b)(l)
may use those data to determine
whether the requirements of this sec-
tion apply.
(iii) Those systems that have not col-
lected four quarters of HAA5 occur-
rence data that meets the provisions of
either paragraph (a)(2)(l) or (ii) of this
section by March 16,1999 must either:
(A) Conduct monitoring for HAAS
that meets the routine monitoring
sample number and location require-
ments for TTHM in §§141.12 and 141.30
and handling and analytical method re-
quirements of §141.142(b)(l) to deter-
mine the HAAS annual average and
whether the requirements of paragraph
(b) of this section apply. This moni-
toring must be completed so that the
applicability determination can be
made no later than March 31, 2000, or
(B) Comply with all other provisions
of this section as if the HAAS moni-
toring had been conducted and the re-
sults required compliance with para-
graph (b) of this section.
(3) The system may request that the
State approve a more representative
annual data set than the data set de-
termined under paragraph (a)(l) or (2)
of this section for the purpose of deter-
mining applicability of the require-
ments of this section.
(4) The State may require that a sys-
tem use a more representative annual
data set than the data set determined
under paragraph (a)(l) or (2) of this sec-
tion for the purpose of determining ap-
plicability of the requirements of this
section.
(5) The system must submit data to
the State on the schedule in para-
graphs (a)(5)(i) through (v) of this sec-
tion.
(i) Those systems that collected
TTHM and HAAS data under the provi-
sions of subpart M (Information Collec-
tion Rule), as required by paragraphs
(a)(l)(i) and (a)(2)(i) of this section,
must submit the results of the samples
collected during the last 12 months of
required monitoring under §141.142 not
later than December 31,1999.
529
-------
S141.T72
40 CFR Ch.! (7-1-04 Edition)
(ii) Those systems that have col-
lected four consecutive quarters of
HAAS occurrence data that meets the
routine monitoring sample number and
location for TTHM in §§141.12 and 141.30
and handling and analytical method re-
quirements of §141.142(b)(l), as allowed
by paragraphs (a)(l)(ii) and (a)(2)(ii) of
this section, must submit those data to
the State not later than April 16, 1999.
Until the State has approved the data,
the system must conduct monitoring
for HAA5 using the monitoring require-
ments specified under paragraph
(a)(2)(iii) of this section.
(ill) Those systems that conduct
monitoring for HAAS using the moni-
toring requirements specified by para-
graphs (a)(l)(iii) and (a)(2)(iii)(A) of
this section, must submit TTHM and
HAAS data not later than March 31,
2000.
(iv) Those systems that elect to com-
ply with all other provisions of this
section as if the HAA5 monitoring had
been conducted and the results re-
quired compliance with this section, as
allowed under paragraphs (a)(2)(iii)(B)
of this section, must notify the State
in writing of their election not later
than December 31,1999.
(v) If the system elects to request
that the State approve a more rep-
resentative annual data set than the
data set determined under paragraph
(a)(2)(i) of this section, the system
must submit this request in writing
not later than December 31,1999.
(6) Any system having either a TTHM
annual average >0.084 mg/L or an HAA5
annual average >0.048 mg/L during the
period identified in paragraphs (a)(l)
and (2) of this section must comply
with paragraph (b) of this section.
(b) Disinfection profiling. (1) Any sys-
tem that meets the criteria in para-
graph (a)(6) of this section must de-
velop a disinfection profile of its dis-
infection practice for a period of up to
three years.
(2) The system must monitor daily
for a period of 12 consecutive calendar
months to determine the total logs of
inaetivation for each day of operation,
based on the OT99.9 values in Tables
1.1-1.6, 2.1, and 3.1 of §141.74(b). as ap-
propriate, through the entire treat-
ment plant. This system must begin
this monitoring not later than April 1,
2000. As a minimum, the system with a
single point of disinfectant application
prior to entrance to the distribution
system must conduct the monitoring
in paragraphs (b)(2)(i) through (iv) of
this section. A system with more than
one point of disinfectant application
must conduct the monitoring in para-
graphs (b)(2)(i) through (iv) of this sec-
tion for each disinfection segment. The
system must monitor the parameters
necessary to determine the total inac-
tivation ratio, using analytical meth-
ods in §141.74(a), as follows:
(i) The temperature of the disinfected
water must be measured once per day
at each residual disinfectant con-
centration sampling point during peak
hourly flow.
(ii) If the system uses chlorine, the
pH of the disinfected water must be
measured once per day at each chlorine
residual disinfectant concentration
sampling point during peak hourly
flow.
(iii) The disinfectant contact time(s)
("T") must be determined for each day
during peak hourly flow.
(iv) The residual disinfectant con-
centration^) ("C") of the water before
or at the first customer and prior to
each additional point of disinfection
must be measured each day during
peak hourly flow.
(3) In lien of the monitoring con-
ducted under the provisions of para-
graph (b)(2) of this section to develop
the disinfection profile, the system
may elect to meet the requirements of
paragraph (b)(3)(i) of this section. In
addition to the monitoring conducted
under the provisions of paragraph (b)(2)
of this section to develop the disinfec-
tion profile, the system may elect to
meet the requirements of paragraph
(b)(3)(ii) of this section.
(i) A PWS that has three years of ex-
isting operational data may submit
those data, a profile generated using
those data, and a request that the
State approve use of those data in lieu
of monitoring under the provisions of
paragraph (b)(2) of this section not
later than March 31, 2000. The State
must determine whether these oper-
ational data are substantially equiva-
lent to data collected under the provi-
sions of paragraph (b)(2) of this section.
These data must also be representative
530
-------
Environmental Protection Agency
§141.172
of Giardia lamblia inactivation through
the entire treatment plant and not just
of certain treatment segments. Until
the State approves this request, the
system is required to conduct moni-
toring under the provisions of para-
graph (b)(2) of this section.
(ii) In addition to the disinfection
profile generated under paragraph
(b)(2) of this section, a PWS that has
existing operational data may use
those data to develop a disinfection
profile for additional years. Such sys-
tems may use these additional yearly
disinfection profiles to develop a
benchmark under the provisions of
paragraph (c) of this section. The State
must determine whether these oper-
ational data are substantially equiva-
lent to data collected under the provi-
sions of paragraph (b)(2) of this section.
These data must also be representative
of inactivation through the entire
treatment plant and not just of certain
treatment segments.
(4) The system must calculate the
total inactivation ratio as follows:
(i) If the system uses only one point
of disinfectant application, the system
may determine the total inactivation
ratio for the disinfection segment
based on either of the methods in para-
graph (b)(4)(i)(A) or (b)(4)(i)(B) of this
section.
(A) Determine one inactivation ratio
(CTcale/OT»,9) before or at the first
customer during peak hourly flow.
(B) Determine successive CTcalc/
CT99.9 values, representing sequential
inactivation ratios, between the point
of disinfectant application and a point
before or at the first customer during
peak hourly flow. Under this alter-
native, the system must calculate the
total inactivation ratio by determining
(CTcalc/CT99.9) for each sequence and
then adding the (CTealc/CT<>9.9) values
together to determine (E (CTcalc/
CT99.9)).
(ii) If the system uses more than one
point of disinfectant application before
the first customer, the system must de-
termine the CT value of each disinfec-
tion segment immediately prior to the
next point of disinfectant application,
or for the final segment, before or at
the first customer, during peak hourly
flow. The (CTealc/CT99.9) value of each
segment and (Z(CTcale/CT99,9)) must be
calculated using the method in para-
graph (b)(4)(i) of this section.
(iii) The system must determine the
total logs of inactivation by multi-
plying the value calculated in para-
graph (b)(4)(i) or (ii) of this section by
3.0.
(5) A system that uses either
chloramines or ozone for primary dis-
infection must also calculate the logs
of inactivation for viruses using a
method approved by the State.
(6) The system must retain disinfec-
tion profile data in graphic form, as a
spreadsheet, or in some other format
acceptable to the State for review as
part of sanitary surveys conducted by
the State.
(c) Disinfection benchmarking. (1) Any
system required to develop a disinfec-
tion profile under the provisions of
paragraphs (a) and (b) of this section
and that decides to make a significant
change to its disinfection practice
must consult with the State prior to
making such change. Significant
changes to disinfection practice are:
(i) Changes to the point of disinfec-
tion;
(ii) Changes to the disinfectant(s)
used in the treatment plant;
(iii) Changes to the disinfection proc-
ess; and
(iv) Any other modification identi-
fied by the State.
(2) Any system that is modifying its
disinfection practice must calculate its
disinfection benchmark using the pro-
cedure specified in paragraphs (e)(2)(i)
through (ii) of this section.
(i) For each year of profiling data
collected and calculated under para-
graph (b) of this section, the system
must determine the lowest average
monthly Giardia lamblia inactivation in
each year of profiling data. The system
must determine the average Giardia
lamblia inactivation for each calendar
month for each year of profiling data
by dividing the sum of daily Giardia
lamblia of inactivation by the number
of values calculated for that month.
(ii) The disinfection benchmark is
the lowest monthly average value (for
systems with one year of profiling
data) or average of lowest monthly av-
erage values (for systems with more
than one year of profiling data) of the
531
-------
§141.173
40 CFR Ch. 1 (7-1-04 Edition)
monthly logs of Giardia lamblia inac-
tivation in each year of profiling data.
(3) A system that uses either
chloramines or ozone for primary dis-
infection must also calculate the dis-
infection benchmark for viruses using
a method approved by the State.
(4) The system must submit informa-
tion in paragraphs (c)(4)(i) through (ill)
of this section to the State as part of
its consultation process.
(i) A description of the proposed
change;
(ii) The disinfection profile for
Giardia lamblia (and, if necessary, vi-
ruses) under paragraph (b) of this sec-
tion and benchmark as required by
paragraph (c)(2) of this section; and
(iii) An analysis of how the proposed
change will affect the current levels of
disinfection.
[63 FR 69516, Deo, 16, 1998, as amended at 66
FR 3779, Jan. 16, 2001]
§ 141.173 Filtration.
A public water system subject to the
requirements of this subpart that does
not meet all of the criteria in this sub-
part and subpart H of this part for
avoiding filtration must provide treat-
ment consisting of both disinfection, as
specified in §141.72(b), and filtration
treatment which complies with the re-
quirements of paragraph (a) or (b) of
this section or §141.73 (b) or (c) by De-
cember 31, 2001.
(a) Conventional filtration treatment or
direct filtration. (1) For systems using
conventional filtration .or direct filtra-
tion, the turbidity level of representa-
tive samples of a system's filtered
water must be less than or equal to 0.3
NTU in at least 95 percent of the meas-
urements taken each month, measured
as specified in §141.74(a) and (c).
(2) The turbidity level of representa-
tive samples of a system's filtered
water must at no time exceed 1 NTU,
measured as specified in §141.74(a) and
(c).
(3) A system that uses lime softening
may acidify representative samples
prior to analysis using a protocol ap-
proved by the State.
(b) Filtration technologies other than
conventional filtration treatment, direct
filtration, slow sand filtration, or diato-
maceous earth filtration. A public water
system may use a filtration technology
not listed in paragraph (a) of this sec-
tion or in §141.73(b) or (c) if it dem-
onstrates to the State, using pilot
plant studies or other means, that the
alternative filtration technology, in
combination with disinfection treat-
ment that meets the requirements of
§141.72(b), consistently achieves 99,9
percent removal and/or inactivation of
Giardia lamblia cysts and 99.99 percent
removal and/or inactivation of viruses,
and 99 percent removal of
Cryptosporidium oocysts, and the State
approves the use of the filtration tech-
nology. For each approval, the State
will set turbidity performance require-
ments that the system must meet at
least 95 percent of the time and that
the system may not exceed at any time
at a level that consistently achieves
99,9 percent removal and/or inactiva-
tion of Giardia lamblia cysts, 99.99 per-
cent removal and/or inactivation of vi-
ruses, and 99 percent removal of
Cryptosporidium oocysts.
[63 PR 69516, Deo. 16, 1998, as amended at 65
PR 20313, Apr. 14, 2000; 66 PR 3779, Jan. 16,
2001]
§ 141.174 Filtration sampling require-
ments.
(a) Monitoring requirements for sys-
tems using filtration treatment. In ad-
dition to monitoring required by
§141.74, a public water system subject
to the requirements of this subpart
that provides conventional filtration
treatment or direct filtration must
conduct continuous monitoring of tur-
bidity for each individual filter using
an approved method in §141,74(a) and
must calibrate turbidirneters using the
procedure specified by the manufac-
turer. Systems must record the results
of individual filter monitoring every 15
minutes.
(b) If there is a failure in the contin-
uous turbidity monitoring equipment,
the system must conduct grab sam-
pling every four hours in lieu of contin-
uous monitoring, but for no more than
five working days following the failure
of the equipment.
§ 141.175 Reporting and recordkeeping
requirements.
In addition to the reporting and rec-
ordkeeping requirements in §141.75, a
532
-------
Environmental Protection Agency
§141.175
public water system subject to the re-
quirements of this subpart that pro-
vides conventional filtration treatment
or direct filtration must report month-
ly to the State the information speci-
fied in paragraphs (a) and (b) of this
section beginning January 1, 2002. In
addition to the reporting and record-
keeping requirements in §141.75, a pub-
lic water system subject to the require-
ments of this subpart that provides fil-
tration approved under §141.173(b) must
report monthly to the State the infor-
mation specified in paragraph (a) of
this section beginning January 1, 2002.
The reporting in paragraph (a) of this
section is in lieu of the reporting speci-
fied in §141.7500(1).
(a) Turbidity measurements as re-
quired by §141.173 must be reported
within 10 days after the end of each
month the system serves water to the
public. Information that must be re-
ported includes:
(1) The total number of filtered water
turbidity measurements taken during
the month.
(2) The number and percentage of fil-
tered water turbidity measurements
taken during the month which are less
than or equal to the turbidity limits
specified in §141.173(a) or (b).
(3) The date and value of any tur-
bidity measurements taken during the
month which exceed 1 NTU for systems
using conventional filtration treat-
ment or direct filtration, or which ex-
ceed the maximum level set by the
State under §141.173(b).
(b) Systems must maintain the re-
sults of individual filter monitoring
taken under §141.174 for at least three
years. Systems must report that they
have conducted individual filter tur-
bidity monitoring under §141.174 within
10 days after the end of each month the
system serves water to the public. Sys-
tems must report individual filter tur-
bidity measurement results taken
under §141.174 within 10 days after the
end of each month the system serves
water to the public only if measure-
ments demonstrate one or more of the
conditions in paragraphs (b)(l) through
(4) of this section. Systems that use
lime softening may apply to the State
for alternative exceedance levels for
the levels specified in paragraphs (b)(l)
through (4) of this section if they can
demonstrate that higher turbidity lev-
els in individual filters are due to lime
carryover only and not due to degraded
filter performance.
(1) For any individual filter that has
a measured turbidity level of greater
than 1.0 NTU in two consecutive meas-
urements taken 15 minutes apart, the
system must report the filter number,
the turbidity measurement, and the
date(s) on which the exceedance oc-
curred. In addition, the system must
either produce a filter profile for the
filter within 7 days of the exceedance
(if the system is not able to identify an
obvious reason for the abnormal filter
performance) and report that the pro-
file has been produced or report the ob-
vious reason for the exceedance.
(2) For any individual filter that has
a measured turbidity level of greater
than 0.5 NTU in two consecutive meas-
urements taken 15 minutes apart at
the end of the first four hours of con-
tinuous filter operation after the filter
has been backwashed or otherwise
taken offline, the system must report
the filter number, the turbidity, and
the date(s) on which the exceedance oc-
curred. In addition, the system must
either produce a filter profile for the
filter within 7 days of the exceedance
(if the system is not able to identify an
obvious reason for the abnormal filter
performance) and report that the pro-
file has been produced or report the ob-
vious reason for the exceedance.
(3) For any individual filter that has
a measured turbidity level of greater
than 1.0 NTU in two consecutive meas-
urements taken 15 minutes apart at
any time in each of three consecutive
months, the system must report the
filter number, the turbidity measure-
ment, and the date(s) on which the ex-
ceedance occurred. In addition, the sys-
tem must conduct a self-assessment of
the filter within 14 days of the exceed-
ance and report that the self-assess-
ment was conducted. The self assess-
ment must consist of at least the fol-
lowing components: assessment of fil-
ter performance; development of a fil-
ter profile; identification and
prioritization of factors limiting filter
performance; assessment of the appli-
cability of corrections; and preparation
of a filter self-assessment report.
533
-------
§141.201
40 CFR Ch. I (7-1-04 Edition)
(4) For any individual filter that has
a measured turbidity level of greater
than 2.0 NTU in two consecutive meas-
urements taken 15 minutes apart at
any time in each of two consecutive
months, the system must report the
filter number, the turbidity measure-
ment, and the date(s) on which the ex-
ceedance occurred. In addition, the sys-
tem must arrange for the conduct of a
comprehensive performance evaluation
by the State or a third party approved
by the State no later than 30 days fol-
lowing1 the exceedance and have the
evaluation completed and submitted to
the State no later than 90 days fol-
lowing the exceedance.
(c) Additional reporting requirements.
(1) If at any time the turbidity exceeds
1 NTU in representative samples of fil-
tered water in a system using conven-
tional filtration treatment or direct
filtration, the system must inform the
State as soon as possible, but no later
than the end of the next business day.
(2) If at any time the turbidity in
representative samples of filtered
water exceeds the maximum level set
by the State under § 141.173(b) for filtra-
tion technologies other than conven-
tional filtration treatment, direct fil-
tration, slow sand filtration, or diato-
maceous earth filtration, the system
must inform the State as soon as pos-
sible, but no later than the end of the
next business day.
[63 PR 69516, Dec. 16, 1998, as amended at 66
FR 3779, Jan. 16, 20011
Subpart Q—Public Notification of
Drinking Water Violations
SOURCE: 65 FR 26035, May 4, 2000, unless
otherwise noted.
§ 141.201 General public notification
requirements.
Public water systems in States with
primacy for the public water system
supervision (PWSS) program must
comply with the requirements in this
subpart no later than May 6, 2002 or on
the date the State-adopted rule be-
comes effective, whichever comes first.
Public water systems in jurisdictions
where EPA directly implements the
PWSS program must comply with the
requirements in this subpart on Octo-
ber 31, 2000. Prior to these dates, public
water systems must continue to com-
ply with the public notice require-
ments in §141.32 of this part. The term
"primacy agency" is used in this sub-
part to refer to either EPA or the State
or the Tribe in cases where EPA, the
State, or the Tribe exercises primary
enforcement responsibility for this sub-
part.
(a) Who must give public notice? Each
owner or operator of a public water
system (community water systems,
non-transient non-community water
systems, and transient non-community
water systems) must give notice for all
violations of national primary drink-
ing water regulations (NPDWB) and for
other situations, as listed in Table 1.
The term "NPDWB violations" is used
in this subpart to include violations of
the maximum contaminant level
(MOD, maximum residual disinfection
level (MRDL), treatment technique
(TT), monitoring requirements, and
testing procedures in this part 141. Ap-
pendix A to this subpart identifies the
tier assignment for each specific viola-
tion or situation requiring a public no-
tice.
TABLE 1 TO §141.201—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A PUBLIC
NOTICE
(1) NPDWR violations:
(i) Failure to comply with an applicable
maximum contaminant level (MCL) or
maximum residua] disinfectant level
(MRDL).
(ii) Failure to comply with a prescribed
treatment technique (TT).
(lii) Failure to perform water quality mon-
itoring, as required by the drinking
water regulations.
(iv) Failure to comply with testing proce-
dures as prescribed by a drinking
water regulation.
(2) Variance and exemptions under sections
1415 and 1416 of SDWA:
(i) Operation under a variance or an ex-
emption.
(ii) Failure to comply with the require-
ments of any schedule that has been
set under a variance or exemption.
(3) Special public notices:
534
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Environmental Protection Agency
§141.202
TABLE 1 TO §141,201—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A PUBLIC
NOTICE—Continued
(i) Occurrence of a waterborne disease
outbreak or other waterborne emer-
gency.
(iij Exceedance of the nitrate MCL by
non-community water systems
(NCWS), where granted permission by
the primacy agency under 141.11(d) of
this part.
(iii) Exceedance of the secondary max-
imum contaminant level (SMCL) for
fluoride,
(iv) Availability of unregulated contami-
nant monitoring data.
(v) Other violations and situations deter-
mined by the primacy agency to re-
quire a public notice under this sub-
part, not already listed in Appendix A.
(b) What type of public notice is re-
quired for each violation or situation?
Public notice requirements are divided
into three tiers, to take into account
the seriousness of the violation or situ-
ation and of any potential adverse
health effects that may be involved.
The public notice requirements for
each violation or situation listed in
Table 1 of this section are determined
by the tier to which it is assigned.
Table 2 of this section provides the def-
inition of each tier. Appendix A of this
part identifies the tier assignment for
each specific violation or situation.
TABLE 2 TO § 141.201—DEFINITION OF PUBLIC
NOTICE TIERS
(1) Tier 1 public notice—required for NPDWR
violations and situations with significant po-
tential to have serious adverse effects on
human health as a result of short-term ex-
posure.
(2) Tier 2 public notice—required for all other
NPDWR violations and situations with po-
tential to have serious adverse effects on
human health.
(3) Tier 3 public notice—required for all other
NPDWR violations and situations not in-
cluded in Tier 1 and Tier 2.
(c) Who must be notified?
(1) Bach public water system must
provide public notice to persons served
by the water system, in accordance
with this subpart. Public water sys-
tems that sell or otherwise provide
drinking water to other public water
systems (i.e., to consecutive systems)
are required to give public notice to
the owner or operator of the consecu-
tive system; the consecutive system is
responsible for providing public notice
to the persons it serves.
(2) If a public water system has a vio-
lation in a portion of the distribution
system that is physically or hydrau-
lically isolated from other parts of the
distribution system, the primacy agen-
cy may allow the system to limit dis-
tribution of the public notice to only
persons served by that portion of the
system which is out of compliance.
Permission by the primacy agency for
limiting distribution of the notice
must be granted in writing.
(3) A copy of the notice must also be
sent to the primacy agency, in accord-
ance with the requirements under
§141.31(d).
§141,202 Tier 1 Public Notice—Form,
manner, and frequency of notice,
(a) Which violations or situations re-
quire a Tier 1 public notice? Table 1 of
this section lists the violation cat-
egories and other situations requiring
a Tier 1 public notice. Appendix A to
this subpart identifies the tier assign-
ment for each specific violation or sit-
uation.
TABLE 1 TO §141.202—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A TIER 1
PUBLIC NOTICE
(1) Violation of the MCL for total coliforms
when fecal coliform or E. coli are present
in the water distribution system (as speci-
fied in § 141.63(b)), or when the water sys-
tem fails to test for fecal coliforms or E.
coli when any repeat sample tests positive
for coliform (as specified in § 141.21 (e));
(2) Violation of the MCL for nitrate, nitrite, or
total nitrate and nitrite, as defined in
§ 141.62, or when the water system fails to
take a confirmation sample within 24 hours
of the system's receipt of the first sample
showing an exceedance of the nitrate or
nitrite MCL, as specified in § 141.23(f)(2);
535
203-160 D-18
-------
§141.203
40 CFR Ch. I (7-1-04 Edition)
TABLE 1 TO §141.202—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A TIER 1
PUBLIC NOTICE—Continued
(3) Exceedance of the nitrate MCL by non-
community water systems, where permitted
to exceed the MCL by the primacy agency
under §141,11(d), as required under
§141.209;
(4) Violation of the MRDL for chlorine diox-
ide, as defined in §141.65(a), when one or
more samples taken in the distribution sys-
tem the day following an exceedance of
the MRDL at the entrance of the distribu-
tion system exceed the MRDL, or when
the water system does not take the re-
quired samples in the distribution system,
as specified in §141.133(c)(2)(i);
(5) Violation of the turbidity MCL under
§ 141.13{b), where the primacy agency de-
termines after consultation that a Tier 1 no-
tice is required or where consultation does
not take place within 24 hours after the
system learns of the violation;
(6) Violation of the Surface Water Treatment
Rule (SWTR), Interim Enhanced Surface
Water Treatment Rule (IESWTR) or Long
Term 1 Enhanced Surface Water Treat-
ment Rule (LT1ESWTR) treatment tech-
nique requirement resulting from a single
exceedance of the maximum allowable tur-
bidity limit (as identified in Appendix A),
where the primacy agency determines after
consultation that a Tier 1 notice is required
or where consultation does not take place
within 24 hours after the system learns of
the violation;
(7) Occurrence of a waterborne disease out-
break, as defined in §141.2, or other wa-
terborne emergency (such as a failure or
significant interruption in key water treat-
ment processes, a natural disaster that dis-
rupts the water supply or distribution sys-
tem, or a chemical spill or unexpected
loading of possible pathogens into the
source water that significantly increases
the potential for drinking water contamina-
tion);
(8) Other violations or situations with signifi-
cant potential to have serious adverse ef-
fects on human health as a result of short-
term exposure, as determined by the pri-
macy agency either in its regulations or on
a case-by-case basis.
(b) When is the Tier 1 public notice to
be provided? What additional steps are
required? Public water systems must:
(1) Provide a public notice as soon as
practical but no later than 24 hours
after the system learns of the viola-
tion;
(2) Initiate consultation with the pri-
macy agency as soon as practical, but
no later than 24 hours after the public
water system learns of the violation or
situation, to determine additional pub-
lic notice requirements; and
(3) Comply with any additional public
notification requirements (including
any repeat notices or direction on the
duration of the posted notices) that are
established as a result of the consulta-
tion with the primacy agency. Such re-
quirements may include the timing,
form, manner, frequency, and content
of repeat notices (if any) and other ac-
tions designed to reach all persons
served.
(c) What is the form and manner of the
public notice? Public water systems
must provide the notice within 24
hours in a form and manner reasonably
calculated to reach all persons served.
The form and manner used by the pub-
lic water system are to fit the specific
situation, but must be designed to
reach residential, transient, and non-
transient users of the water system. In
order to reach all persons served, water
systems are to use, at a minimum, one
or more of the following forms of deliv-
ery:
(1) Appropriate broadcast media
(such as radio and television);
(2) Posting of the notice in con-
spicuous locations throughout the area
served by the water system;
(3) Hand delivery of the notice to per-
sons served by the water system: or
(4) Another delivery method approved
in writing by the primacy agency.
[65 FR 26035, May 4, 2000, as amended at 67
PE 1836, Jan. 14,
§141.203 Tier 2 Public Notice—Form,
manner, and frequency of notice.
(a) Which violations or situations re-
quire a Tier 2 public notice? Table 1 of
this section lists the violation cat-
egories and other situations requiring'
a Tier 2 public notice. Appendix A to
this subpart identifies the tier assign-
ment for each specific violation or sit-
uation.
536
-------
Environmental Protection Agency
§141.203
TABLE 1 TO §141.203—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A TIER 2
PUBLIC NOTICE
(1) All violations of the MCL, MRDL, and
treatment technique requirements, except
where a Tier 1 notice is required under
§141.202(a) or where the primacy agency
determines that a Tier 1 notice is required;
(2) Violations of the monitoring and testing
procedure requirements, where the pri-
macy agency determines that a Tier 2 rath-
er than a Tier 3 public notice is required,
taking into account potential health impacts
and persistence of the violation; and
(3) Failure to comply with the terms and con-
ditions of any variance or exemption in
place.
(b) When is the Tier 2 public notice to
be provided?
(1) Public water systems must pro-
vide the public notice as soon as prac-
tical, but no later than 30 days after
the system learns of the violation. If
the public notice is posted, the notice
must remain in place for as long as the
violation or situation persists, but in
no case for less than seven days, even if
the violation or situation is resolved.
The primacy agency may, in appro-
priate circumstances, allow additional
time for the initial notice of up to
three months from the date the system
learns of the violation. It is not appro-
priate for the primacy agency to grant
an extension to the 30-day deadline for
any unresolved violation or to allow
across-the-board extensions by rule or
policy for other violations or situa-
tions requiring a Tier 2 public notice.
Extensions granted by the primacy
agency must be in writing.
(2) The public water system must re-
peat the notice every three months as
long as the violation or situation per-
sists, unless the primacy agency deter-
mines that appropriate circumstances
warrant a different repeat notice fre-
quency. In no circumstance may the
repeat notice be given less frequently
than once per year. It is not appro-
priate for the primacy agency to allow
less frequent repeat notice for an MCL
violation under the Total Coliform
Rule or a treatment technique viola-
tion under the Surface Water Treat-
ment Rule or Interim Enhanced Sur-
face Water Treatment Rule. It is also
not appropriate for the primacy agency
to allow through its rules or policies
across-the-board reductions in the re-
peat notice frequency for other ongoing
violations requiring a Tier 2 repeat no-
tice. Primacy agency determinations
allowing repeat notices to be given less
frequently than once every three
months must be in writing.
(3) For the turbidity violations speci-
fied in this paragraph, public water
systems must consult with the primacy
agency as soon as practical but no
later than 24 hours after the public
water system learns of the violation, to
determine whether a Tier 1 public no-
tice under §141.202(a) is required to pro-
tect public health. When consultation
does not take place within the 24-hour
period, the water system must dis-
tribute a Tier 1 notice of the violation
within the next 24 hours (i.e., no later
than 48 hours after the system learns of
the violation), following the require-
ments under §141.202(b) and (c). Con-
sultation with the primacy agency is
required for:
(i) Violation of the turbidity MCL
under §141.13(b); or
(ii) Violation of the SWTR, IESWTR
or LT1ESWTR treatment technique re-
quirement resulting from a single ex-
ceedance of the maximum allowable
turbidity limit.
(c) What is the form and manner of the
Tier 2 public notice? Public water sys-
tems must provide the initial public
notice and any repeat notices in a form
and manner that is reasonably cal-
culated to reach persons served in the
required time period. The form and
manner of the public notice may vary
based on the specific situation and type
of water system, but it must at a min-
imum meet the following require-
ments:
(1) Unless directed otherwise by the
primacy agency in writing, community
water systems must provide notice by:
(i) Mail or other direct delivery to
each customer receiving a bill and to
other service connections to which
water is delivered by the public water
system; and
(ii) Any other method reasonably cal-
culated to reach other persons regu-
larly served by the system, if they
would not normally be reached by the
notice required in paragraph (c)(l)(i) of
537
-------
§141.204
40 CFR Ch. I (7-1-04 Edition)
this section. Such persons may include
those who do not pay water bills or do
not have service connection addresses
(e.g., house renters, apartment dwell-
ers, university students, nursing home
patients, prison inmates, etc.). Other
methods may include: Publication in a
local newspaper; delivery of multiple
copies for distribution by customers
that provide their drinking water to
others (e.g., apartment building owners
or large private employers); posting in
public places served by the system or
on the Internet; or delivery to commu-
nity organizations.
(2) Unless directed otherwise by the
primacy agency in writing, non-com-
munity water systems must provide
notice by:
(i) Posting the notice in conspicuous
locations throughout the distribution
system frequented by persons served by
the system, or by mail or direct deliv-
ery to each customer and service con-
nection (where known); and
(ii) Any other method reasonably cal-
culated to reach other persons served
by the system if they would not nor-
mally be reached by the notice re-
quired in paragraph (c)(2)(i) of this sec-
tion. Such persons may include those
served who may not see a posted notice
because the posted notice is not in a lo-
cation they routinely pass by. Other
methods may include: Publication in a
local newspaper or newsletter distrib-
uted to customers; use of E-mail to no-
tify employees or students; or, delivery
of multiple copies in central locations
(e.g., community centers),
[65 PR 26035, May 4, 2000. as amended at 6?
PR 1836. Jan. 14,
§141.204 Tier 3 Public Notice—Form,
manner, and frequency of notice.
(a) Which violations or situations re-
quire a Tier 3 public notice? Table 1 of
this section lists the violation cat-
egories and other situations requiring
a Tier 3 public notice. Appendix A to
this subpart identifies the tier assign-
ment for each specific violation or sit-
uation.
TABLE 1 TO §141.204—VIOLATION CATEGORIES
AND OTHER SITUATIONS REQUIRING A TIER 3
PUBLIC NOTICE
(1) Monitoring violations under 40 CFR part
141, except where a Tier 1 notice is re-
quired under § 141.202(a) or where the pri-
macy agency determines that a Tier 2 no-
tice is required;
(2) Failure to comply with a testing procedure
established in 40 CFR part 141, except
where a Tier 1 notice is required under
§141.202(a)) or where the primacy agency
determines that a Tier 2 notice is required;
(3) Operation under a variance granted under
Section 1415 or an exemption granted
under Section 1416 of the Safe Drinking
Water Act;
(4) Availability of unregulated contaminant
monitoring results, as required under
§141.207; and
(5) Exceedance of the fluoride secondary
maximum contaminant level (SMCL), as
required under §141.208.
538
(b) When is the Tier 3 public notice to
he provided?
(I) Public water systems must pro-
vide the public notice not later than
one year after the public water system
learns of the violation or situation or
begins operating under a variance or
exemption. Following the initial no-
tice, the public water system must re-
peat the notice annually for as long- as
the violation, variance, exemption, or
other situation persists. If the public
notice is posted, the notice must re-
main in place for as long as the viola-
tion, variance, exemption, or other sit-
uation persists, but in no case less than
seven days (even if the violation or sit-
uation is resolved).
(2) Instead of individual Tier 3 public
notices, a public water system may use
an annual report detailing all viola-
tions and situations that occurred dur-
ing the previous twelve months, as
long as the timing requirements of
paragraph (b)(l) of this section are met.
(c) What is the form and manner of the
Tier 3 public notice? Public water sys-
tems must provide the initial notice
and any repeat notices in a form and
manner that is reasonably calculated
to reach persons served in the required
time period. The form and manner of
the public notice may vary based on
the specific situation and type of water
-------
Environmental Protection Agency
§141.205
system, but it must at a minimum
meet the following requirements:
(1) Unless directed otherwise by the
primacy agency in writing, community
water systems must provide notice by:
(i) Mail or other direct delivery to
each customer receiving a bill and to
other service connections to which
water is delivered by the public water
system; and
(11) Any other method reasonably cal-
culated to reach other persons regu-
larly served by the system, if they
would not normally be reached by the
notice required in paragraph (c)(l)(l) of
this section. Such persons may include
those who do not pay water bills or do
not have service connection addresses
(e.g., house renters, apartment dwell-
ers, university students, nursing home
patients, prison inmates, etc.). Other
methods may include: Publication in a
local newspaper; delivery of multiple
copies for distribution by customers
that provide their drinking water to
others (e.g., apartment building owners
or large private employers); posting in
public places or on the Internet; or de-
livery to community organizations.
(2) Unless directed otherwise by the
primacy agency in writing, non-com-
munity water systems must provide
notice by:
(i) Posting the notice in conspicuous
locations throughout the distribution
system frequented by persons served by
the system, or by mail or direct deliv-
ery to each customer and service con-
nection (where known); and
(ii) Any other method reasonably cal-
culated to reach other persons served
by the system, if they would not nor-
mally "be reached by the notice re-
quired in paragraph (c)(2)(i) of this sec-
tion. Such persons may include those
who may not see a posted notice be-
cause the notice is not in a location
they routinely pass by. Other methods
may include: Publication in a local
newspaper or newsletter distributed to
customers; use of E-mail to notify em-
ployees or students; or, delivery of
multiple copies in central locations
(e.g., community centers).
(d) In what situations may the Con-
sumer Confidence Report be used to meet
the Tier 3 public notice requirements? For
community water systems, the Con-
sumer Confidence Report (OCR) re-
quired under Subpart O of this part
may be used as a vehicle for the initial
Tier 3 public notice and all required re-
peat notices, as long as:
(1) The OCR is provided to persons
served no later than 12 months after
the system learns of the violation or
situation as required under §141.204(b);
(2) The Tier 3 notice contained in the
OCR follows the content requirements
under §141.205; and
(3) The CCR is distributed following
the delivery requirements under
§141.204(0).
[65 PR 26035, May 4, 2000; 65 PR June 21,
2000]
§ 141.205 Content of the public notice.
(a) What elements must be included in
the public notice for violations of National
Primary Drinking Water Regulations
(NPDWR) or other situations requiring a
public notice? When a public water sys-
tem violates a NPDWR or has a situa-
tion requiring public notification, each
public notice must include the fol-
lowing elements:
(1) A description of the violation or
situation, including the contaminant(s)
of concern, and (as applicable) the con-
taminant level(s);
(2) When the violation or situation
occurred;
(3) Any potential adverse health ef-
fects from the violation or situation,
including the standard language under
paragraph (d)(l) or (d)(2) of this sec-
tion, whichever is applicable;
(4) The population at risk, including
subpopulations particularly vulnerable
if exposed to the contaminant in their
drinking water;
(5) Whether alternative water aup-
plies should be used;
(6) What actions consumers should
take, including when they should seek
medical help, if known;
(7) What the system is doing to cor-
rect the violation or situation;
(8) When the water system expects to
return to compliance or resolve the sit-
uation;
(9) The name, business address, and
phone number of the water system
owner, operator, or designee of the pub-
lic water system as a source of addi-
tional information concerning the no-
tice; and
539
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§141.206
40 CFR Ch. I (7-1-04 Edition)
(10) A statement to encourage the no-
tice recipient to distribute the public
notice to other persons served, using
the standard language under paragraph
(d)(3) of this section, where applicable.
(b) What elements must he included in
the public notice for public water systems
operating under a variance or exemption?
(1) If a public water system lias been
granted a variance or an exemption,
the public notice must contain:
(i) An explanation of the reasons for
the variance or exemption;
(ii) The date on which the variance or
exemption was issued;
(iii) A brief status report on the steps
the system is taking to install treat-
ment, find alternative sources of water,
or otherwise comply with the terms
and schedules of the variance or ex-
emption; and
(iv) A notice of any opportunity for
public input in the review of the vari-
ance or exemption.
(2) If a public water system violates
the conditions of a variance or exemp-
tion, the public notice must contain
the ten elements listed in paragraph (a)
of this section.
(c) How is the public notice to be pre-
sented?
(1) Each public notice required by
this section:
(i) Must be displayed in a con-
spicuous way when printed or posted:
(ii) Must not contain overly technical
language or very small print;
(iii) Must not be formatted in a way
that defeats the purpose of the notice;
(iv) Must not contain language which
nullifies the purpose of the notice.
(2) Each public notice required by
this section must comply with multi-
lingual requirements, as follows:
(i) For public water systems serving
a large proportion of non-English
speaking consumers, as determined by
the primacy agency, the public notice
must contain information in the appro-
priate language(s) regarding the impor-
tance of the notice or contain a tele-
phone number or address where persons
served may contact the water system
to obtain a translated copy of the no-
tice or to request assistance in the ap-
propriate language,
(ii) In cases where the primacy agen-
cy has not determined what con-
stitutes a large proportion of non-
English speaking consumers, the public
water system must include in the pub-
lic notice the same information as in
paragraph (c)(2)(i) of this section,
where appropriate to reach a large pro-
portion of non-English speaking per-
sons served by the water system.
(d) What standard language must pub-
lic water systems include in their public
notice? Public water systems are re-
quired to include the following stand-
ard language in their public notice:
(1) Standard health effects language
for MCL or MRDL violations, treat-
ment technique violations, and viola-
tions of the condition of a variance or
exemption. Public water systems must
include in each public notice the
health effects language specified in Ap-
pendix B to this subpart corresponding
to each MCL, MRDL, and treatment
technique violation listed in Appendix
A to this subpart, and for each viola-
tion of a condition of a variance or ex-
emption.
(2) Standard language for monitoring
and testing procedure violations. Pub-
lic water systems must include the fol-
lowing language in their notice, includ-
ing the language necessary to fill in
the blanks, for all monitoring and test-
ing procedure violations listed in Ap-
pendix A to this subpart:
We are required to monitor your drinking
water for specific contaminants on a regular
basis. Results of regular monitoring are an
indicator of whether or not your drinking
water meets health standards. During [com-
pliance period], we "did not monitor or test"
or "did not complete all monitoring' or test-
ing" for [contamlnant(s)]. and therefore can-
not be sure of the quality of your drinking'
water during' that time.
(3) Standard language to encourage
the distribution of the public notice to
all persons served. Public water sys-
tems must include in their notice the
following language (where applicable):
Please share this information with all the
other people who drink this water, especially
those who may not have received this notice
directly (for example, people in apartments,
nursing' homes, schools, and businesses). You
can do this by posting this notice in a public
place or distributing copies by hand or mail.
§ 141.206 Notice to new billing units or
new customers.
(a) What is the requirement for commu-
nity water systems? Community water
540
-------
Environmental Protection Agency
§141.208
systems must give a copy of the most
recent public notice for any continuing
violation, the existence of a variance
or exemption, or other ongoing situa-
tions requiring a public notice to all
new billing units or new customers
prior to or at the time service begins.
(b) What is the requirement for non-
community water systems? Non-commu-
nity water systems must continuously
post the public notice in conspicuous
locations in order to inform new con-
sumers of any continuing violation,
variance or exemption, or other situa-
tion requiring a public notice for as
long as the violation, variance, exemp-
tion, or other situation persists.
§ 141.207 Special notice of the avail-
ability of unregulated contaminant
monitoring results,
(a) When is the special notice to be
given? The owner or operator of a com-
munity water system or non-transient,
non-community water system required
to monitor under §141.40 must notify
persons served by the system of the
availability of the results of such sam-
pling no later than 12 months after the
monitoring results are known.
(b) What is the form and manner of the
special notice? The form and manner of
the public notice must follow the re-
quirements for a Tier 3 public notice
prescribed in §§141.204(c), (d)(l), and
(d)(3). The notice must also identify a
person and provide the telephone num-
ber to contact for information on the
monitoring results.
§ 141.208 Special notice for exceedance
of the SMCL for fluoride.
(a) When is the special notice to be
given? Community water systems that
exceed the fluoride secondary max-
imum contaminant level (SMCL) of 2
mg/1 as specified in §143.3 (determined
by the last single sample taken in ac-
cordance with §141.23), but do not ex-
ceed the maximum contaminant level
(MCL) of 4 mg/1 for fluoride (as speci-
fied in §141.62), must provide the public
notice in paragraph (c) of this section
to persons served. Public notice must
be provided as soon as practical but no
later than 12 months from the day the
water system learns of the exceedance.
A copy of the notice must also be sent
to all new billing units and new cus-
tomers at the time service begins and
to the State public health officer. The
public water system must repeat the
notice at least annually for as long as
the SMCL is exceeded. If the public no-
tice is posted, the notice must remain
in place for as long as the SMCL is ex-
ceeded, but in no case less than seven
days (even if the exceedance is elimi-
nated). On a case-by-case basis, the pri-
macy agency may require an initial no-
tice sooner than 12 months and repeat
notices more frequently than annually.
(b) What> is the form and manner of the
special notice? The form and manner of
the public notice (including repeat no-
tices) must follow the requirements for
a Tier 3 public notice in §141.204(c) and
(d)(l) and (d)(3).
(c) What mandatory language must be
contained in the special notice? The no-
tice must contain the following lan-
guage, including the language nec-
essary to fill in the blanks:
This is an alert about your drinking water
and a cosmetic dental problem that might
affect children under nine years of age. At
low levels, fluoride can help prevent cavities,
but children drinking water containing more
than 2 milligrams per liter (mg/1) of fluoride
may develop cosmetic discoloration of their
permanent teeth (dental fluorosis). The
drinking water provided by your community
water system [ name] has a fluoride con-
centration of [insert value] mg/1.
Dental fluorosis, in its moderate or severe
forms, may result in a brown staining and/or
pitting of the permanent teeth. This problem
occurs only in developing teeth, before they
erupt from the gums. Children under nine
shoald be provided with alternative sources
of drinking water or water that has been
treated to remove the fluoride to avoid the
possibility of staining and pitting of their
permanent teeth. You may also want to con-
tact your dentist about proper use by young
children of fluoride-containing products.
Older children and adults may safely drink
the water.
Drinking water containing more than 4
mg/L of fluoride (the U.S. Environmental
Protection Agency's drinking water stand-
ard) can increase your risk of developing
bone disease. Your drinking water does not
contain more than 4 mg/1 of fluoride, but
we're required to notify you when we dis-
cover that the fluoride levels in your drink-
ing water exceed 2 mg/1 because of this cos-
metic dental problem.
For more information, please call [name of
water system contact] of [nar;<*> of commu-
nity water system] at [phone number]. Some
541
-------
§141.209
40 CFR Ch. I (7-1-04 Edition)
home water treatment units are also avail-
able to remove fluoride from drinking water.
To learn more about available home water
treatment units, you may call NSP Inter-
national at 1-877-a-NSF-HELP."
§141.209 Special notice for nitrate
exceedances above MCL by non-
community water systems (NCWS),
where granted permission by the
primacy agency under § 141.11(d)
(a) When is the special notice to be
given? The owner or operator of a non-
community water system granted per-
mission by the primacy agency under
§141,ll(d) to exceed the nitrate MCL
must provide notice to persons served
according to the requirements for a
Tier 1 notice under §141.202(a) and (b).
(b) What is the form and manner of the
special notice? Non-community water
systems granted permission by the pri-
macy agency to exceed the nitrate
MCL under §141.11(d) must provide con-
tinuous posting of the fact that nitrate
levels exceed 10 mg/1 and the potential
health effects of exposure, according to
the requirements for Tier 1 notice de-
livery under §141,202(c) and the content
requirements under §141,205.
§141,210 Notice by primacy agency on
behalf of the public water system.
(a) May the primacy agency give the
notice on behalf of the public water sys-
tem? The primacy agency may give the
notice required by this subpart on be-
half of the owner and operator of the
public water system if the primacy
agency complies with the requirements
of this sutapart,
(b) What is the responsibility of the
public water system when notice is given
by the primacy agency? The owner or op-
erator of the public water system re-
mains responsible for ensuring that the
requirements of this subpart are met.
APPENDIX A TO SUBPART Q OF PART 141—NPDWB VIOLATIONS AND OTHER
SITUATIONS REQUIRING PUBLIC NOTICE 1
Contaminant
t. Violations of National Primary Drinking
Water Regulations (NPDWB):3
MCL/MRDUTT violations"
Tier of public no-
tice required
A. Microbiological Contaminants 1
Citation
1 Total coiiform . ? > "idi finrat
2. Fecal coliform/E, coll
3. Turbidity MCL
4. Turbidity MCL (average of 2
days' samples >5 NTUj
1 ! 141.63(b)
2
141.13(a)
S2, 1 i 141.13(0)
5- Turbidity (for TT violations result- i
ing from a single exceedance of [
maximum allowable turbidity
level) ... I e? 1
6. Surface Water Treatment Rule
violations, other than violations
resulting from single exceedance
of max. allowable turbidity level
(TT)
7. Interim Enhanced Surface Water
Treatment Rule violations, other
than violations resulting from sin-
gle exceedance of max, turbidity
level (TTJ
8. Filter Backwash Recycling Rule
violations
141.71(a)(2),
141.71(c)(2)(i),
141.73(a)(2).
141.73(b)(2),
141.73(c)(2),
i 141.73(d),
j 141.173(a)(2),
141.173(b),
Monitoring & testing procedure viola-
tions
Tier of public no- ritaHnn
tice required utatlon
3
M, 3
3
3
141.21(a)-(e)
141.21(e)
141.22
141.22
3
141.551(b) i
2 141.70-141.73
72
2
3
!
141.170-141.173, 3
141.500-141,553
141.76
3
141,74(a)(1),
141,74(b)(2),
141.74(c)(1),
141.174,
141,560(aH<*
141.561.
141.74
141.172, 141.174,
141.530-141.544,
141.560-141.564.
141.76
542
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Environmental Protection Agency
Pt. 141,Subpt. Q, App. A
Contaminant
9, Long Term 1 Enhanced Surface
MCL/MRDL/TT violations2 ' Monitoring & testing procedure viola-
Tier ot public no-
tice required
Citation Tier of public no- m^™
tiee required wta"on
Water Treatment Rule violations 2 141.500-141.553 3
141.530-141.544,
141.560-141.564.
B. Inorganic Chemicals (iOCs) | :
1- Antimony 2 141.62(0) | 3 '. 141.23(a). (c)
2. Arsenic 2 e!41.62(b)' 3' 9l41.23fa). (c)
3. Asbestos (fibers >10 pm) 2 141.62(b)i 3
4. Barium 2 141.62(b)| 3
5. Beryllium 2 141.62(b) 3
6. Cadmium 2 141.62(b) 3
7. Chromiym (total) 2 141.62(b}! 3
8. Cyanide 2 I4i,62(b) | 3
9. Fluoride '• 2 141.82(b) : 3
10. Mercury (inorganic) 2; 141.62(b) . 3
11. Nitrate ' 1! 141.62(b) : 101.3
12 Nitrite j 1| 141.62(b) | 101.3
13. Total Nitrate and Nitrite | 1j 141.62(b) 3
141.23(a)-(b)
141 23(a), (c)
141.23(a) (C)
141 ,23(a), (c)
141.23(a), (C)
141 .23(3), (c)
141.23(3), (c)
141.23(3), (c)
141 .23(3}. id).
141.23(0(2)
141.23(a), (e).
14" 23(f)(2)
141,23(3)
14. Selenium | 2| 141.62(b) 3! 141.23(a), (c)
15. Thallium
C, Lead and Copper Rule (Action Level for
ieati
-------
Pt. 141,Subpt. Q, App. A
40 CFRCh. I (7-1-04 Edition)
Contaminant
13 Styrene
14 Tetrachloroethylene
16 1,2,4-Trichlorobenzene
17. 1,1,1-Trichloroethane
1811 2-Trichloroethane
19 Trichloroethylene
21 Xylenes (total)
F. Radioactive Contaminants
1. Beta/photon emitters
3. Combined radium (226 and 228)
G. Disinfection Byproducts (DBFs), Byprod-
uct Precursors, Disinfectant Residuals.
Where disinfection is used in the treat-
ment of drinking water, disinfectants com-
bine with organic and inorganic matter
present in water to form chemicals called
disinfection byproducts (DBPs). EPA sets
standards for controlling the levels of dis-
infectants and DBPs in drinking water, in-
cluding trihalomethanes (THMs) and
haloacetic acids (HAAs).1'
1. Total trihalomethanes (TTHMs) ..
2. Haloacetic Acids (HAAS)
4 Chlorite
5. Chlorine (MRDL)
6 Chloramine (MRDL)
7. Chlorine dioxide (MRDL), where
any 2 consecutive daily samples
at entrance to distribution system
8. Chlorine dioxide (MRDL), where
sample(s) in distribution system
the next day are also above
MRDL
9. Control of DBP precursors —
TOC (TT)
10. Bench marking and disinfection
1 1 . Development of monitoring plan
H. Other Treatment Techniques
1. Acrylamide (TT)
II. Unregulated Contaminant Monitoring: 15
A. Unregulated contaminants
B Nickel
III. Public Notification for Variances and Ex-
emptions:
A. Operation under a variance or exemption
B. Violation of conditions of a variance or
IV. Other Situations Requiring Public Notifi-
cation:
A. Fluoride secondary maximum contami-
nant level (SMCL) exceedance
B. Exceedance of nitrate MCL for non-com-
munity systems, as allowed by primacy
aaencv
MCL/MRDUTT violations2
Tier of public no-
tice required
2
2
2
2
2
2
2
2
2
2
2
2
92
2
2
2
2
2
2
2
14-,
2
N/A
N/A
2
2
N/A
N/A
3
2
3
1
Citation
141. 61 (a)
141. 61 (a)
141. 61 (a)
141.61(a)
141.61(3)
141.61(a)
141.61(a)
141.61(3)
141 .61 (a)
141.66(d)
141 .66(0)
141.66(b)
141.66(e)
12141.12,
141.64(a)
141.64(a)
141.64(a)
141 .64(3)
141.65(3)
141.65(3)
141.65(a),
141.133(c)(3)
141.65(a),
141.133(c)(3)
141.135(a)-(b)
N/A
N/A
141.111
141.111
N/A
N/A
161415, 1416.
1415, 1416,
17 142.307
143.3
141.11(d)
Monitoring & testing procedure viola-
tions
Tier of public no-
tice required
3
3
3
3
3
3
3
3
3
3
3
3
103
3
3
3
3
3
3
213, 3
1
3
3
3
N/A
N/A
3
3
N/A
N/A
N/A
N/A
Citation
141.24(f)
141.24(f)
141.24(f)
141.24(0
141.24(f)
141.24(f)
141.24(0
141.24(0
141.24(0
141.25(a)
141.26(b)
141.25(3)
141.26(3)
141.25(3)
141.26(3)
141 ,25(a)
141.26(3)
141.30,
141.132(a)-(b)
141.132(a)-(b)
141.132(a)-(b)
141.132(a)-(b)
141.132(3), (c)
141.132(3), (c)
141.132(3), (c),
141.133(c)(2)
141.132(3), (c),
141.133(c)(2)
141.132(3), (d)
141.172 141.530-
141.544.
141.132(f)
N/A
N/A
141.40
141.23(0), (k)
N/A
N/A
N/A
N/A
544
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Environmental Protection Agency
Pt. 141,Subpt. Q»App. A
Contaminant
C. Availability of unregulated contaminant
monitoring data
D. Waterborne disease outbreak
E. Other waterborne emergency18
F, Other situations as determined by pri-
MCL/MRDL/TT violations2
Tier of public no-
tice required
3
1
1
macy agency !S1,2,3
Citation
141,4
141.2
141.71 (c)(2)(i
Nit
N/i
I Monitoring & testing procedure viola-
"•-{ tions
Tier of public no- '
tice required j
N/A
N/A
N/A j
I
N/A '
Citation
N/A
N/A
N/A
N/A
APPENDIX A—BNDNOTES
1. Violations and other situations not list-
ed in this table (e.g., reporting violations
and failure to prepare Consumer Confidence
Reports), do not require notice, unless other-
wise determined by the primary a,gency. Pri-
macy agencies may, at their option, also re-
quire a more stringent public notice tier
(e.g., Tier 1 instead of Tier 2 or Tier 2 instead
of Tier 3) for specific violations and situa-
tions listed in this Appendix, as authorized
under §141.202(a) and §141.203(a).
2. MCL—Maximum contaminant level,
MRDL—Maximum residual disinfectant
level, TT—Treatment technique
3. The term Violations of National Pri-
mary Drinking Water Regulations (NPDWR)
is used here to include violations of MCL,
MRDL. treatment technique, monitoring-,
and testing procedure requirements.
4. Failure to test for fecal coliform or E.
coli is a Tier 1 violation if testing is not done
after any repeat sample tests positive for
coliform. All other total coliform moni-
toring and testing procedure violations are
Tier 3.
5. Systems that violate the turbidity MCL
of 5 NTU based on an average of measure-
ments over two consecutive days must con-
sult with the primacy agency within 24 hours
after learning of the violation. Based on this
consultation, the primacy agency may subse-
quently decide to elevate the violation to
Tier 1, If a system is unable to make contact
with the primacy agency in the 24-hour pe-
riod, the violation is automatically elevated
to Tier 1.
6. Systems with treatment technique viola-
tions involving a single exceedance of a max-
imum turbidity limit under the Surface
Water Treatment Rule (SWTB), the Interim
Enhanced Surface Water Treatment Rule
(IESWTR), or the Long Term 1 Enhanced
Surface Water Treatment Rule (LT1ESWTR)
are required to consult with the primacy
agency within 24 hours after learning of the
violation. Based on this consultation, the
primacy agency may subsequently decide to
elevate the violation to Tier 1. If a system is
unable to make contact with the primacy
agency in the 24-hou.r period, the violation is
automatically elevated to Tier 1.
7. Most of the requirements of the Interim
Enhanced Surface Water Treatment Rule (63
FR 69477) (.§§141.170-141.171, 141.173-141.174) be-
come effective January 1, 2002 for Subpart H
systems (surface water systems and ground
water systems under the direct influence of
surface water) serving at least 10,000 persons.
However, §141.172 has some requirements
that become effective as early as April 16,
1999. The Surface Water Treatment Rule re-
mains in effect for systems serving at least
10,000 persons even after 2002; the Interim
Enhanced Surface Water Treatment Rule
adds additional requirements and does not in
many cases supercede the SWTR.
8. The arsenic MCL citations are effective
January 23, 2006. Until then, the citations
are §141.11(b) and §141.23(n).
9. The uranium MCL Tier 2 violation cita-
tions are effective December 8, 2003 for all
community water systems,
10. The uranium Tier 3 violation citations
are effective December 8, 2000 for all commu-
nity water systems.
11. The arsenic Tier 3 violation MCL cita-
tions are effective January 23, 2006. Until
then, the citations are §141.23(a), (1).
12. Failure to take a confirmation sample
within 24 hours for nitrate or nitrite after an
initial sample exceeds the MCL is a Tier 1
violation. Other monitoring violations for
nitrate are Tier 3.
13. Subpart H community and non-tran-
sient non-community systems serving >10,000
must comply with new DBF MCLs, disinfect-
ant MRDLs, and related monitoring- require-
ments beginning January 1, 2002, All other
community and non-transient non-commu-
nity systems must meet the MCLs and
MRDLs beginning- January 1, 2004. Snbpart H
transient non-community systems serving
10,000 or more persons and using chlorine di-
oxide as a disinfectant or oxidant must com-
ply with the chlorine dioxide MRDL begin-
ning January 1, 2002. Subpart H transient
non-community systems serving fewer than
10,000 persons and using only ground water
not under the direct influence of surface
water and using chlorine dioxide as a dis-
infectant or oxidant must comply with the
chlorine dioxide MRDL beginning January 1,
2004.
545
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Pt. 141,Subpt. Q, App. B
40 CFR Ch. I (7-1-04 Edition)
14. §141.12 will no longer apply after Janu-
ary 1, 2004.
15. Failure to monitor for chlorine dioxide
at the entrance to the distribution system
the day after exceeding the MEDL at the en-
trance to the distribution system is a Tier 2
violation.
16, If any daily sample taken at the en-
trance to the distribution system exceeds
the MEDL for chlorine dioxide and one or
more samples taken in the distribution sys-
tem the next day exceed the MRDL, Tier 1
notification is required. Failure to take the
required samples in the distribution system
after the MBDL is exceeded at the entry
point also triggers Tier 1 notification.
17. Some water systems must monitor for
certain unregulated contaminants listed in
§141.40.
18. This citation refers to if 1415 and 1416 of
the Safe Drinking Water Act. §§ 1415 and 1416
require that "a schedule prescribed. . . for a
public water system granted a variance [or
exemption] shall require compliance by the
system. . ."
19. In addition to §§1415 and 1416 of the Safe
Drinking Water Act, 40 CFR 142.307 specifies
the items and schedule milestones that must
be included in a variance for small systems.
20, Other waterborne emergencies require a
Tier 1 public notice under § 141.202(a) for situ-
ations that do not meet the definition of a
waterborne disease outbreak given in 40 CFR
141,2 but that still have the potential to have
serious adverse effects on health as a result
of short-term exposure. These could include
outbreaks not related to treatment defi-
ciencies, as well as situations that have the
potential to cause outbreaks, such as fail-
ures or significant interruption in water
treatment processes, natural disasters that
disrupt the water supply or distribution sys-
tem, chemical spills, or unexpected loading
of possible pathogens into the source water.
21, Primacy agencies may place other situ-
ations in any tier they believe appropriate,
based on threat to public health.
[65 FR 26035, May 4, 2000, as amended at 65
PR 76750, Dec.7, 2000; 66 PR 7065, Jan. 22, 2001;
66 PR 31104. June 8, 2001: 67 PR 1836, Jan. 14,
2002]
EFFECTIVE DATE NOTE: At 69 PR 38856, June
29, 2004, appendix A to snbpart Q of part 141
was amended in entry I.A.(8) by removing
the citation in the third column "141.76" and
adding in its place "141.76(c)" and by remov-
ing the citation in the fifth column "141.76"
and adding in its place "141.76 (b), (d)", and in
endnote 1 by removing the words "reporting
violations and" from the first parenthetical
phrase, effective July 29, 2004.
APPENDIX B TO SUBPART Q OF PART 141—STANDARD HEALTH EFFECTS LANGUAGE
FOR PUBLIC NOTIFICATION
Contaminant
MCLG1 rrig/L MCL2 rng/L
Standard health effects language for public notification
National Primary Drinking Water Regulations (NPDWR)
A. Microbiological Contaminants
1a. Total conform
1b, Fecal coliform/E.
coli.
2a. Turbidity (MCL)4 ...
2b. Turbidity (SWTR
TT)6.
See footnote 3
: Zero
1
T
NTU«/S
NTU
T7
Conforms are bacteria that are naturally present in the environment
and are used as an indicator that other, potentially-harmful, bac-
teria may be present. Conforms were found in more samples than
allowed and this was a warning of potential problems.
Fecal coliforms and E, coil are bacteria whose presence indicates
that the water may be contaminated with human or animal
wastes. Microbes in these wastes can cause short-term effects,
such as diarrhea, cramps, nausea, headaches, or other symp-
toms. They may pose a special health risk for infants, young chil-
dren, some of the elderly, and people wrfh severely compromised
immune systems.
Turbidity has no health effects. However, turbidity can interfere with
disinfection and provide a medium for microbial growth. Turbidity
may indicate the presence of disease-causing organisms. These
organisms include bacteria, viruses, and parasites that can cause
symptoms such as nausea, cramps, diarrhea and associated
headaches.
Turbidity has no health effects. However, turbidity can interfere with
disinfection and provide a medium for microbiai growth- Turbidity
may indicate the presence of disease-causing organisms- These
organisms include bacteria, viruses, and parasites that can cause
symptoms such as nausea, cramps, diarrhea and associated
headaches.
546
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Environmental Protection Agency
Pt. 141,Subpt. Q, App. B
Contaminant
2c. Turbidity (IESWTH
TT and LT1 ESWTR
TT)».
MCLQ1 mg/L
None
MCL2 mg/L
TT
Standard health effects language for public notification
Turbidity has no health effects. However, turbidity can interfere with
disinfection and provide a medium for microbiai growth. Turfcidity
may indicate the presence of disease-causing organisms. These
organisms include bacteria, viruses, and parasites that can cause
symptoms such as nausea, cramps, diarrhea and associated
headaches.
B, Surface Water Treatment Rule (SWTR), Interim Enhanced Surface Water Treatment Bute (IESWTH), Long Term 1 Enhanced
Surface Water Treatment Bute {LT1 ESWTR) and the Filter Backwash Recycling Rule (FBRR) violations
3. Giardia lamblia
(SWTR/IESWTR/
LT1 ESWTR).
4. Viruses (SWTR/
IESWTFV
LT1 ESWTR).
5. Heterotrophic plate
count (HPC) bac-
teria3 (SWTR/
IESWTR/
LT1 ESWTR).
Zero
Trio
6. Legionella (SWTR/ j
IESWTR/
LT1 ESWTR).
7. Ctyptosporidium
(IESWTR/FBRR/
LT1 ESWTR).
Inadequately treated water may contain disease-causing organisms.
These organisms include bacteria, viruses, and parasites
which
can cause symptoms such as nausea, cramps, diarrhea, and as-
sociated headaches.
C. Inorganic Chemicals (lOCs)
8. Antimony
O.Q06
9. Arsenic11 0
O.QQ6
Some people who drink water containing antimony well in excess of
the MCL over many years could experience increases in
cholesterol and decreases in blood sugar.
0,010 Some people who drink water containing arsenic in excess
MCL over many years could experience skin damage or
blood
of the
prob-
lems with their circulatory system, and may have an increased
10. Asbestos (10 ^m) „ ! 7 MFL12
11. Barium ,...,, ; 2
12- Beryllium
13. Cadmium
14- Chromium (total) ....
15. Cyanide
10, Fluoride
17, Mercury (inorganic)
0.004
0.1
0.2
0.002
18. Nitrate 10
risk of getting cancer.
7 MFL i Some people who drink water containing asbestos in excess of the
i MCL over many years may have an increased risk of developing
; benign intestinal polyps
2 , Some people who drink water containing barium in excess of the
i MCL over many years coufd experience an increase in their
i blood pressure.
0.004 i Some people who drink water containing beryllium well in excess of
the MCL over many years could develop intestinal lesions.
0.005 Some people who drink water containing cadmium in excess of the
i MCL over many years could experience kidney damage.
0-1 ! Some people who use water containing chromium well in excess of
; the MCL over many years could experience allergic dermatitis.
0.2 Some people who drink water containing cyanide well in excess of
i the MCL over many years could experience nerve damage or
j j problems with their thyroid.
[ 4,0 j Some people who drink wafer containing fluoride in excess of the
MCL over many years could gel bone disease, including pain and
tenderness of the bones. Fluoride in drinking water at naif the
MCL or more may cause mottling of children's teeth, usually in
children less than nine years old. Mottling, also known as dental
fluorosis, may include brown staining and/or pitting of the teeth,
and occurs only in developing teeth before they erupt from Jhe
gums.
Some people who drink water containing inorganic mercury well in
excess of the MCL over many years couid experience kidney
damage.
Infants below the age of six months who drink water containing ni-
trate in excess of the MCL could become seriously ill and, if un-
treated; may die. Symptoms include shortness of breath and blue
baby syndrome.
Infants below the age of six months who drink water containing ni-
trite in excess of the MCL could become seriously ill and, if un-
treated, may die Symptoms include shortness of breath arid blue
baby syndrome.
541/
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Pt. 141,Subpt. Q, App. B
40 CFR Ch. I (7-1-04 Edition)
Contaminant MCLG1 mg/L MCL2 mg/L Standard health effects language for public notification
20. Total Nitrate and
Nitrite.
21, Selenium ,.,.„..
22. Thallium ,
10
0,05
0,0005
10 Infants below the age of six months who drink water containing ni-
I trafe and nitrite in excess of the MCL couid become seriously il!
| and, if untreated, may die. Symptoms include shortness of breath
i and blue baby syndrome-
0,05 ; Selenium is an essential nutrient. However, some people who drink
water containing selenium in excess of the MCL over many years
• could experience hair of fingernail losses, numbness in fingers or
toes, or problems with their circulation.
0.002 j Some people who drink water containing thallium in excess of the
MCL over many years could experience hair loss, changes in
their blood, or problems with their kidneys, intestines, or liver.
D. Lead and Copper Rule
24. Copper .
Zero
1.3
Infants and children who drink water containing iead in excess of
the action ieve! could experience delays in their physical or men-
tal development. Children could show slight deficits in attention
span and learning abilities Adults who drink this water over many
years could develop kidney problems or high blood pressure.
Copper is an essential nutrient, but some people who drink water
containing copper in excess of the action level over a relatively
short amount of time could experience gastrointestinal distress,
Some people who drink water containing copper in excess of the
action level over many years could suffer liver or kidney damage.
People with Wilson's Disease should consult their personal doc-
tor.
25, 2,4-D ,
E, Synthetic Organic Chemicals (SOCs)
0.07
26. 2,4,5-TP (Silvex) ... | O.Q5
27. Alachlor 1 Zero
0,07
29, Benzo(a)pyrene
(PAHs).
30. Carbofuran
31. Chlordane ,
32. Dalapon
33. Di(2-ethylhexyl) adi-
pate.
34. Di(2-ethyihexy!)
phthalate.
35. Dibromochloro-
propane (DBCP).
36. Dinoseb
0,003
Zero
0,04
0.2
0.4
Zero
0.007
0,4
37. Dioxin (2,3.7,8- [ Zero
TCDD). '
38. Diquat „, 1 0.02
0,0002
0.007
3x10~8
0,02
Some people who drink water containing the weed killer 2,4-O well
in excess of the MCL over many years could experience prob-
lems with their kidneys, liver, or adrenal glands.
Some people who drink water containing siivex in excess of the
MCL over many years could experience liver problems.
Some people who drink wafer containing alachlor in excess of the
MCL over many years could have problems with their eyes, liver,
I kidneys, or spieen, or experience anemia, and may have an in-
{ creased risk of getting cancer.
i Some people who drink water containing atrazine well in excess of
• the MCL over many years could experience problems with their
cardiovascular system or reproductive difficulties,
Some people who drink water containing benzo{a)pyrene in excess
of the MCL over many years may experience reproductive dif-
ficulties and may have an increased risk of getting cancer.
Some people who drink water containing carbofuran in excess of
the MCL over many years could experience problems with their
blood, or nervous or reproductive systems.
Some people who drink water containing chlordane in excess of the
MCL over many years could experience problems with their liver
or nervous system, and may have an increased risk of getting
cancer.
Some people who drink water containing dalapon well in excess of
the MCL over many years couid experience minor kidney
changes.
Some people who drink water containing di(2-ethyihexyl) adipate
weil in excess of the MCL over many years could experience
toxic effects such as weight loss, liver enlargement or possible
reproductive difficulties.
Some people who drink water containing di(2-ethylhexyl) phthalate
well in excess of the MCL over many years may have problems
with their liver, or experience reproductive difficulties, and may
have an increased risk of getting cancer.
Some people who drink water containing DBCP in excess of the
MCL over many years could experience reproductive difficulties
and may have an increased risk of getting cancer,
Some people who drink water containing dinoseb well in excess of
the MCL over many years couid experience reproductive difficul-
ties.
Some people who drink water containing dioxin in excess of the
MCL over many years could experience reproductive difficulties
and may have an increased risk of getting cancer.
Some people who drink water containing diquat in excess of the
yCL over many years couid get cataracts.
548
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Environmental Protection Agency
Pt Ul.Subpt. Q, App. B
Contaminant
39. Endothal! ................
40. Endrin
41, Ethylene dibromide
42. Giyphosate ........
43. Heptachlor .....„,.
MCLG1 mg/L
0.1
0.002
Zero
z mg/L
0,7
Zero
44, Heptachlor epoxide
45, Hexachlorobenzene Zero
48, Hexaohlorocyclo-
pentadiene.
47, Lindane
0.05
| 0,0002
48. Methoxychlor ......... | 0.04
I
49. Oxamy! (Vydate) .,.. 0.2
50. Pentachlorophenol Zero
51- Picioram .,..., ; 0.5
52. Polychlorinated [ Zero
biphenyls (PCBs).
53, Sirnazine
54. Toxaphene ............. j Zero
55- Benzene ,. Zero
56, Carbon tetra-
chloride.
57. Chlorobenzene
(monochloro- ben-
zene).
58. o-Diehiorobenzene
59, p-Dichiofobenzene
0.1
0.002
0.00005
i
0,7
0,0004
jG.05
! 0.04
•0,2
0.001
0.5
j 0.0005
0.003
Standard health effects language lor public notification
Some people who drink water containing endothall in excess of the
MCL over many years could experience problems with their stom-
ach or intestines.
Some people who drink water containing endrin in excess of the
MCL over many years could experience liver problems.
Some people who drink water containing ethylene dibromide in ex-
cess of the MCL over many years could experience problems
with their liver, stomach, reproductive system, or kidneys, and
may have an increased risk of getting cancer.
Some people who drink water containing giyphosate in excess of
the MCL over many years could experience problems with their
kidneys or reproductive difficulties.
Some people who drink water containing heptachlor in excess of
the MCL over many years could experience liver damage and
may have an increased risk of getting cancer.
Some people who drink water containing heptachlor epoxide in ex-
cess of the MCL over many years could experience liver damage,
and may have an increased risk of getting cancer
Some people who drink water containing hexachlorobenzene in ex-
cess of the MCL over many years could experience problems
with their liver or kidneys, or adverse reproductive effects, and
may have an increased risk of getting cancer.
Some people who drink water containing
hexschlorocyciopentadiene well in excess of me MCL over many
years could experience problems with their kidneys or stomach,
Some peopie who drink water containing findane in excess of the
MCL over many years could experience problems with their kid-
neys or liver.
Some people who drink water containing rnethoxycnlor in excess of
the MCL over many years could experience reproductive difficul-
ties.
Some people who drink water containing oxamyl in excess of the
MCL over many years couid experience slight nervous system ef-
fects.
Some people who drink wafer containing pentachloropheno! in ex-
cess of the MCL over many years could experience problems
with their liver or kidneys, and may have an increased risk of get-
ting cancer.
j Some people who drink water containing picloram in excess of the
', MCL over many years could experience problems with their liver.
j Some people who drink water containing PCBs in excess of the
MCL over many years could experience changes in their skin,
| problems with their thymus gland, immune deficiencies, or repro-
ductive or nervous system difficulties, and may have an in-
creased risk of getting cancer.
Some people who drink water containing simazine in excess of the
MCL over many years could experience problems with their
blood.
Some people who drink water containing toxaphene in excess of
the MCL over many years couid have problems with their kid-
neys, liver, or thyroid, and may have an increased risk of getting
cancer.
F. Volatile Organic Chemicals (VOCs)
0.1
0.8
0,075
Some people who drink water containing benzene in excess of the
MCL over many years could experience anemia or a decrease in
j blood platelets, and may have an increased risk of getting can-
| cer.
Some people who drink water containing carbon fetrachioride in ex-
' cess of the MCL over many years could experience problems
with their liver and may have an increased risk of getting cancer.
Some people who drink water containing cnlorobenzene in excess
of the MCL over many years could experience problems with
their fiver or kidneys.
Some people who drink water containing o-dichiorobenzene well in
excess of the MCL over many years coufd experience problems
with their liver s kidneys, or circulatory systems.
Some people who drink water containing p-dichlorobenzene in ex-
cess of the MCL over many years could experience anemia,
damage to their liver, kidneys, or spleen, or changes in their
blood.
549
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Pt, 141,Subpt. Q, App. B
40 CFR Ch. I (7-1-04 Edition)
Contaminant
60, 1,2-Dichloroethane
61. 1,1-
Dichloroethylene.
62. cfe-1,2-
Dichloroethylene.
63- frans-1,2-
Dichloroethyiene.
64. Dichtoromethane ...
65, 1,2-
Diehloropropane.
66. Ethylbenzene
67 Styrene
68, Tetrachloroethyfene
69 Toluene
70, 1,2,4-
Trichiorobenzene,
71. 1,f,l~Trichloro-
ethane.
72. 1,1,2-Trichloro-
ethane.
73. Trichioroethylene ...
74. Vinyl chloride ,..,
75. Xylenes (total)
MCLG ' mg/L
Zero
0.007
0.0?
0,1
Zero
Zero
0.7
0,1
Zero
1
0,0?
0,2
0,003
Zero
Zero
10
MCL s mg/L
0.005
0,007
0.07
0.1
0.005
0.005
0.7
0.1
0.005
1
0.07
0.2
0.005
0,005
0,002
10
Standard health effects language for public notification
Some people who drink water containing 1,2-dichloroethane in ex-
cess of the MCL over many years may have an increased risk of
getting cancer
Some people who drink water containing 1,1-dichioroethylene in ex-
cess of the MCL over many years could experience problems
with their liver.
Some people who drink water containing cis-1,2-dichioroefhyl6!ne in
excess of the MCL over many years could experience problems
with their liver.
Some people who drink water containing trans-1 ,2-dichloroethylene
well in excess of the MCL over many years could experience
problems with their liver.
Some people who drink water containing dichloromethane in excess
of the MCL over many years could have fiver problems and may
have an increased risk of getting cancer.
Some people who drink water containing 1 ,2-dichloropropane in ex-
cess of the MCL over many years may have an increased risk of
getting cancer.
Some people who drink water containing ethylbenzene well in ex-
cess of the MCL over many years could experience problems
with their liver or kidneys.
Some people who drink water containing styrene well in excess of
the MCL over many years could have problems with their liver,
kidneys, or circulatory system.
Some people who drink water containing tetrachioroethylene in ex-
cess of the MCL over many years could have problems with their
Nver, and may have an increased risk of getting cancer,
Some people who drink water containing toluene well in excess of
the MCL over many years could have problems with their nerv-
ous system, kidneys, or liver.
Some people who drink water containing 1,2,4-tnchlorobenzene
well in excess of the MCL over many years could experience
changes in their adrenal glands.
Some people who drink waier containing 1,1,1-trichtofoethane in
excess of the MCL over many years could experience problems
with their liver, nervous system, or circulatory system.
Some people who drink water containing 1,1,2-trichloroethane wel!
in excess of the MCL over many years could have problems with
their liver, kidneys, or immune systems,
Some people who drink water containing trichioroethyiene in excess
of the MCL over many years could experience problems with
their liver and may have an increased risk of getting cancer.
Some people who drink water containing vinyl chloride in excess of
the MCL over many years may have an increased risk of getting
cancer.
Some people who drink water containing xylenes in excess of the
MCL over many years could experience damage to their nervous
system.
76. Beta/photon
emitters.
77. Alpha emitters
78. Combined radium
(226 & 228).
G. Radioactive Contaminants
Zero 4 mrem/yr15 Certain minerals are radioactive and may emit forms of radiation
known as photons and beta radiation. Some people who drink
water containing beta and photon emitters in excess of the MCL
over many years may have an increased risk of getting cancer.
15 pCi/L16 | Certain minerals are radioactive and may emit a form of radiation
F known as alpha radiation. Some people who drink water con-
f taining alpha emitters in excess of the MCL over many years may
[ I have an increased risk of getting cancer.
5 pCi/L Some people who drink water containing radium 226 or 228 in ex-
cess of the MCL over many years may have an increased risk of
getting cancer.
550
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Environmental Protection Agency
Pt. 141, Subpt. Q, App. B
Contaminant | MCLG' rtig/L
79. Uranium16
Zero
MCL2mg/L
30 ug/L
Standard health effects language for public notification
Some people who drink water containing uranium in excess of the
MGL over many years may have an increased risk of getting can-
cer and kidney tcxicity-
H. Disinfection Byproducts (DBFs), Byproduct Precursors, and Disinfectant Residuals: Where disinfection is used in the treat-
ment of drinking water, disinfectants combine with organic and inorganic matter present in water to form chemicals called dis-
infection byproducts (DBFs). EPA sets standards for controlling the levels of disinfectants and DBFs in drinking water, includ-
ing trihalomethanes (THMs) and haioacelic acids (HAAs)17
!0. Total S N/A
trihalomethanes
{TTHMs).
81. Haloacetic Acids
(HAA),
82- Bromate
N/A
83. Chlorite „.,„.,.....,.,,. ; 0.08
84. Chlorine
4(MRDLG)2
4 (MRDLQ)
85, Chloramines
86a. Chlorine dioxide,
where any 2 con-
secutive daily sam-
ples taken at the en-
trance to the distribu-
tion system are
above the MRDL.
86b- Chlorine dioxide. ' 0,8 (MRDLG)
where one or more j
distribution system j
samples ate above >
the MRDL, I
I 0.10/0.080 •'
0-060 2
! 0.010
1.0
4,0 (MRDL)2
4,0 {MRDL)
0.8 (MRDLG) 0,8 (MRDL)
0.8 (MRDL)
87. Control of DBF pre-
cursors (TOC).
None
Some people who drink water containing trihalomethanes in excess
of the MCL over many years may experience problems with their
liver, kidneyss or central nervous system, and may have an in-
creased risk of getting cancer.
Some people who drink water containing haioacetic acids in excess
of the MCL over many years may have an increased risk of get-
ting cancer.
Some people who drink water containing bromate in excess of the
MCL over many years may have an increased risk of getting can-
cer.
Some infants and young children who drink water containing chlo-
rite in excess of the MCL could experience nervous system ef-
fects, Similar effects may occur in fetuses of pregnant women
who drink water containing chlorite in excess of the MCL, Some
people may experience anemia.
Some people who use water containing chlorine well in excess of
the MRDL could experience irritating effects to their eyes and
nose. Some people who drink water containing chlorine well in
excess of the MRDL could experience stomach discomfort.
Some people who use water containing chloramines well in excess
of the MRDL could experience irritating effects to their eyes and
nose. Some people who drink water containing chloramines well
in excess of the MRDL could experience stomach discomfort or
anemia.
Some infants and young children who drink water containing chlo-
rine dioxide in excess of the MRDL could experience nervous
system effects. Similar effects may occur in fetuses of pregnant
women who drink water containing chlorine dioxide in excess of
the MRDL, Some people may experience anemia.
! 40*0* for public notification only: The chlorine dioxide violations re-
[ ported today are the result of exceedances at the treatment facii-
I ity only, not within the distribution system which delivers water to
i consumers. Continued compliance with chlorine dioxide fevels
j within the distribution system minimizes the potential risk of these
I violations to consumers.
: Some infants and young children who drink water containing chio-
i rine dioxide in excess of the MRDL could experience nervous
j system effects. Similar effects may occur in fetuses of pregnant
! women who drink water containing chlorine dioxide in excess of
i the MRDL. Some people may experience anemia.
Add for public notification only: The chlorine dioxide violations re-
I ported today include exceedances of the EPA standard within the
| distribution system which delivers water to consumers. Violations
; ot the chlorine dioxide standard within the distribution system
j may harm human health based on short-term exposures. Certain
groups, including fetuses, infants, and young children, may be es-
pecially susceptible to nervous system effects from excessive
chlorine dioxide exposure.
Total organic carbon (TOC) has no health effects. However, total
organic carbon provides a medium for the formation of disinfec-
tion byproducts. These byproducts include trihalomethanes
{THMs) and haioacetic acids (HAAs). Drinking water containing
these byproducts in excess of the MCL may lead to adverse
health effects, liver or kidney problems, or nervous system ef-
fects, and may lead to an increased risk of getting cancer.
I, Other Treatment Techniques
S. Acrylamide ,
Zero
Some people who drink water containing high levels of acrylamide
over a long period of time could have problems with their nervous
system or blood, and may have an increased risk of getting can-
cer.
551
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Pt. 141,Subpt. Q, App. B
40 CFR Ch. I (7-1-04 Edition)
•
Contaminant
89, Epichlorohydrin ......
MCLG 1 mg/L
Zero
MCL2 mg/L
TT
Standard health effects language for public notification
Some people who drink water containing high levels of
eprchiorohydrin over a long period of time could experience stom-
ach problems, and may have an Increased risk of getting cancer.
APPENDIX B—ENDNOTES
1. MCLG—Maximum contaminant level
goal
2, MCL—Maximum contaminant level
3. For water systems analyzing at least 40
samples per month, no more than 5.0 percent
of the monthly samples may be positive for
total conforms. For systems analyzing fewer
than 40 samples per month, no more than one
sample per month may be positive for total
coliforms.
4. There are various regulations that set
turbidity standards for different types of sys-
tems, including 40 CFR 141.13, and the 1989
Surface Water Treatment Rule, the 1998 In-
terim Enhanced Surface Water Treatment
Rule and the 2001 Long Term 1 Enhanced
Surface Water Treatment Rule. The MCL for
the montly turbidity average is 1 NTU; the
MCL for the 2-day average is 5 NTU for sys-
tems that are required to filter but have not
yet installed filtration (40 CFR 141.13).
5. NTU—Nephelometric turbidity unit
6. There are various regulations that set
turbidity standards for different types of sys-
tems, including 40 CFR 141.13, and tie 1989
Surface Water Treatment Rule, the 1998 In-
terim Enhanced Surface Water Treatment
Rule and the 2001 Long Term 1 Enhanced
Surface Water Treatment Rule, Systems sub-
ject to the Surface Water Treatment Rule
(both filtered and unfiltered) may not exceed
5 NTU. In addition, in filtered systems, 95
percent of samples each month must not ex-
ceed 0.5 NTU in systems using conventional
or direct filtration and must not exceed 1
NTU in systems using slow sand or diatoma-
ceous earth filtration or other filtration
technologies approved by the primacy agen-
cy.
7, TT—Treatment technique
8. There are various regulations that set
turbidity standards for different types of sys-
tems, including 40 CFR 141,13, the 1989 Sur-
face Water Treatment Rule (SWTR), the 1998
Interim Enhanced Surface Water Treatment
Rule (IESWTR) and the 2001 Long Term 1 En-
hanced Surface Water Treatment Rule
(LT1BSWTR). For systems subject to the
IESWTR (systems serving at least 10,000 peo-
ple, using surface water or ground water
under the direct influence of surface water),
that use conventional filtration or direct fil-
tration, after January 1, 2002, the turbidity
level of a system's combined filter effluent
may not exceed 0.3 NTU in at least 95 per-
cent of monthly measurements, and the tur-
bidity level of a system's combined filter ef-
fluent must not exceed 1 NTU at any time.
Systems subject to the IESWTR using tech-
nologies other than conventional, direct,
slow sand, or diatomaceous earth filtration
must meet turbidity limits set by the pri-
macy agency. For systems subject to the
LT1ESWTR (systems serving fewer than
10,000 people, using surface water or ground
water under the direct influence of surface
water) that use conventional filtration or di-
rect filtration, after January 14, 2005 the tur-
bidity level of a system's combined filter ef-
fluent may not exceed 0.3 NTU in at least 95
percent of monthly measurements, and the
turbidity level of a system's combined filter
effluent must not exceed 1 NTU at any time.
Systems subject to the LT1ESWTR using
technologies other than conventional, direct,
slow sand, or diatomaceous earth filtration
must meet turbidity limits set by the pri-
macy agency.
9. The bacteria detected by heterotrophie
plate count (HPC) are not necessarily harm-
ful. HPC Is simply an alternative method of
determining disinfectant residual levels. The
number of such bacteria is an indicator of
whether there is enough disinfectant in the
distribution system.
10. SWTR, IESWTR, and LT1ESWTR treat-
ment technique violations that involve tur-
bidity exceedances may use the health ef-
fects language for turbidity instead.
11. These arsenic values are effective Janu-
ary 28, 2006. Until then, the MCL is 0.05 mg/
L and there is no MCLG.
12. Millions fibers per liter.
13. Action Level = 0,015 mg/L
14. Action Level = 1.3 mg/L
15. Millirems per years
16. The uranium MCL is effective Decem-
ber 8, 2003 for all community water systems.
17, Picoeuries per liter
18. Surface water systems and ground
water systems under the direct influence of
surface water are regulated under Subpart H
of 40 CFR 141, Subpart H community and
non-transient non-community systems serv-
ing 210,000 must comply with DBF MCLs and
disinfectant maximum residual disinfectant
levels (MRDLs) beginning January 1, 2002.
All other community and non-transient non-
community systems must meet the MCLs
and MRDLs beginning January 1, 2004. Sub-
part H transient non-community systems
serving 10,000 or more persons and using
chlorine dioxide as a disinfectant or oxidant
must comply with the chlorine dioxide
MRDL beginning- January 1, 2002. Subpart H
transient non-community systems serving-
fewer than 10,000 persons and systems using
552
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Environmental Protection Agency
Pt. 141,Subpt. Q, App, C
only ground water not under the direct influ-
ence of surface water and using chlorine di-
oxide as a disinfectant or oxidant must com-
ply with the chlorine dioxide MRDL begin-
ning January 1, 2004.
19. The MGL of 0.10 mg/1 for TTHMs is in
effect until January 1, 2002 for Subpart H
community water systems serving1 10,000 or
more. This MCL is in effect until January 1,
2004 for community water systems with a
population of 10,000 or more using only
ground water not under the direct influence
of surface water. After these deadlines, the
MCL will be 0.080 mg/1. On January 1, 2004,
all systems serving less than 10,000 will have
to comply with the new MCL as well.
20. The MCL for total trihalomethanes is
the sum of the concentrations of the indi-
vidual trihalomethanes.
21. The MCL for haloaoetic acids is the sum
of the concentrations of the individual
haloacetic acids.
22. MRDLG—Maximum residual disinfect-
ant level goal.
23. MRDL—Maximum residual disinfectant
level.
[65 FR 26043, May 4, 2000; 65 FR 38629, June 21,
2000; 65 PR 40521, 40522, June 30, 2000, as
amended at 65 FR 76751, Dec. 7, 2000; 66 FR
7065, Jan. 22, 2001; 66 FR 31104. June 8, 2001: 67
FR 1838, Jan. 14, 2002; 67 FR 70857, Nov. 27,
2002; 68 FR 14507, Mar. 25. 2003]
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29, 2004, appendix B to subpart Q of part 141
was amended by revising endnotes 4 and 8,
effective July 29, 2004. For the convenience of
the user, the revised text is set forth as fol-
lows:
APPENDIX B TO SUBPART Q OP PART
141—STANDARD HEALTH EFFECTS
LANGUAGE FOR PUBLIC NOTIFICA-
TION
4. There are various regulations that set
turbidity standards for different types of sys-
tems, including 40 CFR 141.13, and the 1989
Surface Water Treatment Rule, the 1998 In-
terim Enhanced Surface Water Treatment
Rule and the 2002 Long Term 1 Enhanced
Surface Water Treatment Rule. The MCL for
the monthly turbidity average is 1 XTU; the
MCL for the 2-day average is 5 NTU for sys-
tems that are required to filter but have not
yet installed filtration (40 CFR 141.13).
8. There are various regulations that set
turbidity standards for different types of sys-
tems, including 40 CFR 141.13, the 1989 Sur-
face Water Treatment Rule (SWTR), the 1998
Interim Enhanced Surface Water Treatment
Rule (IESWTR) and the 2002 Long Term 1 En-
hanced Surface Water Treatment Rule
(LT1ESWTR). For systems subject to the
IBSWTR (systems serving at least 10,000 peo-
ple, using surface water or ground water
under the direct influence of surface water),
that use conventional filtration or direct fil-
tration, after January 1, 2002, the turbidity
level of a system's combined filter effluent
may not exceed 0.3 NTU in at least 95 per-
cent of monthly measurements, and the tur-
bidity level of a system's combined filter ef-
fluent must not exceed 1 NTU at any time.
Systems subject to the IBSWTR using tech-
nologies other than conventional, direct.
slow sand, or diatomaceous earth filtration
must meet turbidity limits set by the pri-
macy agency. For systems subject to the
LT1ESWTR (systems serving fewer than
10,000 people, using surface water or ground
water under the direct influence of surface
water) that use conventional filtration or di-
rect filtration, after January 1, 2005, the tur-
bidity level of a system's combined filter ef-
fluent may not exceed 0.3 NTU in at least 95
percent of monthly measurements, and the
turbidity level of a system's combined filter
effluent must not exceed 1 NTU at any time.
Systems subject to the LT1BSWTR using
technologies other than conventional, direct,
slow sand, or diatomaceous earth filtration
must meet turbidity limits set by the pri-
macy agency.
APPENDIX C TO SUBPART Q OF PART
141—LIST OF ACRONYMS USED IN-
PUBLIC NOTIFICATION REGULATION
OCR Consumer Confidence Report
CWS Community Water System
DBF Disinfection Byproduct
EPA Environmental Protection Agency
HPC Heterotrophic Plate Count
IESWTR Interim Enhanced Surface Water
Treatment Rule
IOC Inorganic Chemical
LCR Lead and Copper Rule
MCL Maximum Contaminant Level
MCLG Maximum Contaminant Level Goal
MRDL Maximum Residual Disinfectant
Level
MRDLG Maximum Residual Disinfectant
Level Goal
NCWS Non-Community Water System
NPDWR National Primary Drinking Water
Regulation
NTNCWS Non-Transient Non-Community
Water System
NTU Nephelometric Turbidity Unit
OGWDW Office of Ground Water and Drink-
ing Water
OW Office of Water
PN Public Notification
PWS Public Water System
553
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§141.500
40 CFR Ch. I (7-1-04 Edition)
SDWA Safe Drinking Water Act
SMCL Secondary Maximum Contaminant
Level
SOC Synthetic Organic -Chemical
SWTR Surface Water Treatment Rule
TOR Total Ooliform Rule-
TT Treatment Technique
TWS Transient Non-Community Water Sys-
tem
VOC Volatile Organic Chemical
Subparts R-S [Reserved]
Subpart T—Enhanced Filtration
and Disinfection—Systems
Serving Fewer Than 10,000
People
SOURCE: 67 PR 1839, Jan. 14, 2002, unless
otherwise noted.
GENERAL REQUIREMENTS
§ 141.500 General requirements,
The requirements of this subpart
constitute national primary drinking
water regulations. These regulations
establish requirements for filtration
and disinfection that are in addition to
criteria under which filtration and dis-
infection are required under subpart H
of this part. The regulations in this
subpart establish or extend treatment
technique requirements in lieu of max-
imum contaminant levels for the fol-
lowing contaminants: Giardia lamblia,
viruses, heterotrophlc plate count bac-
teria, Legionella, Cryptosporidium and
turbidity. The treatment technique re-
quirements consist of installing and
properly operating water treatment
processes which reliably achieve;
(a) At least 99 percent (2 log) removal
of Cryptosporidium between a point
where the raw water is not subject to
recontamination by surface water run-
off and a point downstream before or at
the first customer for filtered systems,
or Cryptosporidium control under the
watershed control plan for unfiltered
systems; and
(b) Compliance with the profiling and
benchmark requirements in §§141.530
through 141.544.
§ 141.601 Who is subject to the require-
ments of subpart T?
You are subject to these require-
ments if your system:
(a) Is a public water system;
(b) Uses surface water or GWUDI as a
source; and
(c) Serves fewer than 10,000 persons.
§141.502 When must my system com-
ply with these requirements?
You must comply with these require-
ments in this subpart beginning Janu-
ary 14, 2005 except where otherwise
noted.
EFFECTIVE DATE NOTE: At 69 PR 38856, June
29, 2004, §141.502 was revised, effective July
29, 2004. For the convenience of the user, the
revised text is set forth as follows:
f 141.502 When must my system comply with
these requirements?
You must comply witlrthese requirements
in this subpart beginning January 1, 2005, ex-
cept where otherwise noted.
§ 141.503 What does subpart T require?
There are seven requirements of this
subpart, and you must comply with all
requirements that are applicable to
your system. These requirements are:
(a) You must cover any finished
water reservoir that you began to con-
struct on or after March 15, 2002 as de-
scribed in §§141.510 and 141.511;
(b) If your system Is an unfiltered
system, you must comply with the up-
dated watershed control requirements
described in §§141,520-141.522;
(c) If your system is a community or
non-transient non-community water
systems you must develop a disinfec-
tion profile as described in §§141.530-
141.536;
(d) If your system is considering
making a significant change to its dis-
infection practices, you must develop a
disinfection benchmark and consult
with the State for approval of the
change as described in §§141.540-141.544;
(e) If your system is a filtered sys-
tem, you must comply with the com-
bined filter effluent requirements as
described in §§141.550-141.553;
(f) If your system is a filtered system
that uses conventional or direct filtra-
tion, you must comply with the indi-
vidual filter turbidity requirements as
described in §§141.560-141.564; and
(g) You must comply with the appli-
cable reporting and recordkeeping re-
quirements as described in §§141.570
and 141.571.
554
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Environmental Protection Agency
§141,531
FINISHED WATER RESERVOIRS
§ 141.510 Is my system subject to the
new finished water reservoir re-
quirements?
All subpart H systems which serve
fewer than 10,000 are subject to this re-
quirement.
§ 141.511 What is required of new fin-
ished water reservoirs?
If your system begins construction of
a finished water reservoir on or after
March 15, 2002 the reservoir must be
covered. Finished water reservoirs for
which your system began construction
prior to March 15, 2002 are not subject
to this requirement,
ADDITIONAL WATERSHED CONTROL RE-
QUIREMENTS FOR UNFILTERED SYS-
TEMS
§ 141,520 Is my system subject to the
updated watershed control require-
ments?
If you are a subpart H system serving
fewer than 10,000 persons which does
not provide filtration, you must con-
tinue to comply with all of the filtra-
tion avoidance criteria in §141,71, as
well as the additional watershed con-
trol requirements in §141.521.
§141.521 What updated watershed
control requirements must my
unfiltered system implement to con-
tinue to avoid filtration?
Your system must take any addi-
tional steps necessary to minimize the
potential for contamination by
Cryptosporidium oocysts in the source
water. Your system's watershed con-
trol program must, for Cryptosporidium-'.
(a) Identify watershed characteristics
and activities which may have an ad-
verse effect on source water quality;
and
(b) Monitor the occurrence of activi-
ties which may have an adverse effect
on source water quality.
§141.522 How does the State deter-
mine whether my_ system's water-
shed control requirements are ade-
quate?
During an onsite inspection con-
ducted under the provisions of
§141.71(b)(3), the State must determine
whether your watershed control pro-
gram is adequate to limit potential
contamination by Cryptosporidium
oocysts. The adequacy of the program
must be based on the comprehensive-
ness of the watershed review; the effec-
tiveness of your program to monitor
and control detrimental activities oc-
curring in the watershed; and the ex-
tent to which your system has maxi-
mized land ownership and/or controlled
land use within the watershed.
DISINFECTION PROFILE
§ 141.530 What is a disinfection profile
and who must develop one?
A disinfection profile is a graphical
representation of your system's level of
Giardia lamblia or virus reactivation
measured during the course of a year.
If you are a subpart H community or
non-transient non-community water
systems which serves fewer than 10,000
persons, your system must develop a
disinfection profile unless your State
determines that your system's profile
is unnecessary. Your State may ap-
prove the use of a more representative
data set for disinfection profiling than
the data set required under §§141.532-
141.536.
EFFECTIVE DATE NOTE: At 69 FR 38856, June
29. 2004, §141.530 was amended in the second
sentence, by revising- "water systems" to read
"water system", effective July 29, 2004.
§ 141.531 What criteria must a State
use to determine that a profile is
unnecessary?
States may only determine that a
system's profile is unnecessary if a sys-
tem's TTHM and HAAS levels are below
0.064 mg/L and 0.048 mg'L, respectively.
To determine these levels. TTHM and
HAAS samples must be collected after
January 1. 1998, during- the month with
the warmest water temperature, and at
the point of maximum residence time
in your distribution system.
EFFECTIVE DATE NOTE: At 69 PR 38856. June
29, 2004, §141.531 was amended by adding: a
sentence to the end of the section, effective
July 29, 2004. For the convenience of the
user, the added text is set forth as follows:
1141.531 What criteria must a State use to
determine that a profile is unnecessary?
* * * Your State may approve a more rep-
resentative TTHM and HAAS data set to de-
termine these levels.
555
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§141.532
40 CFR Ch. I (7-1-04 Edition)
§ 141,532 How does my system develop
a disinfection profile and •when
must it begin?
A disinfection profile consists of
three steps:
(a) First, your system must collect
data for several parameters from the
plant as discussed In §141,533 over the
course of 12 months. If your system
serves between 500 and 9,999 persons
you must begin to collect data no later
than July 1, 2003. If your system serves
fewer than 500 persons you must begin
to collect data no later than January 1,
2004.
(b) Second, your system must use
this data to calculate weekly log inae-
tivation as discussed in §§141.534 and
141.535; and
(c) Third, your system must use
these weekly log inactivations to de-
velop a disinfection profile as specified
in §141.536.
§141,533 What data must my system
collect to calculate a disinfection
profile?
Your system must monitor the fol-
lowing parameters to determine the
total log inactivation using the analyt-
ical methods in §141.74 (a), once per
week on the same calendar day, over 12
consecutive months:
(a) The temperature of the dis-
infected water at each residual dis-
infectant concentration sampling point
during peak hourly flow;
(b) If your system uses chlorine, the
pH of the disinfected water at each re-
sidual disinfectant concentration sam-
pling point during peak hourly flow;
(c) The disinfectant contact time(s)
("T") during peak hourly flow; and
(d) The residual disinfectant con-
centration(s) ("0") of the water before
or at the first customer and prior to
each additional point of disinfection
during peak hourly flow.
§ 141.534 How does my system use this data to calculate an inactivation ratio?
Calculate the total inactivation ratio as follows, and multiply the value by 3.0
to determine log inactivation of Giardia lamblia:
If your system *
(a) Uses only one point of dis-
infectant application.
(b) Uses more than one point
of disinfectant application be-
fore the first customer
Your system must determine *
(1) One inactivation ratio (CTcalc/CT.» g) before or at the first customer during peak hourly flow
or
(2) Successive CTcalc/CTwi values, representing sequential inactivation ratios, between the
point of disinfectant application and a point before or at the first customer during peak hourly
flow. Under this alternative, your system must calculate the total inactivation ratio by deter-
mining (CTcalc/CT99.ci) for each sequence and then adding the (CTealc/CTy^) values to-
gether to determine (SCTcalc/CTw.,).
The (CTcalG/CTyy») value of each disinfection segment immediately prior to the next point of
disinfectant application, or for the final segment, before or at the first customer, during peak
hourly flow using the procedure specified in paragraph (a)(2) of this section.
EFFECTIVE DATE NOTE: At 69 FB 38856, June 29, 2004, § 141.534 was amended by revising the
introductory paragraph, and in the table in paragraph (a)(2), by removing the "3" and adding
in its place "£", effective July 29, 2004. For the convenience of the user, the revised text is
set forth AS follows:
§ 141,534 How does my system use this data to calculate an inactivation ratio?
Use the tables in §141.74(b)(3)(v) to determine the appropriate GT99.9 value. Calculate tlie
total inaotivatioa ratio as follows, and multiply the value by 3.0 to determine log inactiva-
tion of Giardia lamblia:
§ 141,535 What if my system uses
chloramines, ozone, or chlorine di-
oxide for primary disinfection?
If your system uses chloramines,
ozone, or chlorine dioxide for primary
disinfection, you must also calculate
the logs of inactivation for viruses and
develop an> additional disinfection pro-
file for viruses using methods approved
by the State.
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Environmental Protection Agency
§141,544
§ 141,536 My system has developed an
inactivation ratio; what must we do
now?
Each log inactivation serves as a
data point in your disinfection profile.
Your system will have obtained 52
measurements (one for every week of
the year). This will allow your system
and the State the opportunity to evalu-
ate how microbial inactivation varied
over the course of the year by looking
at all 52 measurements (your Disinfec-
tion Profile). Your system must retain
the Disinfection Profile data in graphic
form, such as a spreadsheet, which
must be available for review by the
State as part of a sanitary survey.
Your system must use this data to cal-
culate a benchmark if you are consid-
ering changes to disinfection practices.
DISINFECTION BENCHMARK
§141.540 Who has to develop a dis-
infection benchmark?
If you are a subpart H system re-
quired to develop a disinfection profile
under §§141.530 through 141.536, your
system must develop a Disinfection
Benchmark if you decide to make a
significant change to your disinfection
practice. Your system must consult
with the State for approval before you
can implement a significant disinfec-
tion practice change.
§ 141.541 What are significant changes
to disinfection practice?
Significant changes to disinfection
practice include:
(a) Changes to the point of disinfec-
tion;
(b) Changes to the disinfectant(s)
used in the treatment plant;
(c) Changes to the disinfection proc-
ess; or
(d) Any other modification identified
by the State.
§ 141.542 What must my system do if
we are considering a significant
change to disinfection practices?
If your system is considering a sig-
nificant change to its disinfection
practice, your system must calculate a
disinfection benchmark(s) as described
in §§141.543 and 141.544 and provide the
benchmark(s) to your State. Your sys-
tem may only make a significant dis-
infection practice change after con-
sulting with the State for approval.
Your system must submit the fol-
lowing information to the State as part
of the consultation and approval proc-
ess:
(a) A description of the proposed
change;
(b) The disinfection profile for
Giardia lamblia (and, if necessary, vi-
ruses) and disinfection benchmark;
(c) An analysis of how the proposed
change will affect the current levels of
disinfection; and
(d) Any additional information re-
quested by the State.
§ 141.543 How is the disinfection
benchmark calculated?
If your system is making a signifi-
cant change to its disinfection prac-
tice, it must calculate a disinfection
benchmark using the procedure speci-
fied in the following table.
To calculate a disinfection benchmark your system must perform the following steps
S!ep 1: Using the data your system collected to develop the Disinfection Profile, determine the average Giardia lamblia inactiva-
tion for each calendar month by dividing the sum of all GJardia Ismblia inactivations tor thai month by the number of values
calculated for that month.
Step 2: Determine the lowest monthly average value out of the twelve values. This value becomes the disinfection benchmark.
§141.544 What if my system uses
ehloramines, ozone, or chlorine di-
oxide for primary disinfection?
If your system uses ehloramines,
ozone or chlorine dioxide for primary
disinfection your system must cal-
culate the disinfection benchmark
from the data your system collected
for viruses to develop the disinfection
profile in addition to the Giardia
lamblia disinfection benchmark cal-
culated under §141.543. This viral
benchmark must be calculated in the
same manner used to calculate the
Giardia lamblia disinfection benchmark
in §141.543.
557
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§141.550
40 CFR Ch. I (7-1-04 Edition)
COMBINED FILTER EFFLUENT
REQUIREMENTS
§ 141.550 Is my system required to
meet subpart T combined filter ef-
fluent turbidity limits?
All subpart H systems which serve
populations fewer than 10,000, are re-
quired to filter, and utilize filtration
other than slow sand filtration or dia-
tomaceous earth filtration must meet
the combined filter effluent turbidity
requirements of §§141.551-141.553 . If
your system uses slow sand or diato-
maceous earth filtration you are not
required to meet the combined filter
effluent turbidity limits of subpart T,
but you must continue to meet the
combined filter effluent turbidity lim-
its in §141.73.
§141.551 What strengthened combined
filter effluent turbidity limits must
my system meet?
Your system must meet two
strengthened combined filter effluent
turbidity limits.
(a) The first combined filter effluent
turbidity limit is a "95th pereentile"
turbidity limit that your system must
meet in at least 95 percent of the tur-
bidity measurements taken each
month. Measurements must continue
to be taken as described in §141.74(a)
and (c). Monthly reporting must be
completed according to §141.570. The
following table describes the required
limits for specific filtration tech-
nologies.
table describes the required limits for
specific filtration technologies.
!f your system consists of * * *
Your 9Sih per-
centile turbidity
value is * * *
(1) Conventional Filtration or Direct Fil- j 0.3 NTU,
{ration. |
(2) A!! other "Alternative" Filtration .. ; A value determined
by the State (no
to exceed 1
NTU) based on
the demonstra-
tion described in
§141.552.
(b) The second combined filter efflu-
ent turbidity limit is a "maximum" tur-
bidity limit which your system may at
no time exceed during the month.
Measurements must continue to be
taken as described in §141.74(a) and (c).
Monthly reporting must be completed
according to §141.570. The following
if your system consists of * * *
1 Your maximum tur-
bidity value is * * *
(1) Conventional Filtration or Direct Fil-
1 NTU.
tration. j
(2) All other "Alternative" ....................... A value determined
by the State (not
to exceed 5
NTU} based on
the demonstra-
tion as described
in §141.552
EFFECTIVE DATE NOTE: At 69 PR 38856, June
29, 2004, §141.551 was amended in paragraph
(a)(2) by removing" "no" and adding in its
place "not", and in paragraph (b)(2) by remov-
ing "Alternative" and adding in its place '"Al-
ternative Filtration", effective July 29, 2004.
§ 141.552 My system consists of "alter-
native filtration" and is required to
conduct a demonstration—what is
required of my system and how
does the State establish my tur-
bidity limits?
(a) If your system consists of alter-
native filtration(filtration other than
slow sand filtration, diatomaceous
earth filtration, conventional filtra-
tion, or direct filtration) you are re-
quired to conduct a demonstration (see
tables in §141.551). Your system must
demonstrate to the State, using pilot
plant studies or other means, that your
system's filtration, in combination
with disinfection treatment, consist-
ently achieves:
(1) 99 percent removal of
Cryptosporidium oocysts;
(2) 99,9 percent removal and/or inac-
tivation of Giardia lamblia cysts; and
(3) 99.99 percent removal and/or inac-
tivation of viruses,
(b) [Reserved]
§ 141,553 My system practices lime
softening—is there any special pro-
vision regarding my combined filter
effluent?
If your system practices lime soft-
ening, you may acidify representative
combined filter effluent turbidity sam-
ples prior to analysis using a protocol
approved by the State.
558
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Environmental Protection Agency
§141.563
INDIVIDUAL FILTER TURBIDITY
REQUIREMENTS
§141.560 Is my system subject to indi-
vidual filter turbidity require-
ments?
If your system is a subpart H system
serving fewer than 10,000 people and
utilizing conventional filtration or di-
rect filtration, you must conduct con-
tinuous monitoring of turbidity for
each individual filter at your system.
The following requirements apply to
continuous turbidity monitoring:
(a) Monitoring must be conducted
using an approved method in §141.74(a);
(b) Calibration of turbidimeters must
be conducted using procedures speci-
fied by the manufacturer;
(c) Results of turbidity monitoring
must be recorded at least every 15 min-
utes;
(d) Monthly reporting must be com-
pleted according to §141,570; and
(e) Records must be maintained ac-
cording to §141,571,
§ 141.561 What happens if my system's
turbidity monitoring equipment
Mis?
If there is a failure in the continuous
turbidity monitoring equipment, your
system must conduct grab sampling
every four hours in lieu of continuous
monitoring until the turbidimeter is
back on-line. Your system has 14 days
to resume continuous monitoring be-
fore a violation is incurred,
§ 141.562 My system only has two or
fewer filters—is there any special
provision regarding individual fil-
ter turbidity monitoring?
Yes, if your system only consists of
two or fewer filters, you may conduct
continuous monitoring of combined fil-
ter effluent turbidity in lieu of indi-
vidual filter effluent turbidity moni-
toring. Continuous monitoring must
meet the same requirements set forth
in §141.560(a) through (d) and §141,561.
§141,563 What follow-up action is my
system required to take based on
continuous turbidity monitoring?
Follow-up action is required accord-
ing to the following tables:
Your system must '
(a) The turbidrty of
an individual filter
(or the turbidity of
combined fitter ef-
fluent (CFE) for
systems with 2 fil-
ters that monitor
CFE in lieu of in-
dividual filters)
exceeds 1.0 NTU
in two consecu-
tive recordings 15
minutes apart.
If a system was re-
quired to report to
the State ' * *
Report to the State by the 10th of the
fofiowing month and include the filter
nurnber(s), corresponding date(s),
turbidity value(s) which exceeded 1.0
NTU, and the cause (if known) for
theexceedanee(s).
(b) For three
months in a row
and turbidity ex-
ceeded 1.0 NTU
in two consecu-
tive recordings 15
minutes apart at
the same filter (or
CFE for systems
with 2 filters that
monitor CFE in
lieu of individual
filters).
(c) For two months
in a row and tur-
bidity exceeded
2.0 BTU in 2 con-
secutive record-
ings 15 minutes
apart at the same
filter {or CFE for
systems with 2 fil-
ters that monitor
CFE in lieu of in-
dividual filters).
Your system must
Conduct a self-assessment of the fil-
ter(s) within 14 days of the day the
filter exceeded 1.0 NTU in two con-
secutive measurements for the third
straight month unless a CPE as
specified in paragraph (c) of (his sec-
tion was required. Systems with 2 fil-
ters that monitor CFE in lieu of indi-
vidual filters must conduct a self as-
sessment on both filters. The self-as-
sessment must consist of at least the
following components: assessment
of filter performance; development of
a filter profile; identification and
prioritization of factors limiting filter
performance; assessment of the ap-
plicability of corrections; and prepa-
ration of a filter self-assessment re-
port. If a sett-assessment is required,
the date tha! it was triggered and the
date that it was completed.
Arrange to have a comprehensive per-
formance evaluation (CPE) con-
ducted by the State or a third party
approved by the State not later than
60 days following the day the filter
exceeded 2.0 NTU in two consecu-
tive measurements for the second
straight month. If a CPE has been
completed by the State or a third
party approved by the State within
the 12 prior months or the system
and State are jointly participating in
an ongoing Comprehensive Tech-
nical Assistance (CTA) project at the
system, a new CPE is not required.
If conducted, a CPE must be com-
pleted and submitted to the Stale no
later than 120 days following the day
the filter exceeded 2.0 NTU in two
consecutive measurements for the
second straight month.
EFFECTIVE DATE NOTE: At 69 PR 38856, June
29, 2004, §141.563 was amended in paragraph
(b) by removing the last sentence in the sec-
ond column of the table, and in paragraph (c)
by removing "BTU" and adding la its place
"NTU" in the first column of the table, effec-
tive July 29, 2004.
559
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§141.564
40 CFR Ch. I (7-1-04 Edition)
§ 141.564 My system practices lime
softening—is there any special pro-
vision regarding my individual fil-
ter turbidity monitoring?
If your system utilizes lime soft-
ening, you may apply to tlie State for
alternative turbidity exceedaace levels
for the levels specified in the table in
§141.563. You must be able to dem-
onstrate to the State that higher tur-
bidity levels are due to lime carryover
only, and not due to degraded filter
performance.
REPORTING AND BECORDKEEPING
REQUIREMENTS
§141,570 What does subpart T require
that my system report to the State?
This subpart T requires your system
to report several items to the State.
The following table describes the items
which must be reported and the fre-
quency of reporting. Your system is re-
quired to report the information de-
scribed in the following table, if it is
subject to the specific requirement
shown in the first column.
Corresponding
requirement
Description of information to report
Frequency
(a) Combined Filter Etlyent
Requirements.
(§§141.550-141.553)
(b) Individual Turbidity Re-
quirements.
(§§141.560-141.564)
(c) Disinfection Profiling
(§§141.530-141.536)
(d) Disinfection
Benchmarking.
(§§141.540-141.544)
(1) The total "number of filtered water turbidity meas-
urements taken during the month.
(2) The number and percentage of filtered water tur-
bidity measurements taken during the month which
are less than or equal to your system's required
95th percentite limit.
(3) The date and value of any turbidity measurements
taken during the month which exceed the maximum
turbidity value for your filtration system.
(1) That your system conducted individual filter tur-
bidity monitoring during the month.
(2) The filter number(s), corresponding date(s), and
the turbidity vaiue(s) which exceeded 1.0 NTU dur-
ing the month, but only if 2 consecutive measure-
ments exceeded 1.0 NTU.
(3) If a self-assessment is required, the dale that it
was triggered and the date that it was completed.
(4) If a CPE is required, that the CPE is required and
the date that it was triggered.
(5) Copy of completed CPE report
(1) Results of optional monitoring which show TTHM
levels <0.064 mg/I and HAAS levels <0.04B mg/1
(Only if your system wishes to forgo profiling) or that
your system has begun disinfection profiling.
(1) A description of the proposed change in disinfec-
tion, your system's disinfection profile for Qiardia
iamblia (and, if necessary, viruses) and disinfection
benchmark, and an analysis of how the proposed
change will affect the current levels of disinfection.
By the 10th of the following month;
By the 10th of the following month.
By the 1Qth of the following month.
By the 10th of the following month.
By the 10th of the following month.
By the 10th of the following month (or 14
days after the self-assessment was
triggered only if the self-assessment
was triggered during the last four days
of the month)
By the 10th of the following month.
Within 120 days after the CPE was trig-
(!) For systems serving 500-9,999 by
July 1, 2003;
(ii) For systems serving fewer than 500
by January 1, 2004.
Anytime your system is considering a
significant change to its disinfection
practice.
EFFECTIVE DATE NOTE: At 69 FE 38857, June 29, 2004, §141.570 was amended by revising para-
graph (b}(2) m the table, effective July 29, 2004. For the convenience of the user, the revised
text is set forth as follows:
1141.670 What does subpart T require that my system report to the State?
Corresponding
requirement
Description of information to report
Frequency
560
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Environmental Protection Agency
Pt. 142
Corresponding
requirement
Description of information to report
Frequency
(b) individual Filter Turbidity
Requirements
(§§141,560-141.564).
(2) The filter number(s), corresponding dale(s), and I By the 10th of the following month-
the turbidity value(s) which exceeded 1.0 NTU dur-
ing the month, and the cause (if known) for the ex-
eeedance(s), but only if 2 consecutive measure-
ments exceeded 1.0 NTU.
§ 141.571 What records does subpart T require my system to keep?
Your system must keep several types of records based on the requirements of
subpart T, in addition to recordkeeping requirements under §141.75, The following:
table describes the necessary records, the length of time these records must be
kept, and for which requirement the records pertain. Your system is required to
maintain records described in this table, if it is subject to the specific require-
ment shown in the first column.
Corresponding requirement
Description of necessary records
Duration of
time records
must be kept
fa} Individual Filter Turbidity Requirements
(§§141,560-141,554)
(b) Disinfection Profiling ,,. .,..„.
{§§141.530-141.536)
(c) Disinfection Benchmarking ,.....,.,...,,
{§§141.540-141 544)
i Results of individual filter monitoring .,,
............. ; At leasts
: | years.
......... Results of Profile (including raw data and analysis) .... ] indefinitely
,.... Benchmark (including raw data and analysis) i Indefinitely,
PART 142—NATIONAL PRIMARY
DRINKING WATER REGULATIONS
IMPLEMENTATION
Sec.
142.1
142.2
142,3
142.4
Subpart A—General Provisions
Applicability.
Definitions.
Scope.
State and local authority.
Subpart B—Primary Enforcement
Responsibility
142.10 Requirements for a determination of
primary enforcement responsibility.
142.11 Initial determination of primary en-
forcement responsibility.
142.12 Revision of State programs.
142.13 Public hearing-.
142.14 Records kept by States.
142.15 Reports by States.
142.16 Special primacy requirements.
142.17 Review of State programs and proce-
dures for withdrawal of approved pri-
macy programs.
142.18 EPA review of State monitoring de-
terminations.
142.19 EPA review of State implementation
of national primary drinking' water regu-
lations for lead and copper.
Subpart C—Review of State-Issued
Variances and Exemptions
142.20 State-issued variances and exemp-
tions under Section 1415(a) and Section
1416 of the Act.
142.21 State consideration of a variance or
exemption request.
142.22 Review of State variances, exemp-
tions and schedules.
142.23 Notice to State.
142.24 Administrator's rescission.
Subpart D—Federal Enforcement
142.30 Failure by State to assure enforce-
ment.
142.31 [Reserved]
142.32 Petition for public hearing,
142.33 Public hearing-.
142.34 Entry and inspection of public water
systems.
Subpart E—Variances issued by the Ad-
ministrator Under Section 1415(a) of
the Act
142.40 Requirements for a variance,
142.41 Variance request.
142.42 Consideration of a variance request.
142.43 Disposition of a variance request,
142,44 Public hearing's on variances and
schedules.
142.45 Action after hearing.
142.46 Alternative treatment techniques.
561
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§142.1
40 CFR Ch. I (7-1-04 Edition)
Subpart F—Exemptions Issued by the
Administrator
142.50 Requirements for an exemption.
142.51 Exemption request.
142.52 Consideration of an exemption re-
quest.
142.53 Disposition of an exemption request.
142.54 Public hearings on exemption sched-
ules,
142.55 Final schedule.
142.56 Extension of date for compliance.
142.57 Bottled water, point-of-ase, and
point-of-entry devices.
Subpart G—Identification of Best Tech-
nology, Treatment Techniques or Other
Means Generally Available
142.60 Variances from the maximum con-
taminant level for total
trihalometlianes.
142.61 Variances from the maximum con-
taminant level for fluoride.
142,62 Variances and exemptions from the
maximum contaminant levels for organic
and inorganic chemicals.
142.63 Variances and exemptions from the
maximum contaminant level for total
coliforms.
142.64 Variances and exemptions from the
requirements of part 141, subpart H—Fil-
tration and Disinfection.
142.65 Variances and exemptions from the
maximum contaminant levels for radio-
nuclides.
Subpart H—Indian Tribes
142.72 Requirements for Tribal eligibility.
142,76 Bequest by an Indian Tribe for a de-
termination of eligibility,
142.78 Procedure for processing an Indian
Tribe's application.
Subpart I—Administrator's Review of State
Decisions that Implement Criteria
Under Which Filtration Is Required
142.80 Review procedures.
142.81 Notice to the State.
Subpart J [Reserved]
Subpart K—Variances tor Small System
GENERAL PROVISIONS
142.301 What is a small system variance?
142.302 Who can issue a small system vari-
ance?
142.303 Which size public water systems can
receive a small system variance?
142.304 For which of the regulatory require-
ments is a small system variance avail-
able?
142,305 When can a small system variance
be granted by a State?
REVIEW OF SMALL SYSTEM VARIANCE
APPLICATION
142.306 What are the responsibilities of the
public water system, State and the Ad-
ministrator in ensuring that sufficient
information is available and for evalua-
tion of a small system variance applica-
tion?
142.307 What terms and conditions must be
included in a small system variance?
PUBLIC PARTICIPATION
142.308 What public notice is required before
a State or the Administrator proposes to
issue a small system variance?
142.309 What are the public meeting require-
ments associated with the proposal of a
small system variance?
142.310 How can a person served by the pub-
lic water system obtain EPA review of a
State proposed small system variance?
EPA REVIEW AND APPROVAL OF SMALL
SYSTIM VARIANCES
142.311 What procedures allow for the Ad-
ministrator to object to a proposed small
system variance or overturn a granted
small system variance for a public water
system serving 3,300 or fewer persons?
142.312 What EPA action is necessary when
a State proposes to grant a small system
variance to a public water system serv-
ing a population of more than 3,300 and
fewer than 10,000 persons?
142.313 How will the Administrator review a
State's program under this subpart?
AUTHORITY: 42 U.S.C. 300f, 300g-l, 300g-2,
300g-3, 300g~4, 30Qg~5, 300g-6, 30Q;M, 300J-9,
and 300J-11.
SOURCE: 41 PR 2918, Jan. 20, 1976, unless
otherwise noted.
Subpart A—General Provisions
§ 142.1 Applicability.
This part sets forth, pursuant to sec-
tions 1413 through 1416, 1445, and 1450 of
the Public Health Service Act, as
amended by the Safe Drinking Water
Act, Public Law 93-523, regulations for
the implementation and enforcement
of the national primary drinking water
regulations contained in part 141 of
this chapter.
§ 142.2 Definitions.
As used in this part, and except as
otherwise specifically provided:
Act means the Public Health Service
Act.
562
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Environmental Protection Agency
§142.2
Administrator means the Adminis-
trator of the United States Environ-
mental Protection Agency or his au-
thorized representative.
Agency means the United States En-
vironmental Protection Agency.
Approved State primacy program con-
sists of those program elements listed
in §142.11(a) that were submitted with
the initial State application for pri-
mary enforcement authority and ap-
proved by the EPA Administrator and
all State program revisions thereafter
that were approved by the EPA Admin-
istrator.
Contaminant means any physical,
chemical, biological, or radiological
substance or matter in water.
Federal agency means any depart-
ment, agency, or instrumentality of
the United States.
Indian Tribe means any Indian Tribe
having a Federally recognized gov-
erning body carrying' out substantial
governmental duties and powers over a
defined area.
Interstate Agency means an agency of
two or more States established by or
under an agreement or compact ap-
proved by the Congress, or any other
agency of two or more States or Indian
Tribes having substantial powers or du-
ties pertaining to the control of pollu-
tion as determined and approved by the
Administrator.
Maximum contaminant level means the
maximum permissible level of a con-
taminant in water which is delivered to
the free flowing outlet of the ultimate
user of a public water system; except in
the case of turbidity where the max-
imum permissible level is measured at
the point of entry to the distribution
system. Contaminants added to the
water under circumstances controlled
by the user, except for those resulting
from corrosion of piping and plumbing
caused by water quality are excluded
from this definition,
Municipality means a city, town, or
other public body created by or pursu-
ant to State law, or an Indian Tribe
which does not meet the requirements
of subpart H of this part.
National primary drinking water regu-
lation means any primary drinking
water regulation contained in part 141
of this chapter.
Person means an individual; corpora-
tion: company; association; partner-
ship; municipality; or State, federal, or
Tribal agency.
Primary enforcement responsibility
means the primary responsibility for
administration and enforcement of pri-
mary drinking water regulations and
related requirements applicable to pub-
lic water systems within a State.
Public water system or PWS means a
system for the provision to the public
of water for human consumption
through pipes or, after August 5, 1998,
other constructed conveyances, if such
system has at least fifteen service con-
nections or regularly serves an average
of at least twenty-five individuals
daily at least 60 days out of the year.
Such term includes:
Any collection, treatment, storage,
and distribution facilities under con-
trol of the operator of such system and
used primarily in connection with such
system; and any collection or
pretreatment storage facilities not
under such control which are used pri-
marily in connection with such system.
Such term does not include any "spe-
cial irrigation district," A public water
system is either a "community water
system" or a "noncommunity water
system" as defined in § 141.2.
Sanitary survey means an onsite re-
view of the water source, facilities,
equipment, operation and maintenance
of a public water system for the pur-
pose of evaluating the adequacy of such
source, facilities, equipment, operation
and maintenance for producing and dis-
tributing safe drinking water,
Service connection, as used in the defi-
nition of public water system, does not
include a connection to a system that
delivers water by a constructed con-
veyance other than a pipe if:
(1) The water is used exclusively for
purposes other than residential uses
(consisting of drinking, bathing, and
cooking, or other similar uses);
(2) The Administrator or the State
exercising primary enforcement re-
sponsibility for public water systems,
determines that alternative water to
achieve the equivalent level of public
health protection provided by the ap-
plicable national primary drinking
563
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§142.3
40 CFi Ch. I (7-1-04 Edition)
water regulation is provided for resi-
dential or similar uses for drinking- and
cooking; or
(3) The Administrator or the State
exercising primary enforcement re-
sponsibility for public water systems,
determines that the water provided for
residential or similar uses for drinking,
cooking, and bathing is centrally treat-
ed or treated at the point of entry "by
the provider, a pass-through entity, or
the user to achieve the equivalent level
of protection provided by the applica-
ble national primary drinking water
regulations.
Special irrigation district means an ir-
rigation district in existence prior to
May 18, 1994 that provides primarily
agricultural service: through a piped
water system with only incidental resi-
dential or similar use where the system
or the residential or similar users of
the system comply with the exclusion
provisions in section 1401(4)(B)(i)(II) or
(III).
State means one of the States of the
United States, the District of Colum-
bia, the Commonwealth of Puerto Rico,
the Virgin Islands, Guam, American
Samoa, the Commonwealth of the
Northern Mariana Islands, the Trust
Territory of the Pacific Islands, or an
eligible Indian tribe.
State primary drinking water regulation
means a drinking water regulation of a
State which is comparable to a nar
tional primary drinking water regula-
tion.
State program revision means a change
in an approved State primacy program.
Supplier of water means any person
who owns or operates a public water
system.
Treatment technique requirement
means a requirement of the national
primary drinking water regulations
which specifies for a contaminant a
specific treatment technique(s) known
to the Administrator which leads to a
reduction in the level of such contami-
nant sufficient to comply with the re-
quirements of part 141 of this chapter.
[41 PR 2918, Jan. 20, 1976, as amended at 53
FR 37410, Sept. 26, 1988; 54 FR 52137, Dec, 20,
1989; 59 FR 64344, Dec. 14, 1994; 63 PR 23367,
Apr. 28, 1998]
§ 142.3 Scope.
(a) Except where otherwise provided,
this part applies to each public water
system in each State; except that this
part shall not apply to a public water
system which meets all of the fol-
lowing conditions:
(1) Which consists only of distribu-
tion and storage facilities (and does
not have any collection and treatment
facilities);
(2) Which obtains all of its water
from, but is not owned or operated by,
a public water system to which such
regulations apply;
(3) Which does not sell water to any
person; and
(4) Which is not a carrier which con-
veys passengers in interstate com-
merce.
(b) In order to qualify for primary en-
forcement responsibility, a State's pro-
gram for enforcement of primary
drinking water regulations must apply
to all other public water systems in the
State, except for:
(1) Public water systems on carriers
which convey passengers in interstate
commerce;
(2) Public water systems on Indian
land with respect to which the State
does not have the necessary jurisdic-
tion or its jurisdiction is in question;
or
(c) Section 1451 of the SDWA author-
izes the Administrator to delegate pri-
mary enforcement responsibility for
public water systems to Indian Tribes.
An Indian Tribe must meet the statu-
tory criteria at 42 U.S.C. 300j-ll(b)(l)
before it is eligible to apply for Public
Water System Supervision grants and
primary enforcement responsibility.
All primary enforcement responsibility
requirements of parts 141 and 142 apply
to Indian Tribes except where specifi-
cally noted.
[41 FR 2918, Jan. 20, 1976, as amended at 53
FR 37410, Sept. 26, 1988; 59 FR 64344, Dec. 14,
1994; 67 FR 70858, Nov. 27, 2002]
§ 142.4 State and local authority.
Nothing in this part shall diminish
any authority of a State or political
subdivision to adopt or enforce any law
or regulation respecting drinking
water regulations or public water sys-
tems, but no such law or regulation
564
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Environmental Protection Agency
§142.10
shall relieve any person of any require-
ments otherwise applicable under this
part,
Subpart B—Primary Enforcement
Responsibility
§ 142.10 Requirements for a determina-
tion of primary enforcement re-
sponsibility.
A State has primary enforcement re-
sponsibility for public water systems in
the State during any period for which
the Administrator determines, based
upon a submission made pursuant to
§142.11, and submission under §142.12,
that such. State, pursuant to appro-
priate State legal authority:
(a) Has adopted drinking water regu-
lations which are no less stringent
than the national primary drinking
water regulations (NPDWBs) in effect
under part 141 of this chapter;
(b) Has adopted and is implementing
adequate procedures for the enforce-
ment of such State regulations, such
procedures to include:
(1) Maintenance of an inventory of
.public water systems.
(2) A systematic program for con-
ducting sanitary surveys of public
water systems in the State, with pri-
ority given to sanitary surveys of pub-
lic water systems not in compliance
with State primary drinking water reg-
ulations.
(3)(i) The establishment and mainte-
nance of a State program for the cer-
tification of laboratories conducting
analytical measurements of drinking
water contaminants pursuant to the
requirements of the State primary
drinking water regulations including
the designation by the State of a lab-
oratory officer, or officers, certified by
the Administrator, as the officlal(s) re-
sponsible for the State's certification
program. The requirements of this
paragraph may be waived by the Ad-
ministrator for any State where all an-
alytical measurements required by the
State's primary drinking water regula-
tions are conducted at laboratories op-
erated by the State and certified by the
Agency. Until such time as the Agency
establishes a National quality assur-
ance program for laboratory certifi-
cation the State shall maintain an in-
terim program for the purpose of ap-
proving those laboratories from which
the required analytical measurements
will be acceptable.
(ii) Upon a showing by an Indian
Tribe of an intergovernmental or other
agreement to have all analytical tests
performed by a certified laboratory,
the Administrator may waive this re-
quirement,
(4) Assurance of the availability to
the State of laboratory facilities cer-
tified by the Administrator and capa-
ble of performing analytical measure-
ments of all contaminants specified in
the State primary drinking water regu-
lations. Until such time as the Agency
establishes a National quality assur-
ance program for laboratory certifi-
cation the Administrator will approve
such State laboratories on an interim
basis.
(5) The establishment and mainte-
nance of an activity to assure that the
design and construction of new or sub-
stantially modified public water sys-
tem facilities will be capable of compli-
ance with the State primary drinking
water regulations.
(6) Statutory or regulatory enforce-
ment authority adequate to compel
compliance with the State primary
drinking water regulations in appro-
priate cases, such authority to include:
(i) Authority to apply State primary
drinking water regulations to all pub-
lic water systems in the State covered
by the national primary drinking
water regulations, except for interstate
carrier conveyances and systems on In-
dian land with respect to which the
State does not have the necessary ju-
risdiction or its jurisdiction is in ques-
tion.
(ii) Authority to sue in courts of
competent jurisdiction to enjoin any
threatened or continuing violation of
the State primary drinking water regu-
lations.
(iii) Right of entry and inspection of
public water systems, including the
right to take water samples, whether
or not the State has evidence that the
system is in violation of an applicable
legal requirement.
(iv) Authority to require suppliers of
water to keep appropriate records and
make appropriate reports to the State.
(v) Authority to require public water
systems to give public notice that is no
565
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§142.11
40 CFR Ch, 1 (7-1-04 Edition)
less stringent than the EPA require-
ments in Subpart Q of Part 141 of this
chapter and §142.16(a).
(vi) Authority to assess civil or
criminal penalties for violation of the
State's primary drinking water regula-
tions and public notification require-
ments, including the authority to as-
sess daily penalties or multiple pen-
alties when a violation continues;
(vii) Authority to require community
water systems to provide consumer
confidence reports as required under 40
CFR part 141, subpart 0.
(c) Has established and will maintain
record keeping and reporting of its ac-
tivities under paragraphs (a), (b) and
(d) in compliance with §§142.14 and
142.15;
(d) Variances and exemptions. (1) If it-
permits small system "variances pursu-
ant to Section 1415(e) of the Act, it
must provide procedures no less strin-
gent than the Act and Subpart K of
this part,
(2) If it permits variances (other than
small system variances) or exemptions,
or both, from the requirements of the
State primary drinking water regula-
tions, it shall do so under conditions
and in a manner no less stringent than
the requirements of Sections 1415 and
1416 of the Act. In granting these
variances, the State must adopt the
Administrator's finding's of best avail-
able technology, treatment techniques,
or other means available as specified in
Subpart G of this part. (States with
primary enforcement responsibility
may adopt procedures different from
those set forth in Subparts E and P of
this part, which apply to the issuance
of variances (other than small system
variances) and exemptions by the Ad-
ministrator in States that do not have
primary enforcement responsibility,
provided that the State procedures
meet the requirements of this para-
graph); and
(e) Has adopted and can implement
an adequate plan for the provision of
safe drinking water under emergency
circumstances including, but not lim-
ited to, earthquakes, floods, hurri-
canes, and other natural disasters.
(f)(l) Has adopted authority for as-
sessing administrative penalties unless
the constitution of the State prohibits
the adoption of such authority. For
public water systems serving a popu-
lation of more than 10,000 individuals,
States must have the authority to im-
pose a penalty of at least $1,000 per day
per violation. For public water systems
serving a population of 10,000 or fewer
individuals, States must have penalties
that are adequate to ensure compliance
with the State regulations as deter-
mined by the State.
(2) As long as criteria in paragraph
(f)(l) of this section are met, States
may establish a maximum administra-
tive penalty per violation that may be
assessed on a public water system.
(g) An Indian Tribe shall not be re-
quired to exercise criminal enforce-
ment jurisdiction to meet the require-
ments for primary enforcement respon-
sibility.
[41 FR 2918, Jan. 20, 1976, as amended at 43
FR 5373, Feb. 8, 1978; 52 FR 20675, June 2, 1987:
52 PR 41550, Oct. 28. 1987; 53 FR 37410. Sept.
26, 1988; 54 FR 15188, Apr. 17, 1989; 54 FR 52138,
Dec. 20, 1989; 63 FR 23367, Apr. 28, 1998; 63 FR
43846, Aug. 14. 1998; 63 FR 44535. Aug. 19, 1998;
65 PR 26048, May 4, 2000]
1142.11 Initial determination of pri-
mary enforcement responsibility.
(a) A State may apply to the Admin-
istrator for a determination that the
State has primary enforcement respon-
sibility for public water systems in the
State pursuant to section 1413 of the
Act. The application shall be as concise
as possible and include a side-by-side
comparison of the Federal require-
ments and the corresponding State au-
thorities, including citations to the
specific statutes and administrative
regulations or ordinances and, wher-
ever appropriate, judicial decisions
which demonstrate adequate authority
to meet the requirements of §142.10.
The following information is to be in-
cluded with the State application.
(1) The text of the State's primary
drinking water regulations, with ref-
erences to those State regulations that
vary from comparable regulations set
forth in part 141 of this chapter, and a
demonstration that any different State
regulation is at least as stringent as
the comparable regulation contained in
part 141.
(2) A description, accompanied by ap-
propriate documentation, of the
State's procedures for the enforcement
566
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Environmental Protection Agency
§142.11
of the State primary drinking water
regulations. The submission shall in-
clude:
(i) A brief description of the State's
program to maintain a current inven-
tory of public water systems.
(ii) A brief description of the State's
program for conducting" sanitary sur-
veys, including an explanation of the
priorities given to various classes of
public water systems,
(iii) A brief description of the State's
laboratory approval or certification
program, including the name(s) of the
responsible State laboratory officer(s)
certified by the Administrator.
(iv) Identification of laboratory fa-
cilities, available to the State, cer-
tified or approved by the Adminis-
trator and capable of performing ana-
lytical measurements of all contami-
nants specified in the State's primary
drinking water regulations.
(v) A brief description of the State's
program activity to assure that the de-
sign and construction of new or sub-
stantially modified public water sys-
tem facilities will be capable of compli-
ance with the requirements of the
State primary drinking water regula-
tions.
(vi) Copies of State statutory and
regulatory provisions authorizing the
adoption and enforcement of State pri-
mary drinking water regulations, and a
brief description of State procedures
for administrative or judicial action
with respect to public water systems
not in compliance with such regula-
tions.
(3) A statement that the State will
make such reports and will keep such
records as may be required pursuant to
§§142.14 and 142.15.
(4) If the State permits variances or
exemptions from its primary drinking
water regulations, the text of the
State's statutory and regulatory provi-
sions concerning variances and exemp-
tions.
(5) A brief description of the State's
plan for the provision of safe drinking
water under emergency conditions.
NOTE: In satisfaction of this requirement,
for public water supplies from groundwater
sources, EPA will accept the contingency
plan for providing alternate drinking water
supplies that is part of a State's Wellhead
Protection Program, where such program
has been approved by EPA pursuant to sec-
tion 1428 of the SDWA.
<6)(i) A copy of the State statutory
and regulatory provisions authorizing
the executive branch of the State gov-
ernment to impose an administrative
penalty on all public water systems,
and a brief description of the State's
authority for administrative penalties
that will ensure adequate compliance
of systems serving a population of
10,000 or fewer individuals.
(ii) In instances where the State con-
stitution prohibits the executive
branch of the State government from
assessing any penalty, the State shall
submit a copy of the applicable part of
its constitution and a statement from
its Attorney General confirming this
interpretation.
(7)(i) A statement by the State Attor-
ney General (or the attorney for the
State primacy agency if it has inde-
pendent legal counsel) or the attorney
representing the Indian tribe that cer-
tifies that the laws and regulations
adopted by the State or tribal ordi-
nances to carry out the program were
duly adopted and are enforceable. State
statutes and regulations cited by the
State Attorney General and tribal ordi-
nances cited by the attorney rep-
resenting the Indian tribe shall be in
the form of lawfully adopted State
statutes and regulations or tribal ordi-
nances at the time the certification is
made and shall be fully effective by the
time the program is approved by EPA,
To qualify as "independent legal coun-
sel," the attorney signing the state-
ment required by this section shall
have full authority to independently
represent the State primacy agency or
Indian tribe in court on all matters
pertaining to the State or tribal pro-
gram.
(ii) After EPA has received the docu-
ments required under paragraph (a) of
this section, EPA may selectively re-
quire supplemental statements by the
State Attorney General (or the attor-
ney for the State primacy agency if it
has independent legal counsel) or the
attorney representing- the Indian tribe.
Each supplemental statement shall ad-
dress all issues concerning the ade-
quacy of State authorities to meet the
requirements of §142,10 that have been
567
203-160 D-19
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§142.12
40 CFR Ch, i (7-1-04 Edition)
identified by EPA after thorough ex-
amination as unresolved by the docu-
ments submitted under paragraph (a)
of this section.
(b)(l) The administrator shall act on
an application submitted pursuant to
§142.11 within 90 days after receiving
such application, and shall promptly
inform the State in writing of this ac-
tion. If he denies the application, his
written notification to the State shall
include a statement of reasons for the
denial.
(2) A final determination by the Ad-
ministrator that a State has met or
has not met the requirements for pri-
mary enforcement responsibility shall
take effect in accordance with the pub-
lic notice requirements and related
procedures under §142.13.
(3) When the Administrator's deter-
mination becomes effective pursuant
to §142.13, it shall continue in effect
unless terminated pursuant to §142.17.
.[41 FB 2918, Jan, 20, 1976, as amended at 54
FE 52138, Dec. 20, 1989: 60 FB 33661, June 28,
1995; 63 FB 23367, Apr. 28, 1998]
§ 142,12 Revision of State programs.
(a) General requirements. Either EPA
or the primacy State may initiate ac-
tions that require the State to revise
its approved State primacy program.
To retain primary enforcement respon-
sibility, States must adopt all new and
revised national primary drinking
water regulations promulgated in part
141 of this chapter and any other re-
quirements specified in this part,
(1) Whenever a State revises its ap-
proved primacy program to adopt new
or revised Federal regulations, the
State must submit a request to the Ad-
ministrator for approval of the pro-
gram revision, using the procedures de-
scribed in paragraphs (b), (c), and (d) of
this section. The Administrator shall
approve or disapprove each State re-
quest for approval of a program revi-
sion based on the requirements of the
Safe Drinking Water Act and of this
part.
(2) For all State program revisions
not covered under §142.12(a)(l), the re-
view procedures outlined in §142.17(a)
shall apply.
(b) Timing of State requests for ap-
proval of program revisions to adopt new
or revised Federal regulations. (1) Com-
plete and final State requests for ap-
proval of program revisions to adopt
new or revised EPA regulations must
be submitted to the Administrator not
later than 2 years after promulgation
of the new or revised EPA regulations,
unless the State requests an extension
and the Administrator has approved
the request pursuant to paragraph
(b)(2) of this section. If the State ex-
pects to submit a final State request
for approval of a program revision to
EPA more than 2 years after promulga-
tion of the new or revised EPA regula-
tions, the State shall request an exten-
sion of the deadline before the expira-
tion of the 2-year period.
(2) The final date for submission of a
complete and final State request for a
program revision may be extended by
EPA for up to a two-year period upon a
written application by the State to the
Administrator. In the extension appli-
cation the State must demonstrate it
is requesting the extension because it
cannot meet the original deadline for
reasons beyond its control despite a
good faith effort to do so. The applica-
tion must include a schedule for the
submission of a final request by a cer-
tain time and provide sufficient infor-
mation to demonstrate that the State:
(i)(A) Currently lacks the legislative
or regulatory authority to enforce the
new or revised requirements, or
(B) Currently lacks the program ca-
pability adequate to implement the
new or revised requirements; or
(C) Is requesting the extension to
group two or more program revisions
in a single legislative or regulatory ac-
tion; and
(ii) Is implementing the EPA require-
ments to be adopted by the State in its
program revision pursuant to para-
graph (b)(3) of this section within the
scope of its current authority and ca-
pabilities.
(3) To be granted an extension, the
State must agree with EPA to meet
certain requirements during the exten-
sion period, which may include the fol-
lowing types of activities as deter-
mined appropriate by the Adminis-
trator on a case-by-case basis:
568
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Environmental Protection Agency
§142.12
(i) Informing public water systems of
the new EPA (and upcoming State) re-
quirements and that EPA will be over-
seeing implementation of the require-
ments until the State, if eligible for in-
terim primacy, submits a complete and
final primacy revision request to EPA,
or in all other cases, until EPA ap-
proves the State program revision;
(ii) Collecting, storing and managing
laboratory results, public notices, and
other compliance and operation data
required by the EPA regulations;
(iii) Assisting EPA in the develop-
ment of the technical aspects of en-
forcement actions and conducting in-
formal follow-up on violations (tele-
phone calls, letters, etc.):
(iv) Providing technical assistance to
public water systems;
(v) Providing EPA with all informa-
tion prescribed by §142.15 of this part
on State reporting; and
(vi) For States whose request for an
extension is based on a current lack of
program capability adequate to imple-
ment the new requirements, taking
steps agreed to by EPA and the State
during the extension period to remedy
the deficiency.
(c) Contents of a State request for ap-
proval of a program revision. (1) The
State request for EPA approval of a
program revision shall be concise and
must include:
(11 The documentation necessary
(pursuant to §142.1i(a)) to update the
approved State primacy program, and
identification of those elements of the
approved State primacy program that
have not changed because of the pro-
gram revision. The documentation
shall include a side-by-side comparison
of the Federal requirements and the
corresponding State authorities, in-
cluding citations to the specific stat-
utes and administrative regulations or
ordinances and, wherever appropriate,
judicial decisions which demonstrate
adequate authority to meet the re-
quirements of §142.10 as they apply to
the program revision.
(ii) Any additional materials that are
listed in §142.16 of this part for a spe-
cific EPA regulation, as appropriate:
and
(iii) For a complete and final State
request only, unless one of the condi-
tions listed in paragraph (c}(2) of this
section are met, a statement by the
State Attorney General (or the attor-
ney for the State primacy agency if it
has independent legal counsel) or the
attorney representing the Indian tribe
that certifies that the laws and regula-
tions adopted by the State or tribal or-
dinances to carry out the program revi-
sion were duly adopted and are enforce-
able. State statutes and regulations
cited by the State Attorney General
and tribal ordinances cited by the at-
torney for the Indian tribe shall be in
the form of lawfully adopted State
statutes and regulations or tribal ordi-
nances at the time the certification is
made and shall be fully effective by the
time the request for program revision
is approved by EPA, To qualify as
"independent legal counsel," the attor-
ney signing the statement required by
this section shall have full authority to
independently represent the State pri-
macy agency or tribe in court on all
matters pertaining to the State or trib-
al program.
(2) An Attorney General's statement
will be required as part of the State re-
quest for EPA approval of a program
revision unless EPA specifically waives
this requirement for a specific regula-
tion at the time EPA promulgates the
regulation, or by later written notice
from the Administrator to the State.
(3) After EPA has received the docu-
ments required under paragraph (c)(l)
of this section, EPA may selectively
require supplemental statements by
the State Attorney General (or the at-
torney for the State primacy agency if
it has independent legal counsel) or the
attorney representing- the Indian tribe.
Each supplemental statement shall ad-
dress all issues concerning the ade-
quacy of State authorities to meet the
requirements of §142.10 that have been
identified by EPA after thorough ex-
amination as unresolved by the docu-
ments submitted under paragraph (c)(l)
of this section.
(d) Procedures for review of a State re-
quest for approval of a program revision—
(1) Preliminary request, (i) The State
may submit to the Administrator for
his or her review a preliminary request
for approval of each program revision,
containing the information listed in
paragraph (c)(l) of this section, in draft
form. The preliminary request does not
569
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§142.13
40 CFR Ch. I (7-1-04 Edition)
require an Attorney General's state-
ment in draft form, but does require
draft State statutory or regulatory
changes and a side-by-side comparison
of State authorities with EPA require-
ments to demonstrate that the State
program revision meets EPA require-
ments under §142.10 of this part. The
preliminary request should be sub-
mitted to the Administrator as soon as
practicable after the promulgation of
the EPA regulations.
(ii) The Administrator will review
the preliminary request submitted in
accordance with paragraph (d)(l)(i) of
this section and make a tentative de-
termination on the request. The Ad-
ministrator will send the tentative de-
termination and other comments or
suggestions to the State for its use in
developing the State's final request
under paragraph (d)(2) of this section.
(2) Final request. The State must sub-
mit a complete and final request for
approval of a program revision to the
Administrator for his or her review and
approval. The request must contain the
information listed in paragraph (c)(l)
of this section in complete and final
form, in accordance with any tentative
determination EPA may have issued.
Complete and final State requests for
program revisions shall be submitted
within two years of the promulgation
of the new or revised EPA regulations,
as specified in paragraph (b) of this sec-
tion.
(3) EPA's determination on a complete
and final request, (i) The Administrator
shall act on a State's request for ap-
proval of a program revision within 90
days after determining that the State
request is complete and final and shall
promptly notify the State of his/her de-
termination.
(ii) If the Administrator disapproves
a final request for approval of a pro-
gram revision, the Administrator will
notify the State in writing. Such noti-
fication will include a statement of the
reasons for disapproval.
(iii) A final determination by the Ad-
ministrator on a State's request for ap-
proval of a program revision shall take
effect in accordance with the public no-
tice requirements and related proce-
dures under §142.13.
(e) Interim primary enforcement author-
ity. A State with an approved primacy
program for each existing national pri-
mary drinking water regulation shall
be considered to have interim primary
enforcement authority with respect to
each new or revised national drinking
water regulation that it adopts begin-
ning when the new or revised State
regulation becomes effective or when
the complete primacy revision applica-
tion is submitted to the Administrator,
whichever is later, and shall end when
the Administrator approves or dis-
approves the State's revised primacy
program.
[54 FB 52138, Dec. 20, 1989, as amended at 63
FR 23367, Apr. 28, 1998; 66 FB 3780, Jan. 16,
2001]
§142.13 Public hearing.
(a) The Administrator shall provide
an opportunity for a public hearing be-
fore a final determination pursuant to
§ 142.11 that the State meets or does not
meet the requirements for obtaining
primary enforcement responsibility, or
a final determination pursuant to
§142.12(d)(3) to approve or disapprove a
State request for approval of a program
revision, or a final determination pur-
suant to §142.17 that a State no longer
meets the requirements for primary en-
forcement responsibility.
(b) The Administrator shall publish
notice of any determination specified
in paragraph (a) of this section in the
FEDERAL REGISTER and in a newspaper
or newspapers of general circulation in
the State involved within 15 days after
making such determination, with a
statement of his reasons for the deter-
mination. Such notice shall inform in-
terested persons that they may request
a public hearing on the Administra-
tor's determination. Such notice shall
also indicate one or more locations in
the State where information submitted
by the State pursuant to §142.11 is
available for inspection by the general
public. A public hearing may be re-
quested by any interested person other
than a Federal agency. Frivolous or in-
substantial requests for hearing may
be denied by the Administrator.
(c) Bequests for hearing submitted
pursuant to paragraph (b) of this sec-
tion shall be submitted to the Adminis-
trator within 30 days after publication
of notice of opportunity for hearing in
the FEDERAL REGISTER. Such requests
570
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Environmental Protection Agency
§142.14
shall include the following informa-
tion:
(1) The name, address and telephone
number of the individual, organization
or other entity requesting a hearing.
(2) A brief statement of the request-
ing person's interest in the Adminis-
trator's determination and of informa-
tion that the requesting person intends
to submit at such hearing'.
(3) The signature of the individual
making the request; or, if the request
is made on behalf of an organization or
other entity, the signature of a respon-
sible official of the organization or
other entity.
(d) The Administrator shall give no-
tice in the FEDERAL REGISTER and in a
newspaper or newspapers of general cir-
culation in the State involved of any
hearing to be held pursuant to a re-
quest submitted by an interested per-
son or on his own motion. Notice of the
hearing shall also be sent to the person
requesting a hearing, if any, and to the
State involved. Notice of the hearing
shall include a statement of the pur-
pose of the hearing, information re-
garding the time and location or loca-
tions for the hearing and the address
and telephone number of an office at
which interested persons may obtain
further information concerning the
hearing. At least one hearing location
specified in the public notice shall be
within the involved State. Notice of
hearing- shall be given not less than 15
days prior to the time scheduled for
the hearing.
(e) Hearings convened pursuant to
paragraph (d) of this section shall be
conducted before a hearing officer to be
designated by the Administrator. The
hearing shall be conducted by the hear-
ing officer in an informal, orderly and
expeditious manner. The hearing offi-
cer shall have authority to call wit-
nesses, receive oral and written testi-
mony and take such other action as
may be necessary to assure the fair and
efficient conduct of the hearing. Fol-
lowing the conclusion of the hearing,
the hearing officer shall forward the
record of the hearing to the Adminis-
trator.
(f) After reviewing the record of the
hearing, the Administrator shall issue
an order affirming the determination
referred to in paragraph (a) of this sec-
tion or rescinding such determination.
If the determination is affirmed, it
shall become effective as of the date of
the Administrator's order.
(g) If no timely request for hearing is
received and the Administrator does
not determine to hold a hearing on his
own motion, the Administrator's deter-
mination shall become effective 30 days
after notice is issued pursuant to para-
graph (b) of this section.
(h) If a determination of the Admin-
istrator that a State no longer meets
the requirements for primary enforce-
ment responsibility becomes effective,
the State may subsequently apply for a
determination that it meets such re-
quirements by submitting to the Ad-
ministrator information demonstrating
that it has remedied the deficiencies
found by the Administrator without
adversely sacrificing other aspects of
its program required for primary en-
forcement responsibility.
[41 PR 2918. Jan. 20. 1976. as amended at 54
FR 52140, Dec. 20, 1989; 60 FR 33661, June 28,
1995]
§ 142.14 Records kept by States.
(a) Each State which has primary en-
forcement responsibility shall main-
tain records of tests, measurements,
analyses, decisions, and determinations
performed on each public water system
to determine compliance with applica-
ble provisions of State primary drink-
ing water regulations,
(1) Records of microbiological anal-
yses shall be retained for not less than
1 year. Actual laboratory reports may
be kept or data may be transferred to
tabular summaries, provided that the
information retained includes:
(1) The analytical method used;
(ii) The number of samples analyzed
each month;
(iii) The analytical results, set forth
in a form which makes possible com-
parison with the limits specified in
§§141,63, 141.71, and 141,72 of this chap-
ter.
(2) Records of microbiological anal-
yses of repeat or special samples shall
be retained for not less than one year
in the form of actual laboratory re-
ports or in an appropriate summary
form.
(3) Records of turbidity measure-
ments must be kept for not less than
571
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§142.14
40 CFR Ch. 1 (7-1-04 Edition)
one year. The Information retained
must be set forth in a form which
makes possible comparison with the
limits specified in §§141.71, 141.73,
141.173 and 141.175, 141,550-141.553 and
141.560-141.564 of this chapter. Until
June 29, 1993, for any public water sys-
tem which is providing filtration treat-
ment and until December 30, 1991, for
any public water system not providing
filtration treatment and not required
by the State to provide filtration treat-
ment, records kept must be set forth in
a form which makes possible compari-
son with the limits contained in §141.13
of this chapter.
(4)(i) Records of disinfectant residual
measurements and other parameters
necessary to document disinfection ef-
fectiveness in accordance with §§141.72
and 141.74 of this chapter and the re-
porting requirements of §§141.75,
141.175, and 141.570, of this chapter must
be kept for not less than one year.
(ii) Records of decisions made on a
system-by-system and case-by-case
basis under provisions of part 141, sub-
part H, subpart P, or subpart T of this
chapter, must be made in writing and
kept by the State.
(A) Records of decisions made under
the following provisions shall be kept
for 40 years (or until one year after the
decision is reversed or revised) and a
copy of the decision must be provided
to the system:
(7) Section 141.73(a)(l)—Any decision
to allow a public water system using
conventional filtration treatment or
direct filtration to substitute a tur-
bidity limit greater than 0.5 NTU;
(2) Section 141.73(b)(l)—Any decision
to allow a public water system using
slow sand filtration to substitute a tur-
bidity limit greater than 1 NTU;
(3) Section 141.74(b)(2)—Any decision
to allow an unfiltered public water sys-
tem to use continuous turbidity moni-
toring;
(4) Section 141.74(b)(6)(i)—Any deci-
sion to allow an unfiltered public water
system to sample residual disinfectant
concentration at alternate locations if
it also has ground water source(s);
(5) Section 141.74(c)(l)—Any decision
to allow a public water system using
filtration treatment to use continuous
turbidity monitoring; or a public water
system using- slow sand filtration or fil-
tration treatment other than conven-
tional treatment, direct filtration or
diatomaceous earth filtration to re-
duce turbidity sampling to once per
day; or for systems serving 500 people
or fewer to reduce turbidity sampling
to once per day;
(6) Section 141.74(e)(3)(i)—Any deci-
sion to allow a filtered public water
system to sample disinfectant residual
concentration at alternate locations if
it also has ground water source(s);
(7) Section 141.75(a)(2)(ix)—Any deci-
sion to allow reduced reporting by an
unfiltered public water system;
(8) Section 141.75(b)(2)(iv>—Any deci-
sion to allow reduced reporting by a fil-
tered public water system; and
(9) Section 141.76—Any decisions
made to approve alternate recycle lo-
cations, require modifications to recy-
cle return locations, or require modi-
fications to recycle practices.
(B) Records of decisions made under
the following provisions shall be kept
for one year after the decision is made:
(7) Section 141.71(b)(l)(i)—Any deci-
sion that a violation of monthly CT
compliance requirements was caused
by circumstances that were unusual
and unpredictable.
(2) Section 141.71(b)(l)(iv)—Any deci-
sion that a violation of the disinfection
effectiveness criteria was not caused by
a deficiency in treatment of the source
water;
(3) Section 141.71(b)(5)—Any decision
that a violation of the total coliform
MCL was not caused by a deficiency in
treatment of the source water;
(4) Section 141.74(b)(l)—Any decision
that total coliform monitoring other-
wise required because the turbidity of
the source water exceeds 1 NTU is not
feasible, except that if such decision al-
lows a system to avoid monitoring
without receiving State approval in
each instance, records of the decision
shall be kept until one year after the
decision is rescinded or revised.
(0) Records of decisions made under
the following provisions shall be kept
for the specified period or 40 years,
whichever is less.
(7) Section 141.71(a)(2)(i)—Any deci-
sion that an event in which the source
water turbidity which exceeded 5 NTU
for an unfiltered public water system
572
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Environmental Protection Agency
§142,14
was unusual and unpredictable shall be
kept for 10 years.
(2) Section 141.71(b)(l)(iii)—Any deci-
sion by the State that failure to meet
the disinfectant residual concentration
requirements of §141.72(a)(3)(i) was
caused by circumstances that were un-
usual and unpredictable, shall be kept
unless filtration is Installed. A copy of
the decision must be provided to the
system.
(3) Section 141.71(b)(2>—Any decision
that a public water system's watershed
control program meets the require-
ments of this section shall be kept
until the next decision is available and
filed.
(4) Section 141.70(c)—Any decision
that an individual is a qualified oper-
ator for a public water system using a
surface water source or a ground water
source under the direct influence of
surface water shall be maintained until
the qualification is withdrawn. The
State may keep this information in the
form of a list which is updated periodi-
cally. If such qualified operators are
classified by category, the decision
shall include that classification.
(5) Section 141.71(b)(3)—Any decision
that a party other than the State is ap-
proved by the State to conduct on-site
inspections shall be maintained until
withdrawn. The State may keep this
information in the form of a list which
is updated periodically.
(6) Section 141.71(b)(4)—Any decision
that an unfiltered public water system
has been identified as the source of a
waterborne disease outbreak, and, if
applicable, that it has been modified
sufficiently to prevent another such oc-
currence shall be kept until filtration
treatment is installed. A copy of the
decision must be provided to the sys-
tem.
(7) Section 141.72—Any decision that
certain interim disinfection require-
ments are necessary for an unfiltered
public water system for which the
State has determined that filtration is
necessary, and a list of those require-
ments, shall be kept until filtration
treatment is installed. A copy of the
requirements must be provided to the
system.
(
-------
§142.14
40 CFR Ch. I (7-1-04 Idltion)
kept until the decision is reversed or
revised. A copy of the list of required
values must be provided to the system.
(13) Section 141.74(b)(3)(v)—Any deci-
sion that a system using a disinfectant
other than chlorine may use OT99.9 val-
ues other than those in tables 2,1 or 3,1
and/or other operational parameters to
determine if the minimum total inac-
tivation rates required by §141.72(a)(l)
are being met, and what those values
or parameters are, shall be kept until
the decision is reversed or revised. A
copy of the list of required values or
parameters must be provided to the
system.
(14) Section 142.16(b)(2)(i)(B)—Any de-
cision that a system using a ground
water source is under the direct influ-
ence of surface water.
(iii) Records of any determination
that a public water system supplied by
a surface water source or a ground
water source under the direct influence
of surface water is not required to pro-
vide filtration treatment shall be kept
for 40 years or until withdrawn, which-
ever is earlier, A copy of the deter-
mination must be provided to the sys-
tem.
(5) Records of each of the following
decisions made pursuant to the total
coliform provisions of part 141 shall be
made in writing and retained by the
State.
(1) Records of the following decisions
must be retained for 5 years.
(A) Section 141.21(b)(l)—Any decision
to waive the 24-hour time limit for col-
lecting repeat samples after a total
coliform-positive routine sample if the
public water system has a logistical
problem in collecting the repeat sam-
ple that is beyond the system's control,
and what alternative time limit the
system must meet.
(B) Section 141.21(b)(5)—Any decision
to allow a system to waive the require-
ment for five routine samples the
month following a total coliform-posi-
tive sample. If the waiver decision is
made as provided in §141.21(b)(5), the
record of the decision must contain all
the items listed in that paragraph.
(C) Section 141.21(c>—Any decision to
invalidate a total coliform-positive
sample. If the decision to invalidate a
total coliform-positive sample as pro-
vided in §141.21(c)(l)(iii) is made, the
record of the decision must contain all
the items listed in that paragraph.
(ii) Records of each of the following
decisions must be retained in such a
manner so that each system's current
status may be determined.
(A) Section 141.21(a)(2)—Any decision
to reduce the total coliform moni-
toring frequency for a community
water system serving 1,000 persons or
fewer, that has no history of total coli-
form contamination in its current con-
figuration and had a sanitary survey
conducted within the past five years
showing that the system is supplied
solely by a protected groundwater
source and is free of sanitary defects,
to less than once per month, as pro-
vided in §141.21(a)(2); and what the re-
duced monitoring frequency is. A copy
of the reduced monitoring frequency
must be provided to the system.
(B) Section 141.21(a)(3)(i)—Any deci-
sion to reduce the total coliform moni-
toring frequency for a non-community
water system using only ground water
and serving 1,000 persons or fewer to
less than once per quarter, as provided
in §141.21(a)(3)(i), and what the reduced
monitoring frequency is. A copy of the
reduced monitoring frequency must be
provided to the system.
(C) Section 141.21(a)(3)(ii)—Any deci-
sion to reduce the total coliform moni-
toring frequency for a non-community
water system using only ground water
and serving more than 1,000 persons
during any month the system serves
1,000 persons or fewer, as provided in
§ 141.21(a)(3)(ii). A copy of the reduced
monitoring frequency must be provided
to the system.
(D) Section 141.21(a)(5)—Any decision
to waive the 24-hour limit for taking a
total coliform sample for a public
water system which uses surface water,
or ground water under the direct influ-
ence of surface water, and which does
not practice filtration in accordance
with part 141, subpart H, and which
measures a source water turbidity level
exceeding 1 NTU near the first service
connection as provided in §141.21(a)(5).
(B) Section 141.21(d)(l>—Any decision
that a non-community water system is
using only protected and disinfected
ground water and therefore may reduce
the frequency of its sanitary survey to
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Environmental Protection Agency
§142,14
less than once every five years, as pro-
vided in §141,21(d). and what that fre-
quency is. A copy of the reduced fre-
quency must be provided to the sys-
tem.
(F) Section 141.21(d)(2)—A list of
agents other than the State, if any, ap-
proved by the State to conduct sani-
tary surveys.
(G) Section 141.21(e)(2)—Any decision
to allow a public water system to forgo
fecal coliform or E. coli testing on a
total coliform-posltive sample if that
system assumes that the total coli-
form-positive sample is fecal coliform-
positive or E. coli- positive, as provided
in §141.21(e)(2).
(6) Records of analysis for other than
microbiological contaminants (includ-
ing total coliform, fecal coliform, and
heterotrophic plate count), residual
disinfectant concentration, other pa-
rameters necessary to determine dis-
infection effectiveness (including tem-
perature and pH measurements), and
turbidity shall be retained for not less
than 12 years and shall include at least
the following information:
(i) Date and place of sampling.
(ii) Date and results of analyses.
(7) Any decisions made pursuant to
the provisions of part 141, subpart P or
subpart T of this chapter.
(i) Records of systems consulting
with the State concerning a modifica-
tion to disinfection practice under
§§141.170(d), 141.172(c), and 141.542 of
this chapter, including the status of
the consultation.
(ii) Records of decisions that a sys-
tem using alternative filtration tech-
nologies, as allowed under §§141.1730))
and §141.552 of this chapter, can con-
sistently achieve a 99.9 percent re-
moval and/or inactivation of Giardia
lamblia cysts, 99.99 percent removal
and/or inactivation of viruses, and 99
percent removal of Cryptosporidium
oocysts. The decisions must include
State-set enforceable turbidity limits
for each system. A copy of the decision
must be kept until the decision is re-
versed or revised. The State must pro-
vide a copy of the decision to the sys-
tem.
(iii) Records of systems required to
do filter self-assessment, OPE. or COP
under the requirements of §§141.175 and
141.563 of this chapter.
(b) Records required to be kept pur-
suant to paragraph (a) of this section
must be in a form admissible as evi-
dence in State enforcement pro-
ceedings.
(c) Each State which has primary en-
forcement responsibility shall main-
tain current inventory information for
every public water system in the State
and shall retain inventory records of
public water systems for not less than
12 years.
(d) Each State which has primary en-
forcement responsibility shall retain,
for not less than 12 years, files which
shall include for each such public water
system in the State:
(1) Reports of sanitary surveys;
(2) Records of any State approvals:
(3) Records of any enforcement ac-
tions,
(4) A record of the most recent vul-
nerability determination, including the
monitoring results and other data sup-
porting the determination, the State's
findings based on the supporting data
and any additional bases for such de-
termination; except that it shall be
kept in perpetuity or until a more cur-
rent vulnerability determination has
been issued.
(5) A record of all current monitoring
requirements and the most recent mon-
itoring frequency decision pertaining
to each contaminant, including the
monitoring results and other data sup-
porting the decision, the State's find-
ings based on the supporting data and
any additional bases for such decision:
except that the record shall be kept in
perpetuity or until a more recent mon-
itoring frequency decision has been
issued,
(6) A record of the most recent asbes-
tos repeat monitoring determination,
including the monitoring results and
other data supporting the determina-
tion, the State's findings based on the
supporting data and any additional
bases for the determination and the re-
peat monitoring frequency; except that
these records shall be maintained in
perpetuity or until a more current re-
peat monitoring determination has
been issued.
(7) Records of annual certifications
received from systems pursuant to part
141, subpart K demonstrating the sys-
tem's compliance with the treatment
575
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§142.14
40 CFR Ch. I (7-1-04 Edition)
techniques for aerylamide and/or
epichlorohydrin in §14.111.
(8) Records of the currently applica-
ble or most recent State determina-
tions, including all supporting informa-
tion and an explanation of the tech-
nical "basis for each decision, made
under the following provisions of 40
OPB, part 141, subpart I for the control
of lead and copper:
(i) Section 141.8Kb)—for any water
system deemed to be optimized under
§141.81(b)(l) or (b)(3) of this chapter,
any conditions imposed by the State on
specific water systems to ensure the
continued operation and maintenance
of corrosion control treatment in
place;
(ii) Section 141.82(b)—decisions to re-
quire a water system to conduct corro-
sion control treatment studies;
(iii) Section 141.82(d>—designations of
optimal corrosion control treatment;
(iv) Section 141.82(f)—designations of
optimal water quality parameters;
(v) Section 141.82(h)—decisions to
modify a public water system's optimal
corrosion control treatment or water
quality parameters;
(vi) Section 141.83(b)(2)—determina-
tions of source water treatment;
(vii) Section 141.83(b)(4)—designa-
tions of maximum permissible con-
centrations of lead and copper in
source water:
(viii) Section 141.84(e)—determina-
tions establishing shorter lead service
line service line replacement schedules
under §141.84;
(ix) Sections 141.81(b)(3)(iii).
141.86(d)(4)(vii), and 141.86(g)(4)(iii)—de-
terminations of additional monitoring
requirements and/or other actions re-
quired to maintain optimal corrosion
control by systems monitoring for lead
and copper at the tap less frequently
than once every six months that
change treatment or add a new source
of water;
(x) Section 141.85—system-specific de-
cisions regarding the content of writ-
ten public education materials and/or
the distribution of these materials;
(xi) Section 141.86(b)(5)—-system-spe-
cific determinations regarding use of
non-first-draw samples at non-tran-
sient non-community water systems,
and community water systems meeting
the criteria of §§141.85(c)(7)(i) and (ii) of
this chapter, that operate 24 hours a
day;
(xii) Section 141.86(c)—system-spe-
cific designations of sampling locations
for systems subject to reduced moni-
toring;
(xiii) Section 141.86(d)(iv)(A)—sys-
tem-specific determinations pertaining
to alternative sample collection peri-
ods for systems subject to reduced
monitoring;
(xiv) Section 141,86(g)—determina-
tions of small system monitoring waiv-
ers, waiver recertifications, and waiver
revocations;
(xv) Section 141.87(c)(3)—determina-
tions regarding representative entry
point locations at ground water sys-
tems;
(xvi) Section 141.90(e)(4)—system-spe-
cific determinations regarding the sub-
mission of information to demonstrate
compliance with partial lead service
line replacement requirements; and
(xvii) Section 141.90(f)—system-spe-
cific decisions regarding the resubmis-
sion of detailed documentation dem-
onstrating completion of public edu-
cation requirements.
(9) Records of reports and any other
information submitted by PWSs under
§141.90 of this chapter, including
records of any 90th percentile values
calculated by the State under § 141.90(h)
of this chapter.
(10) Records of State activities, and
the results thereof, to:
(i) Verify compliance with State de-
terminations issued under §§141.82(f) of
this chapter, 141.82(h) of this chapter,
141.83(b)(2) of this chapter, and
141.83(b)(4) of this chapter;
(ii) Verify compliance with the re-
quirements related to partial lead serv-
ice line replacement under §141.84(d) of
this chapter and compliance with lead
service line replacement schedules
under § 141.84(e) of this chapter: and
(iii) Invalidate tap water lead and
copper samples under §141,86(f) of this
chapter.
(11) Records of each system's cur-
rently applicable or most recently des-
ignated monitoring requirements. If,
for the records identified in paragraphs
(d)(8)(i) through (d)(8)(xvii) of this sec-
tion, no change is made to State deter-
minations during a 12-year retention
period, the State shall retain the
576
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Environmental Protection Agency
§142.15
record until a new decision, determina-
tion, or designation has been issued.
(12) Records of the currently applica-
ble or most recent State determina-
tions, including all supporting informa-
tion and an explanation of the tech-
nical basis for each decision, made
under the following provisions of 40
CPB part 141, subpart L for the control
of disinfectants and disinfection by-
products. These records must also in-
clude interim measures toward instal-
lation.
(i) States must keep records of sys-
tems that are installing GAC or mem-
brane technology in accordance with
§141.64(b)(2) of this chapter. These
records must include the date by which
the system is required to have com-
pleted installation.
(ii) States must keep records of sys-
tems that are required, by the State, to
meet alternative minimum TOO re-
moval requirements or for whom the
State has determined that the source
water is not amenable to enhanced co-
agulation in accordance with
§141.135(b){3) and (4) of this chapter, re-
spectively. These records must include
the alternative limits and rationale for
establishing the alternative limits.
(iii) States must keep records of sub-
part H systems using conventional
treatment meeting any of the alter-
native compliance criteria in
§141.135{a)(2) or (3) of this chapter.
(iv) States must keep a register of
qualified operators that have met the
State requirements developed under
§142.16(f)(2),
(13) Records of systems with multiple
wells considered to be one treatment
plant in accordance with §141.132(a)(2)
of this chapter and §142.16(f)(5).
(14) Monitoring plans for subpart H
systems serving more than 3,300 per-
sons in accordance with §141.132(f) of
this chapter.
(15) List of laboratories approved for
analyses in accordance with §141.131(b)
of this chapter.
(16) List of systems required to mon-
itor for disinfectants and disinfection
byproducts in accordance with part 141,
subpart L of this chapter. The list
must indicate what disinfectants and
DBFs, other than chlorine, TTHM, and
HAA5. if any, are measured.
(e) Each State which has primary en-
forcement responsibility shall retain
records pertaining to each variance and
exemption granted by it for a period of
not less than 5 years following the ex-
piration of such variance or exemption.
(f) Public notification records under
Subpart Q of Part 141 of this chapter
received from public water systems (in-
cluding certifications of compliance
and copies of public notices) and any
state determinations establishing al-
ternative public notification require-
ments for the water systems must be
retained for three years,
(g) Records required to be kept under
this section shall be available to the
Regional Administrator upon request.
The records required to be kept under
this section shall be maintained and
made available for public inspection by
the State, or, the State at its option
may require suppliers of water to make
available for public inspection those
records maintained in accordance with
§141.33.
[41 FR 2918, Jan. 20, 1976, as amended at 54
PR 27537, June 29. 1989; 55 FE 25065, June 19.
1990; 56 FR 3595, Jan. 30. 1991; 56 FR 26562.
June 7, 1991; 63 FR 69475, 69519. Deo. 16, 1998:
65 FR 2014, Jan. 12, 2000; 65 FR 26048, May 4.
2000; 66 FR 31105. June 8, 2001: 67 FR 1843, Jan.
14, 2002]
EFFECTIVE DATE NOTE; At 69 FR 38857, June
29, 2004, §142.14 was amended in paragraph
(d)(12)(iv) by removing the citation
"|142.16(f)(2)" and adding in its place
"§142.16(hX2)". and in paragraph (d)(13) by re-
moving the citation "§142.16(f)(5)" and adding
in its place "§142.16(h)(5)", effective July 29,
2004.
§ 142.15 Reports by States,
Each State which has primary en-
forcement responsibility shall submit
to the Administrator the following in-
formation:
(a) Bach State which has primary en-
forcement responsibility shall submit
quarterly reports to the Administrator
on a schedule and in a format pre-
scribed by the Administrator, con-
sisting of the following information:
(1) New violations by public water
systems in the State during the pre-
vious quarter of State regulations
adopted to incorporate the require-
ments of national primary drinking
water regulations, including violations
of the public notification requirements
577
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§142.15
40 CFR Ch. I (7-1-04 Idftion)
under Subpart Q of Part 141 of this
chapter;
(2) New enforcement actions taken by
the State during the previous quarter
against public water systems with re-
spect to State regulations adopted to
incorporate the requirements of na-
tional primary drinking water regula-
tions;
(3) Notification of any new variance
or exemption granted during the pre-
vious quarter. The notice shall include
a statement of reasons for the granting
of the variance or exemption, including
documentation of the need for the vari-
ance or exemption and the finding that
the granting of the variance or exemp-
tion will not result in an unreasonable
risk to health. The State may use a
single notification statement to report
two or more similar variances or ex-
emptions.
(b) Bach State which has primary en-
forcement responsibility shall submit
annual reports to the Administrator on
a schedule and in a format prescribed
by the Administrator, consisting of the
following information:
(1) All additions or corrections to the
State's inventory of public water sys-
tems;
(2) A summary of the status of each
variance and exemption currently in
effect.
(c) Special reports. (1) Surface Water
Treatment Rule. (i)(A) A list identifying
the name, PWS identification number
and date of the determination for each
public water system supplied by a sur-
face water source or a ground water
source under the direct influence of
surface water, which the State has de-
termined is not required to provide fil-
tration treatment.
(B) A list identifying the name and
PWS identification number of each
public water system supplied by a sur-
face water source or ground water
source under the direct influence of
surface water, which the State has de-
termined, based on an evaluation of
site-specific considerations, has no
means of having a sample transported
and analyzed for HPC by a certified
laboratory under the requisite time
and temperature conditions specified
in § 141.74(a)(3) and is providing ade-
quate disinfection in the distribution
system, regardless of whether the sys-
tem is in compliance with the criteria
of §141.72 (a)(4)(i) or (b)(3)(i) of this
chapter, as allowed by §141.72 (a)(4)(ii)
and (b)(3)(ii). The list must include the
effective date of each determination.
(ii) Notification within 60 days of the
end of the calendar quarter of any de-
termination that a public water system
using a surface water source or a
ground water source under the direct
influence of surface water is not re-
quired to provide filtration treatment.
The notification must include a state-
ment describing the system's compli-
ance with each requirement of the
State's regulations that implement
§141.71 and a summary of comments, if
any, received from the public on the
determination. A single notification
may be used to report two or more
such determinations.
(2) Total coliforms. A list of public
water systems which the State is al-
lowing to monitor less frequently than
once per month for community water
systems or less frequently than once
per quarter for non-community water
systems as provided in §141.21(a), in-
cluding the effective date of the re-
duced monitoring requirement for each
system.
(3) [Reserved]
(4) States shall report quarterly, in a
format and on a schedule prescribed by
the Administrator, the following infor-
mation related to each system's com-
pliance with the treatment techniques
for lead and copper under 40 CPR part
141, subpart I during the preceding cal-
endar quarter. Specifically, States
shall report as follows:
(i) For any reports provided prior to
May 15, 2000, States shall report the
name and PWS identification number:
(A) Each public water system which
exceeded the lead and copper action
levels and the date upon which the ex-
ceedance occurred;
(B) Bach public water system re-
quired to complete the corrosion con-
trol evaluation specified in §141.82(c)
and the date the State received the re-
sults of the evaluations from each sys-
tem;
(C) Bach public water system for
which the State has designated optimal
corrosion control treatment under
§141.82(d), the date of the determina-
tion, and each system that completed
578
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Environmental Protection Agency
§142.15
installation of treatment as certified
under §141.90(e)(3);
(D) Bach public water system for
which the State has designated optimal
water quality parameters under
§141.82(f) and the date of the deter-
mination;
(E) Each public water system which
the State has required to install source
water treatment under §141.83(b)(2), the
date of the determination, and each
system that completed installation of
treatment as certified under
§141.90(d)(2);
(P) Each public water system for
which the State has specified max-
imum permissible source water levels
under §141.83(b)(4>; and
(G) Each public water system re-
quired to begin replacing lead service
lines as specified in §141.84, each public
water system for which the State has
established a replacement schedule
under §141.84(f), and each system re-
porting compliance with its replace-
ment schedule under §141,90(e)(2).
(ii) For any reports provided after
May 14, 2000 and before January 14,
2002, States may report in accordance
with either paragraph (c)(4)(i) or
(c)(4)(iii) of this section,
(ill) For all reports submitted on or
after January 14, 2002, States shall re-
port the PWS identification number of
each public water system identified in
paragraphs (c)(4)(iii)(A) through (F) of
this section.
(A) For each large and medium-size
public water system, all 90th percentile
lead levels calculated during each mon-
itoring period specified in §141.86 of
this chapter, and the first and last day
of the monitoring period for which the
90th percentile lead level was cal-
culated;
(B) For each small public water sys-
tem, the 90th percentile lead level cal-
culated during each monitoring period
in which the system exceeds the lead
action level, and the first and last day
of each monitoring period in which an
exceedance occurred;
(C) For each public water system (re-
gardless of size), the 90th percentile
copper level calculated during each
monitoring period in which the system
exceeds the copper action level, and
the first and last day of each moni-
toring period in which an exceedance
occurred;
(D) For each public water system for
which the State has designated optimal
water quality parameters under
§141.82(f) of this chapter, or which the
State has deemed to have optimized
corrosion control under §141.81(b)(l) or
(b)(3) of this chapter, the date of the
determination and the paragraph(s)
under which the State made its deter-
mination;
(E) For each public water system re-
quired to begin replacing lead service
lines as specified in §141.84 of this chap-
ter and the date each system must
begin replacement; and
(F) For each public water system
that has implemented optimal corro-
sion control, completed applicable
source water treatment requirements
pursuant to §141.83 of this chapter and'
or completed lead service line replace-
ment requirements pursuant to §141.84
of this chapter, and the date of the
State's determination that these re-
quirements have been met. The date re-
ported shall be the latest of the fol-
lowing events:
(1) The date the State designates op-
timal water quality parameters under
§141.82(f) of this chapter or deems the
system to have optimized corrosion
control pursuant to §141.81(b)(l) or
(b)(3) of this chapter;
(2) For systems triggered into source
water treatment, the date the State
designates maximum permissible
source water levels under §141.83(b)(4)
of this chapter or determines pursuant
to §141.83(b)(2) of this chapter that
source water treatment is not required;
or
(3) For systems triggered into lead
service line replacement, the date the
system completes lead service line re-
placement or becomes eligible to cease
lead service line replacement pursuant
to § 141.84(f) of this chapter.
(5) Sanitary surveys, A list of subpart
H systems that have had a sanitary
survey completed during the previous
year and an annual evaluation of the
State's program for conducting sani-
tary surveys under §142.16(b)(3) of this
chapter.
(d) The reports submitted pursuant
to this section shall be made available
579
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§142.16
40 CFR Ch. I (7-1-04 Edition)
by the State to the public for inspec-
tion at one or more locations within
the State.
[41 FR 2918, Jan. 20, 1976, as amended at 43
FR 5373, Feb. 8, 1978; 54 FR 27539, June 29,
1989; 55 FR 52140, Deo. 20, 1989; 55 FE 25065,
June 19, 1990; 56 PR 3595, Jan. 30, 1991; 56 PR
26562, June 7, 1991; 63 FR 69520, Deo. 16, 1998;
64 PR 50620, Sept. 17, 1999; 65 FR 2014, Jan. 12,
2000; 65 FR 20313, Apr. 14, 2000; 65 FR 26048,
May 4, 2000; 66 FR 3780, Jan. 16, 2001]
§ 142.16 Special primacy requirements.
(a) State public notification require-
ments.
(1) Each State that has primary en-
forcement authority under this part
must submit complete and final re-
quests for approval of program revi-
sions to adopt the requirements of Sub-
part Q of Part 141 of this chapter, using
the procedures in § 142.12(b) through (d).
At its option, a State may, by rule, and
after notice and comment, establish al-
ternative public notification require-
ments with respect to the form and
content of the public notice required
under Subpart Q of Part 141 of this
chapter. The alternative requirements
must provide the same type and
amount of information required under
Subpart Q and must meet the primacy
requirements under § 142.10,
(2) As part of the revised primacy
program, a State must also establish
enforceable requirements and proce-
dures when the State adds to or
changes the requirements under:
(i) Table 1 to 40 CFR 141.201 (a)(Item
(3)(v))—To require public water sys-
tems to give a public notice for viola-
tions or situations other than those
listed in Appendix A of Subpart Q of
Part 141 of this chapter;
(ii) 40 CFR 141.201(c)(2)—To allow pub-
lic water systems, under the specific
circumstances listed in §141.201(c)(2), to
limit the distribution of the public no-
tice to persons served by the portion of
the distribution system that is out of
compliance;
(iii) Table 1 of 40 CFR 141.202(a) (Items
(5), (6), and (8))—To require public
water systems to give a Tier 1 public
notice (rather than a Tier 2 or Tier 3
notice) for violations or situations list-
ed in Appendix A of Subpart Q of Part
141 of this chapter;
(iv) 40 CFR 141.202(b)(3)~To require
public water systems to comply with
additional Tier 1 public notification re-
quirements set by the State subsequent
to the initial 24-hour Tier 1 notice, as
a result of their consultation with the
State required under |§141.202(b)(2);
(v) 40 CFR 141.202(0), 141.203(c) and
141.204(c)—To require a different form
and manner of delivery for Tier 1, 2 and
3 public notices.
(vi) Table 1 to 40 CFR 141.203(a) (Item
(2))—To require the public water sys-
tems to provide a Tier 2 public notice
(rather than Tier (3)) for monitoring or
testing procedure violations specified
by the State;
(vii) 40 CFR 141.203(b)(l)—To grant
public water systems an extension up
to three months for distributing the
Tier 2 public notice in appropriate cir-
cumstances (other than those specifi-
cally excluded in the rule);
(viii) 40 CFR 141.203(b)(2)—To grant a
different repeat notice frequency for
the Tier 2 public notice in appropriate
circumstances (other than those spe-
cifically excluded in the rule), but no
less frequently than once per year;
(ix) 40 CFR 141.203(b)(3)~To respond
within 24 hours to a request for con-
sultation by the public water system to
determine whether a Tier 1 (rather
than a Tier 2) notice is required for a
turbidity MCL violation under
§141.13(b) or a SWTR/IESWTR TT vio-
lation due to a single exceedance of the
maximum allowable turbidity limit;
(x) 40 CFR 141,205(c)—To determine
the specific multilingual requirement
for a public water system, including de-
fining "large proportion of non-English-
speaking consumers."
(b) Requirements for States to adopt 40
CFR part 141, subpart H Filtration and
Disinfection. In addition to the general
primacy requirements enumerated
elsewhere in this part, including the re-
quirement that State provisions are no
less stringent than the federal require-
ments, an application for approval of a
State program revision that adopts 40
CPR part 141, subpart H Filtration and
Disinfection, must contain the infor-
mation specified in this paragraph (b),
except that States which require with-
out exception all public water systems
using a surface water source or a
ground water source under the direct
580
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Environmental Protection Agency
§142.16
influence of surface water to provide
filtration need not demonstrate that
the State program has provisions that
apply to systems which do not provide
filtration treatment. However, such
States must provide the text of the
State statutes or regulations which
specifies that all public water systems
using a surface water source or a
ground water source under the direct
influence of surface water must provide
filtration.
(1) Enforceable requirements, (i) In ad-
dition to adopting criteria no less
stringent than those specified in part
141, subpart H of this chapter, the
State's application must include en-
forceable design and operating criteria
for each filtration treatment tech-
nology allowed or a procedure for es-
tablishing design and operating condi-
tions on a system-by-system basis (e.g.,
a permit system).
(ii) States must have the appropriate
rules or other authority to assure that
PWSs respond in writing to significant
deficiencies outlined in sanitary survey
reports required under paragraph (b)(3)
of this section no later than 45 days
after receipt of the report, indicating
how and on what schedule the system
will address significant deficiencies
noted in the survey.
(iii) States must have the appro-
priate rules or other authority to as-
sure that PWSs take necessary steps to
address significant deficiencies identi-
fied in sanitary survey reports required
under paragraph (b)(3) of this section,
if such deficiencies are within the con-
trol of the PWS and its governing body,
(2) State practices or procedures, (i) A
State application for program revision
approval must include a description of
how the State will accomplish the fol-
lowing:
(A) Section 141.70(c) (qualification of
operators)—Qualify operators of sys-
tems using a surface water source or a
ground water source under the direct
influence of surface water,
(B) Determine which systems using a
ground water source are under the di-
rect influence of surface water by June
29, 1994 for community water systems
and by June 39, 1999 for non-community
water systems.
(C) Section 141.72(b)(l) (achieving re-
quired Giardia lamblia and virus re-
moval in filtered systems)—Determine
that the combined treatment process
incorporating disinfection treatment
and filtration treatment will achieve
the required removal and/or inactiva-
tion of Giardia lamblia and viruses,
(D) Section 141.74(a) (State approval
of parties to conduct analyses)—ap-
prove parties to conduct pH, tempera-
ture, turbidity, and residual disinfect-
ant concentration measurements.
(B) Determine appropriate filtration
treatment technology for source wa-
ters of various qualities.
(ii) For a State which does not re-
quire all public water systems using a
surface water source or ground water
source under the direct influence of
surface water to provide filtration
treatment, a State application for pro-
gram revision approval must include a
description of how the State will ac-
complish the following:
(A) Section 141.71(b)(2) (watershed
control program)—Judge the adequacy
of watershed control programs.
(B) Section 141.71(b)(3) (approval of
on-site inspectors)—Approve on-site in-
spectors other than State personnel
and evaluate the results of on-site in-
spections.
(iii) For a State which adopts any of
the following discretionary elements of
part 141 of this chapter, the application
must describe how the State will:
(A) Section 141.72 (interim disinfec-
tion requirements)—Determine interim
disinfection requirements for unfil-
tered systems which the State has de-
termined must filter which will be in
effect until filtration is installed.
(B) Section 141.72 (a)(4)(ii) and
(b)(3)(ii) (determination of adequate
disinfection in system without dis-
infectant residual)—Determine that a
system is unable to measure HPC but
is still providing adequate disinfection
in the distribution system, as allowed
by §141.72(a)(4)(ii) for systems which do
not provide filtration treatment and
§141.72(b)(3)(ii) for systems which do
provide filtration treatment.
(C) Section 141.73 (a)(l) and (b)(l) (al-
ternative turbidity limit)—Determine
whether an alternative turbidity limit
is appropriate and what the level
should be as allowed by §141.73(a)(l) for
a system using conventional filtration
treatment or direct filtration and by
581
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§142.16
40 CFR Ch. I (7-1-04 Edition)
§141.73(b)(l) for a system using slow
sand filtration,
(D) Section 141.73(d) (alternative fil-
tration technologies)—Determine that
a public water system has dem-
onstrated that an alternate filtration
technology, in combination with dis-
infection treatment, achieves adequate
removal and/or disinfection of Giardla
lamblia and viruses,
(E) Section 141.74(a)(5) (alternate an-
alytical method for chlorine)—Approve
DPD colorimetric test kits for free and
combined chlorine measurement or ap-
prove calibration of automated meth-
ods by the Indigo Method for ozone de-
termination.
(P) Section 141.74 (b)(2) and (c)(l) (ap-
proval of continuous turbidity moni-
toring)—Approve continuous turbidity
monitoring, as allowed by §141.74(b)(2)
for a public water system which does
not provide filtration treatment and
§141.74(c)(l) for a system which does
provide filtration treatment.
(G) Section 141.74 (b)(6)(i) and (c)(3)(i)
(approval of alternate disinfectant re-
sidual concentration sampling plans)—
Approve alternate disinfectant residual
concentration sampling plans for sys-
tems which have a combined ground
water and surface water or ground
water and ground water under the di-
rect influence of a surface water dis-
tribution system, as allowed by
§141.74(b)(6)(i) for a public water sys-
tem which does not provide filtration
treatment and §141.74(c)(3)(i) for a pub-
lic water system which does provide
filtration treatment.
(H) Section 141.74(c)(l) (reduction of
turbidity monitoring)—Decide whether
to allow reduction of turbidity moni-
toring for systems using slow sand fil-
tration, an approved alternate filtra-
tion technology or serving 500 people or
fewer.
(I) Section 141.75 (a)(2)(ix) and
(b)(2)(iv) (reduced reporting)—Deter-
mine whether reduced reporting is ap-
propriate, as allowed by §141.75(a)(2)(ix)
for a public water system which does
not provide filtration treatment and
§141.75(b)(2)(iv) for a public water sys-
tem which does provide filtration
treatment.
(iv) For a State which does not re-
quire all public water systems using a
surface water source or ground water
source under the direct influence of
surface water to provide filtration
treatment and which uses any of the
following discretionary provisions, the
application must describe how the
State will:
(A) Section 141.71(a)(2)(i) (source
water turbidity requirements)—Deter-
mine that an exceedance of turbidity
limits in source water was caused by
circumstances that were unusual and
unpredictable.
(B) Section 141.71(b)(l)(i) (monthly
CT compliance requirements)—Deter-
mine whether failure to meet the re-
quirements for monthly CT compliance
in §141.72(a)(l) was caused by cir-
cumstances that were unusual and un-
predictable.
(O) Section 141.71(b)(l)(iii) (residual
disinfectant concentration require-
ments)—Determine whether failure to
meet the requirements for residual dis-
infectant concentration entering the
distribution system in §141.72(a)(3)(i)
was caused by circumstances that were
unusual and unpredictable,
(D) Section 141.71(b)(l)(iv) (distribu-
tion system disinfectant residual con-
centration requirements)—Determine
whether failure to meet the require-
ments for distribution system residual
disinfectant concentration in
§141.72(a)(4) was related to a deficiency
in treatment.
(B) Section 141.71(b)(4) (system modi-
fication to prevent waterborne disease
outbreak)—Determine that a system,
after having been identified as the
source of a waterborne disease out-
break, has been modified sufficiently
to prevent another such occurrence.
(P) Section 141.71(b)(5) (total coliform
MOL)—Determine whether a total coli-
form MOL violation was caused by a
deficiency in treatment.
(G) Section 141.72(a)(l) (disinfection
requirements)—Determine that dif-
ferent ozone, chloramine, or chlorine
dioxide CT99.9 values or conditions are
adequate to achieve required disinfec-
tion.
(H) Section 141.72(a)(2)(ii) (shut-off of
water to distribution system)—Deter-
mine whether a shut-off of water to the
distribution system when the disinfect-
ant residual concentration entering the
distribution system is less than 0.2 mg/
582
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Environmental Protection Agency
§142.16
1 will cause an unreasonable risk to
health or interfere with fire protection.
(I) Section 141,74(b)(l) (coliform mon-
itoring)—Determine that coliform
monitoring which otherwise might be
required is not feasible for a system.
(J) Section 141.74(b), table 3.1 (dis-
infection with chloramines)—Deter-
mine the conditions to be met to insure
99.99 percent removal and/or inactiva-
tion of viruses in systems which use ei-
ther preformed chloramines or
chloramines for which ammonia is
added to the water before chlorine, as
allowed by table 3.1.
(3) Sanitary survey. In addition to the
general requirements for sanitary sur-
veys contained in §142.10(b)(2), an ap-
plication must describe how the State
will implement a sanitary survey pro-
gram that meets the requirements in
paragraphs (b)(3)(i) through (v) of this
section. For the purposes of this para-
graph, "sanitary survey" means an on-
site review of the water source (identi-
fying sources of contamination using
results of source water assessments
where available), facilities, equipment,
operation, maintenance, and moni-
toring compliance of a public water
system to evaluate the adequacy of the
system, its sources and operations and
the distribution of safe drinking water.
(i) The State must conduct sanitary
surveys for all surface water systems
(including groundwater under the in-
fluence) that address the eight sanitary
survey components listed in para-
graphs (b)(3)(i)(A) through (H) of this
section no less frequently than every
three years for community systems
and no less frequently than every five
years for noncommunity systems. The
State may allow sanitary surveys con-
ducted after December 1995 to serve as
the first set of required sanitary sur-
veys if the surveys address the eight
sanitary survey components listed in
paragraphs (b)(3)(i)(A) through (H) of
this section.
(A) Source.
(B) Treatment.
(0) Distribution system.
(D) Finished water storage.
(E) Pumps, pump facilities, and con-
trols.
(F) Monitoring and reporting and
data verification.
(Q) System management and oper-
ation.
(H) Operator compliance with State
requirements.
(ii) For community systems deter-
mined by the State to have out-
standing performance based on prior
sanitary surveys, subsequent sanitary
surveys may be conducted no less than
every five years. In its primacy appli-
cation, the State must describe how it
will decide whether a system has out-
standing performance and is thus eligi-
ble for sanitary surveys at a reduced
frequency.
(ill) Components of a sanitary survey
may be completed as part of a staged
or phased state review process within
the established frequency.
(iv) When conducting sanitary sur-
veys for systems required to comply
with the disinfection profiling require-
ments in §141.172 of this chapter, the
State must also review the disinfection
profile as part of the sanitary survey.
(v) In its primacy application, the
State must describe how it will decide
whether a deficiency identified during
a sanitary survey is significant for the
purposes of paragraph (b)(l)(ii) of this
section.
(c) Total coliform requirements. In addi-
tion to meeting the general primacy
requirements of this part, an applica-
tion for approval of a State program
revision that adopts the requirements
of the national primary drinking water
regulation for total coliforms must
contain the following information:
(1) The application must describe the
State's plan for determining whether
sample siting plans are acceptable (in-
cluding periodic reviews), as required
by§141.21(a)(l).
(2) The national primary drinking
water regulation for total coliforms in
part 141 gives States the option to
impose leaser requirements in certain
circumstances, which are listed below.
If a State chooses to exercise any of
these options, its application for appro-
val of a program revision must include
the information listed below (the State
need only provide the information list-
ed for those options it has chosen to
use).
(i) Section 141.21(a)(2) (Reduced moni-
toring requirements for community
water systems serving 1,000 or fewer
583
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§142.16
40 CFR Ch. i (7-1-04 Edition)
persons)—A description of how the
State will determine whether it is ap-
propriate to reduce the total coliform
monitoring frequency for such systems
using the criteria in §141.21(a)(2) and
how it will determine the revised fre-
quency.
(it) Section 141.21(a)(3)(i) (Reduced
monitoring requirements for non-com-
munity water systems using ground
water and serving 1,000 persons or
fewer)—A description of how the State
will determine whether it is appro-
priate to reduce the total coliform
monitoring frequency for such systems
using the criteria in §141.21(a)(3)(i) and
how it will determine the revised fre-
quency.
(iii) Section 141.21(a)(3)(ii) (Reduced
monitoring for non-cornmunity water
systems using ground water and serv-
ing more than 1,000 persons)—A de-
scription of how the State will deter-
mine whether it is appropriate to re-
duce the total coliform monitoring fre-
quency for non-community water sys-
tems using only ground water and serv-
ing more than 1,000 persons during any
month the system serves 1,000 persons
or fewer and how it will determine the
revised frequency.
(iv) Section 141.21(a)(5) (Waiver of
time limit for sampling after a tur-
bidity sampling result exceeds 1
NTU)—A description of how the State
will determine whether it is appro-
priate to waive the 24-hour time limit.
(v) Section 141.21(b)(l) (Waiver of
time limit for repeat samples)—A de-
scription of how the State will deter-
mine whether it is appropriate to waive
the 24-hour time limit and how it will
determine what the revised time limit
will be.
(vi) Section 141.21(b)(3) (Alternative
repeat monitoring requirements for
systems with a single service connec-
tion)—A description of how the State
will determine whether it is appro-
priate to allow a system with a single
service connection to use an alter-
native repeat monitoring scheme, as
provided in §141.21(b)(3), and what the
alternative requirements will be.
(vii) Section 141.21(b)(5) (Waiver of re-
quirement to take five routine samples
the month after a system has a total
coliform-positive sample)—A descrip-
tion of how the State will determine
whether it is appropriate to waive the
requirement for certain systems to col-
lect five routine samples during the
next month it serves water to the pub-
lic, using the criteria in §141.21(b)(5).
(viii) Section 141.21(c) (Invalidation
of total coliform-positive samples)—A
description of how the State will deter-
mine whether it is appropriate to in-
validate a total coliform-positive sam-
ple, using the criteria in §141.21(0),
(ix) Section 141.21(d) (Sanitary sur-
veys)—A description of the State's cri-
teria and procedures for approving
agents other than State personnel to
conduct sanitary surveys.
(x) Section 141.21(e)(2) (Waiver of
fecal coliform or E. coll testing on a
total coliform-positive sample)—A de-
scription of how the State will deter-
mine whether it is appropriate to waive
fecal coliform or E. coli testing on a
total coliform-positive sample.
(d) Requirements for States to adopt
40 CPR part 141, subpart I—Control of
Lead and Copper. An application for
approval of a State program revision
which adopts the requirements speci-
fied in 40 CPR part 141, subpart 1, must
contain (in addition to the general pri-
macy requirements enumerated else-
where in this part, including the re-
quirement that State regulations be at
least as stringent as the federal re-
quirements) a description of how the
State will accomplish the following
program requirements:
(1) Section 141.82—State designation
of optimal corrosion control.
(i) Sections 141.82(d), 141.82(f), and
141.82(h)—Designating optimal corro-
sion control treatment methods, opti-
mal water quality parameters, and
modifications thereto.
(ii) Section 141.82(g)—Designating an
alternative approach for aggregating
multiple measurements collected dur-
ing the same day for a water quality
parameter at a sampling location, if
the State elects to adopt a formula
other than the one specified in
§141.82(g)(l) of this chapter,
(2) Sections 141.83(b)(2) and
141.83(b)(4)—Designating source water
treatment methods, maximum permis-
sible source water levels for lead and
copper and modifications thereto.
584
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Environmental Protection Agency
§142,16
(3) Section 141.90(e)—Verifying- com-
pliance with lead service line replace-
ment schedules and completion of all
partial lead service line replacement
activities.
(4) Section 141.86(d)(4)(iv)(A)—Desig-
nating an alternative period for sample
collection for community water sys-
tems subject to reduced monitoring.
(e) An application for approval of a
State program revision which adopts
the requirements specified in §§141.11.
141.23, 141.24, 141.32, 141.40, 141.61 and
141.62 for a newly regulated contami-
nant must contain the following (in ad-
dition to the general primacy require-
ments enumerated elsewhere in this
part, including the requirement that
State regulations be at least as strin-
gent as the federal requirements):
(1) If a State chooses to issue waivers
from the monitoring requirements in
§§141.23 and 141.24, the State shall de-
scribe the procedures and criteria
which it will use to review waiver ap-
plications and issue waiver determina-
tions.
(i) The procedures for each contami-
nant or class of contaminants shall in-
clude a description of:
(A) The waiver application require-
ments;
(B) The State review process for "use"
waivers and for "susceptibility" waiv-
ers; and
(C) The State decision criteria, in-
cluding the factors that will be consid-
ered in deciding to grant or deny waiv-
ers. The decision criteria must include
the factors specified in §§141.24(f)(8)
and 141.24(h)(6).
(ii) The State must specify the moni-
toring data and other documentation
required to demonstrate that the con-
taminant is eligible for a "use" and/or
"susceptibility" waiver.
(2) A monitoring- plan for the initial
monitoring period by which the State
will assure all systems complete the
required initial monitoring within the
regulatory deadlines.
NOTE: States may update their monitoring
plan submitted under the Phase II Rule or
simply note in their application that they
will use the same monitoring plan for the
Phase V Rule,
(i) The initial monitoring plan must
describe how systems will be scheduled
during the initial monitoring period
and demonstrate that the analytical
workload on certified laboratories for
each of the three years has been taken
into account, to assure that the State's
plan will result in a high degree of
monitoring compliance and that as a
result there is a high probability of
compliance and will be updated as nec-
essary.
(ii) The State must demonstrate that
the initial monitoring plan is enforce-
able under State law.
(f) Consumer Confidence Report require-
ments. (1) Bach State that has primary
enforcement responsibility must adopt
the requirements of 40 OFR part 141,
subpart O no later than August 21, 2000.
States must submit revised programs
to EPA for approval using the proce-
dures in §142.12(b) through (d).
(2) Bach State that has primary en-
forcement responsibility must make
reports submitted to the States in
compliance with 40 CFR 141.155(c)
available to the public upon request.
(3) Each State that has primary en-
forcement responsibility must main-
tain a copy of the reports for a period
of one year and the certifications ob-
tained pursuant to 40 OPR 141.155(c) for
a period of 5 years.
(4) Bach State that has primary en-
forcement responsibility must report
violations of this subpart in accordance
with the requirements of §142.15(a)(l).
(g) Requirements for States to adopt 40
CFR part 141, Subpart P—Enhanced Fil-
tration and Disinfection—Systems Serving
10,000 or More People, In addition to the
general primacy requirements enumer-
ated elsewhere in this part, including
the requirement that State provisions
are no less stringent than the Federal
requirements, an application for ap-
proval of a State program revision that
adopts 40 CFR part 141, Subpart P En-
hanced Filtration and Disinfection—
Systems Serving 10,000 or More People,
must contain the information specified
in this paragraph:
(1) Enforceable requirements. States
must have the appropriate rules or
other authority to require PWSs to
conduct a Composite Correction Pro-
gram (COP) and to assure that PWSs
implement any followup recommenda-
tions that result as part of the COP.
The OOP consists of two elements—a
585
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§142.16
40 CFR Ch, 1 (7-1-04 Edition)
Comprehensive Performance Evalua-
tion (CPE) and Comprehensive Tech-
nical Assistance (CTA). A CPE is a
thorough review and analysis of a
plant's performance-based capabilities
and associated administrative, oper-
ation and maintenance practices. It is
conducted to identify factors that may
be adversely impacting a plant's capa-
bility to achieve compliance and em-
phasizes approaches that can be imple-
mented without significant capital im-
provements. A CTA is the performance
improvement phase that is imple-
mented if the CPE results indicate im-
proved performance potential. During
the CTA phase, the system must iden-
tify and systematically address plant-
specific factors. The CTA is a combina-
tion of utilizing CPE results as a basis
for followup, implementing process
control priority-setting techniques and
maintaining1 long-term involvement to
systematically train staff and adminis-
trators.
(2) State practices or procedures, (i)
Section 141.172(a)(3) of this chapter-
How the State will approve a more rep-
resentative annual data set than the
data set determined under §141.172
(a)(l) or (2) of this chapter for the pur-
pose of determining applicability of the
requirements of §141-172 of this chap-
ter.
(ii) Section 141.172(b)(5) of this chap-
ter—How the State will approve a
method to calculate the logs of inac-
tivation for viruses for a system that
uses either chloramines or ozone for
primary disinfection.
(iii) Section 141.172(c) of this chap-
ter—How the State will consult with
PWSs to evaluate modifications to dis-
infection practice.
(iv) Section 141.173(b) of this chap-
ter—For filtration technologies other
than conventional filtration treat-
ment, direct filtration, slow sand fil-
tration, or diatomaceous earth filtra-
tion, how the State will determine that
a public water system may use a filtra-
tion technology If the PWS dem-
onstrates to the State, using pilot
plant studies or other means, that the
alternative filtration technology, in
combination with disinfection treat-
ment that meets the requirements of
§141.172(b) of this chapter, consistently
achieves 99.9 percent removal and/or in-
activation of Giardia lamblia cysts and
99.99 percent removal and/or inactiva-
tion of viruses, and 99 percent removal
of Crypto&poridium oocysts. For a sys-
tem that makes this demonstration,
how the State will set turbidity per-
formance requirements that the sys-
tem must meet 95 percent of the time
and that the system may not exceed at
any time at a level that consistently
achieves 99,9 percent removal and/or in-
activation of Giardia lamblia cysts, 99.99
percent removal and/or inactivation of
viruses, and 99 percent removal of
Cryptosporidium oocysts.
(h) Requirements for States to adopt 40
CFR part 141, subpart L. In addition to
the general primacy requirements else-
where in this part, including the re-
quirement that State regulations be at
least as stringent as federal require-
ments, an application for approval of a
State program revision that adopts 40
CPR part 141, subpart L, must contain
a description of how the State will ac-
complish the following program re-
quirements:
(1) Section 141.64(b)(2) of this chapter
(interim treatment requirements). De-
termine any interim treatment re-
quirements for those systems electing
to install GAG or membrane filtration
and granted additional time to comply
with §141.64 of this chapter.
(2) Section 141.130(c) of this chapter
(qualification of operators). Qualify op-
erators of public water systems subject
to 40 CPR part 141, subpart L. Quali-
fication requirements established for
operators of systems subject to 40 CPR
part 141, subpart H—Filtration and Dis-
infection may be used in whole or in
part to establish operator qualification
requirements for meeting 40 CFR part
141, subpart L requirements if the
State determines that the 40 CFR part
141, subpart H requirements are appro-
priate and applicable for meeting sub-
part L requirements.
(3) Section 141.131(c)(2) of this chap-
ter (DPD colorimetric test kits). Ap-
prove DPD colorimetric test kits for
free and total chlorine measurements.
State approval granted under
§141.74(a)(2) of this chapter for the use
of DPD colorimetric test kits for free
chlorine testing is acceptable for the
use of DPD test kits in measuring free
586
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Environmental Protection Agency
§142.16
chlorine residuals as required in 40
CFR part 141, subpart L,
(4) Sections 141.131(c)(3) and (d) of
this chapter (State approval of parties
to conduct analyses). Approve parties
to conduct pH, bromide, alkalinity, and
residual disinfectant concentration
measurements. The State's process for
approving parties performing water
quality measurements for systems sub-
ject to 40 CFR part 141, subpart H re-
quirements in paragraph (b)(2)(i)(D) of
this section may be used for approving
parties measuring water quality pa-
rameters for systems subject to sub-
part L requirements, if the State deter-
mines the process is appropriate and
applicable.
(5) Section 141.132(a)(2) of this chap-
ter (multiple wells as a single source).
Define the criteria to use to determine
if multiple wells are being drawn from
a single aquifer and therefore be con-
sidered a single source for compliance
with monitoring requirements.
(6) Approve alternate minimum TOG
removal (Step 2) requirements, as al-
lowed under the provisions of
§ 141.135(b) of this chapter.
(i) Requirements for States to adopt 40
CFR part 141, §141.76 Recycle provisions,
In addition to the general primacy re-
quirements enumerated elsewhere in
this part, including the requirement
that the State provisions are no less
stringent than the federal require-
ments, an application for approval of a
State program revision that adopts 40
CFE part 141, §141.76 Recycle Provi-
sions must contain the information
specified in this paragraph:
(1) State practices or procedures, (i)
Section 141.76(d) of this chapter-
States must have the proper rules and
authority to use Sanitary Surveys,
comprehensive performance evalua-
tions (CPEs), other inspections, or
other activities to evaluate recycle
data maintained by systems under
§141.76(d) of this chapter and require
modifications to recycle practices.
(ii) [Reserved]
(2) [Reserved]
(j) Requirements for States to adopt 40
CFR part 141, Subpart T—-Enhanced Fil-
tration and Disinfection—Systems Serving
Fewer than 10,000 People. In addition to
the general primacy requirements enu-
merated elsewhere in this part, includ-
ing the requirement that State provi-
sions are no less stringent than the
Federal requirements, an application
for approval of a State program revi-
sion that adopts 40 CFR part 141, Sub-
part T Enhanced Filtration and Dis-
infection—Systems Serving Fewer than
10,000 People, must contain the infor-
mation specified in this paragraph:
(1) Enforceable requirements. States
must have rules or other authority to
require systems to participate in a
Comprehensive Technical Assistance
(CTA) activity, the performance im-
provement phase of the Composite Cor-
rection Program (CCP). The State
must determine whether a CTA must
be conducted based on results of a CPE
which indicate the potential for im-
proved performance, and a finding by
the State that the system is able to re-
ceive and implement technical assist-
ance provided through the CTA. A CPE
is a thorough review and analysis of a
system's performance-based capabili-
ties and associated administrative, op-
eration and maintenance practices. It
is conducted to identify factors that
may be adversely impacting a plant's
capability to achieve compliance. Dur-
ing the CTA phase, the system must
identify and systematically address
factors limiting performance. The CTA
is a combination of utilizing CPE re-
sults as a basis for follow-up, imple-
menting process control priority-set-
ting techniques and maintaining long-
term involvement to systematically
train staff and administrators.
(2) State practices or procedures, (i)
Section 141.530-141.536—How the State
will approve a more representative
data set for optional TTHM and HAA5
monitoring and profiling.
(ii) Section 141.536 of this chapter-
How the State will approve a method
to calculate the logs of inactivation for
viruses for a system that uses either
chloramines, ozone, or chlorine dioxide
for primary disinfection.
(iii) Section 141.542 of this chapter-
How the State will consult with the
system and approve significant changes
to disinfection practices.
(iv) Section 141,552 of this chapter—
For filtration technologies other than
conventional filtration treatment, di-
rect filtration, slow sand filtration, or
diatomaceous earth filtration, how the
587
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§142,16
40 CFR Ch, I (7-1-04 Edition)
State will determine that a public
water system may use a filtration
technology if the PWS demonstrates to
the State, using pilot plant studies or
other means, that the alternative fil-
tration technology, in combination
with disinfection treatment that meets
the requirements of §141.72(b) of this
chapter, consistently achieves 99.9 per-
cent removal and/or inactivation of
Giardia lamblia cysts and 99.99 percent
removal and/or inactivation of viruses,
and 99 percent removal of
Cryptosporidium oocysts. For a system
that makes this demonstration, how
the State will set turbidity perform-
ance requirements that the system
must meet 95 percent of the time and
that the system may not exceed at any
time at a level that consistently
achieves 99.9 percent removal and/or in-
activation of Giardia lamblia cysts, 99.99
percent removal and/or inactivation of
viruses, and 99 percent removal of
Cryptosporidium oocysts.
EDITORIAL NOTE: At 6? FR 1844, Jan. 14,
2002. the above paragraph (j) was added, ef-
fective Feb. 13. 2002. However, at 66 PR 7066,
Jan. 22, 2001, paragraph (j) had already teen
added, effective Jan. 22, 2004. The paragraph
(j) effective Jan. 22, 2004, follows.
(j) An application for approval of a
State program revision which adopts
the requirements specified in §§141.11,
141.23, 141.24, 141.32, 141.40, 141.61 and
141.62 for an existing regulated con-
taminant must contain the following
(in addition to the general primacy re-
quirements enumerated elsewhere in
this part, including the requirement
that State regulations be at least as
stringent as the federal requirements):
(1) If a State chooses to issue waivers
from the monitoring requirements in
§§141.23, 141.24, and 141.40, the State
shall describe the procedures and cri-
teria which it will use to review waiver
applications and issue wavier deter-
minations. The State shall provide the
same information required in para-
graph (e)(l)(i) and (ii) of this section.
States may update their existing waiv-
er criteria or use the requirements sub-
mitted under the National Primary
Drinking Water Regulations for the in-
organic and organic contaminants (i.e.,
Phase II/V rule) in 16(e) of this section.
States may simply note in their appli-
cation any revisions to existing waiver
criteria or note that the same proce-
dures to issue waivers will be used.
(2) A monitoring plan by which the
State will ensure all systems complete
the required monitoring by the regu-
latory deadlines. States may update
their existing monitoring plan or use
the same monitoring plan submitted
under the National Primary Drinking
Water Regulations for the inorganic
and organic contaminants (i.e. Phase
II/V rule) in 16(e) of this section. States
may simply note in their application
any revisions to an existing monitoring
plan or note that the same monitoring
plan will be used. The State must dem-
onstrate that the monitoring plan is
enforceable under State law.
(k) States establish the initial moni-
toring requirements for new systems
and new sources. States must explain
their initial monitoring schedules and
how these monitoring schedules ensure
that public water systems and sources
comply with MCL's and monitoring re-
quirements. States must also specify
the time frame in which new systems
will demonstrate compliance with the
MCLs.
(1) An application for approval of a
State program revision for radio-
nuclides which adopts the require-
ments specified in §141.26(a)(2)(ii)(C) of
this chapter must contain the fol-
lowing (in addition to the general pri-
macy requirements enumerated in this
part, including that State regulations
be at least as stringent as the Federal
requirements):
(1) If a State chooses to use grand-
fathered data in the manner described
in §141.26(a)(2)(ii)(C) of this chapter,
then the State must describe the proce-
dures and criteria which it will use to
make these determinations (whether
distribution system or entry point
sampling points are used).
(i) The decision criteria that the
State will use to determine that data
collected in the distribution system are
representative of the drinking water
supplied from each entry point to the
distribution system. These determina-
tions must consider:
(A) All previous monitoring data.
(B) The variation in reported activity
levels.
588
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Environmental Protection Agency
§142.17
(C) Other factors affecting the rep-
resentativeness of the data (e.g. geol-
ogy).
(ii) [Reserved]
(2) A monitoring plan by which the
State will assure all systems complete
the required monitoring within the
regulatory deadlines. States may up-
date their existing monitoring plan or
use the same monitoring plan sub-
mitted for the requirements in
§ 142.16(e)(5) under the national primary
drinking water regulations for the in-
organic and organic contaminants (i.e.
the phase II/V rules). States may note
in their application any revision to an
existing monitoring plan or note that
the same monitoring plan will be used.
The State must demonstrate that the
monitoring plan is enforceable under
State law.
[54 FE 15188, Apr, 17, 1989, as amended at 54
FR 27539, June 29, 1989; 55 FR 25065, June 19,
1990; 56 FR 3595, Jan. 30, 1991; 56 FE 26563,
June 7, 1991; 57 FE 31847. July 17, 1992; 59 FR
33864, June 30, 1994: 63 FR 44535, Aug. 19, 1998;
63 FE 69475, 69520, Deo. 18, 1998; 64 FE 34733,
June 29, 1999; 64 FR 50620, Sept. 17,1999; 65 FR
2015, Jan. 12, 2000; 65 FR 26048, 26049, May 4,
2000; 65 FR 76751, Dec. 7, 2000; 66 FE 7066, Jan.
22, 2001; 66 FR 31105, June 8, 2001; 67 FR 1844,
Jan. 14, 2002]
EFFECTIVE DATE NOTE; At 69 FR 38857, June
29, 2004, §142.16 was amended in paragraph
(1X2) by removing the citation "§ 142.16(e)(5)"
and adding in its place "§142,16(e)(2)"; by add-
ing and reserving paragraphs (m), (n), and
(o); by redesignatingr the first paragraph (j)
as paragraph (p); and in newly designated
paragraph (p)(2)(ii) by removing the citation
"141.536" and adding in its place "141.535", ef-
fective July 29, 2004.
§ 142.17 Review of State programs and
procedures for withdrawal of ap-
proved primacy programs.
(a)(l) At least annually the Adminis-
trator shall review, with respect to
each State determined to have primary
enforcement responsibility, the compli-
ance of the State with the require-
ments set forth in 40 CFR part 142, sub-
part B, and the approved State primacy
program. At the time of this review,
the State shall notify the Adminis-
trator of any State-initiated program
changes (i.e., changes other than those
to adopt new or revised EPA regula-
tions), and of any transfer of all or part
of its program from the approved State
agency to any other State agency.
(2) When, on the basis of the Admin-
istrator's review or other available in-
formation, the Administrator deter-
mines that a State no longer meets the
requirements set forth in 40 CFR part
142, subpart B, the Administrator shall
initiate proceedings to withdraw pri-
macy approval. Among the factors the
Administrator intends to consider as
relevant to this determination are the
following, where appropriate: whether
the State has requested and has been
granted, or is awaiting EPA's decision
on, an extension under §142.12(b)(2) of
the deadlines for meeting those re-
quirements; and whether the State is
taking corrective actions that may
have been required by the Adminis-
trator. The Administrator shall notify
the State In writing that EPA is initi-
ating primacy withdrawal proceedings
and shall summarize in the notice the
information available that indicates
that the State no longer meets such re-
quirements.
(3) The State notified pursuant to
paragraph (a)(2) of this section may,
within 30 days of receiving the Admin-
istrator's notice, submit to the Admin-
istrator evidence demonstrating that
the State continues to meet the re-
quirements for primary enforcement
responsibility,
(4) After reviewing the submission of
the State, if any, made pursuant to
paragraph (a)(3) of this section, the Ad-
ministrator shall make a final deter-
mination either that the State no
longer meets the requirements of 40
OFB part 142, subpart B, or that the
State continues to meet those require-
ments, and shall notify the State of his
or her determination. Any final deter-
mination that the State no longer
meets the requirements of 40 CFR part
142, subpart B, shall not become effec-
tive except as provided in § 142.13.
(b) If a State which has primary en-
forcement responsibility decides to re-
linquish that authority, it may do so
by notifying the Administrator in writ-
ing of the State's decision at least 90
days before the effective date of the de-
cision.
[54 FR 52140, Dec. 20, 1989, as amended at 60
FE 33661, June 28, 1995]
589
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§142.18
40 CFR Ch. I (7-1-04 Edition)
§142.18 EPA review of State moni-
toring determinations.
(a) A Regional Administrator may
annul a State monitoring- determina-
tion for the types of determinations
identified in §§141.23(b), 141.23(c),
141.24(f), 141.24(h). and 141.40(n) in ac-
cordance with the procedures in para-
graph (b) of this section.
(b) When information available to a
Regional Administrator, such as the
results of an annual review, indicate a
State determination fails to apply the
standards of the approved State pro-
gram, he may propose to annul the
State monitoring determination by
sending the State and the affected PWS
a draft Rescission Order. The draft
order shall:
(1) Identify the PWS, the State deter-
mination, and the provisions at issue;
(2) Explain why the State determina-
tion is not in compliance with the
State program and must be changed;
and
(3) Describe the actions and terms of
operation the PWS will be required to
implement.
(c) The State and PWS shall have 60
days to comment on the draft Rescis-
sion Order.
(d) The Regional Administrator may
not issue a Rescission Order to impose
conditions less stringent than those
imposed by the State.
(e) The Regional Administrator shall
also provide an opportunity for com-
ment upon the draft Rescission Order,
by
(1) Publishing a notice in a news-
paper in general circulation in commu-
nities served by the affected system;
and
(2) Providing 30 days for public com-
ment on the draft order.
(f) The State shall demonstrate that
the determination is reasonable, based
on its approved State program.
(g) The Regional Administrator shall
decide within 120 days after issuance of
the draft Rescission Order to:
(1) Issue the Rescission Order as
drafted:
(2) Issue a modified Rescission Order;
or
(3) Cancel the Rescission Order.
(h) The Regional Administrator shall
set forth the reasons for his decision,
including a responsiveness summary
addressing significant comments from
the State, the PWS and the public.
(i) The Regional Administrator shall
send a notice of his final decision to
the State, the PWS and all parties who
commented upon the draft Rescission
Order.
(j) The Rescission Order shall remain
in effect until cancelled by the Re-
gional Administrator. The Regional
Administrator may cancel a Rescission
Order at any time, so long as he noti-
fies those who commented on the draft
order.
(k) The Regional Administrator may
not delegate the signature authority
for a final Rescission Order or the can-
cellation of an order.
(1) Violation of the actions, or terms
of operation, required by a Rescission
Order is a violation of the Safe Drink-
ing Water Act.
[56 PR 3595, Jan. 30, 1991]
§142.19 EPA review of State imple-
mentation of national primary
drinking water regulations for lead
and copper.
(a) Pursuant to the procedures in this
section, the Regional Administrator
may review state determinations es-
tablishing corrosion control or source
water treatment requirements for lead
or copper and may issue an order estab-
lishing federal treatment requirements
for a public water system pursuant to
§141.82 (d) and (f) and §141.83(b) (2) and
(4) where the Regional Administrator
finds that:
(1) A State has failed to issue a treat-
ment determination by the applicable
deadline:
(2) A State has abused its discretion
in making corrosion control or source
water treatment determinations in a
substantial number of cases or in cases
affecting a substantial population, or
(3) The technical aspects of State's
determination would be indefensible in
an expected federal enforcement action
taken against a system.
(b) If the Regional Administrator de-
termines that review of state determi-
nation(s) under this section may be ap-
propriate, he shall request the State to
590
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Environmental Protection Agency
§142.19
forward to EPA the state determina-
tion and all information that was con-
sidered by the State in making its de-
termination, including public com-
ments, if any, within 60 days of the Re-
gional Adminstrator's request.
(c) Proposed review of state deter-
minations:
(1) Where the Regional Administrator
finds that review of a state determina-
tion under paragraph (a) of this section
is appropriate, he shall issue a pro-
posed review order which shall:
(i) Identify the public water sys-
tem(s) affected, the State determina-
tion being reviewed and the provisions
of state and/or federal law at issue;
(ii) Identify the determination that
the State failed to carry out by the ap-
plicable deadline, or identify the par-
ticular provisions of the State deter-
mination which, in the Eegional Ad-
ministrator's judgment, fail to carry
out properly applicable treatment re-
quirements, and explain the basis for
the Regional Administrator's conclu-
sion:
(iii) Identify the treatment require-
ments which the Regional Adminis-
trator proposes to apply to the affected
system(s), and explain the basis for the
proposed requirements;
(iv) Request public comment on the
proposed order and the supporting
record,
(2) The Regional Administrator shall
provide notice of the proposed review
order by:
(i) Mailing the proposed order to the
affected public water system(s), the
state agency whose order is being
reviewed, and any other parties of
interest known to the Regional Admin-
istrator; and
(ii) Publishing a copy of the proposed
order in a newspaper of general circula-
tion in the affected communities.
(3) The Regional Administrator shall
make available for public inspection
during the comment period the record
supporting the proposed order, which
shall include all of the information
submitted by the State to EPA under
paragraph (b) of this section, all other
studies, monitoring data and other in-
formation considered by the Agency in
developing the proposed order,
(d) Final review order:
(1) Based upon review of all informa-
tion obtained regarding the proposed
review order, including public com-
ments, the Regional Administrator
shall issue a final review order within
120 days after issuance of the proposed
order which affirms, modifies, or with-
draws the proposed order. The Regional
Administrator may extend the time pe-
riod for issuing the final order for good
cause. If the final order modifies or
withdraws the proposed order, the final
order shall explain the reasons sup-
porting the change.
(2) The record of the final order shall
consist of the record supporting the
proposed order, all public comments,
all other information considered by the
Regional Administrator in issuing the
final order and a document responding
to all significant public comments sub-
mitted on the proposed order. If new
points are raised or new material sup-
plied during the public comment pe-
riod, the Regional Administrator may
support the responses on those matters
by adding new materials to the record.
The record shall be complete when the
final order is issued.
(3) Notice of the final order shall be
provided by mailing the final order to
the affected system(s), the State, and
all parties who commented on the pro-
posed order.
(4) Upon issuance of the final order,
its terms constitute requirements of
the national primary drinking water
regulation for lead and/or copper until
such time as the Regional Adminis-
trator issues a new order (which may
include recision of the previous order)
pursuant to the procedures in this sec-
tion. Such requirements shall super-
sede any inconsistent treatment re-
quirements established by the State
pursuant to the national primary
drinking water regulations for lead and
copper.
(5) The Regional Administrator may
not issue a final order to impose condi-
tions less stringent than those imposed
by the State.
(e) The Regional Administrator may
not delegate authority to sign the final
order under this section.
(f) Final action of the Regional Ad-
ministrator under paragraph (d) of this
section shall constitute action of the
591
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§142.20
40 CFR Ch. I (7-1-04 Edition)
Administrator for purposes of 42 U.S.C.
§300j-7(aX2).
[56 FR 26563, June 7, 1991]
Subpart C—Review of State-Issued
Variances and Exemptions
§ 142.20 State-issued variances and ex-
emptions under Section 1415(a) and
Section 1416 of the Act.
(a) States with primary enforcement
responsibility may issue variances to
public water systems (other than small
system variances) from the require-
ments of primary drinking water regu-
lations under conditions and in a man-
ner which are not less stringent than
the requirements under Section 1415(a)
of the Act. In States that do not have
primary enforcement responsibility,
variances may "be granted by the Ad-
ministrator pursuant to Subpart E of
this part.
(1) A State must document all find-
ings that are required under Section
1415(a) of the Act.
(2) If a State prescribes a schedule
pursuant to section 1415(a) of the Act
requiring compliance with a contami-
nant level for which the variance is
granted later than five years from the
date of issuance of the variance the
State must—
(i) Document its rationale for the ex-
tended compliance schedule;
(ii) Discuss the rationale for the ex-
tended compliance schedule in the re-
quired public notice and opportunity
for public hearing; and
(iii) Provide the shortest practicable
time schedule feasible under the cir-
cumstances.
(b) States with primary enforcement
responsibility may issue exemptions
from the requirements of primary
drinking water regulations under con-
ditions and in a manner which are not
less stringent than the requirements
under Section 1416 of the Act. In States
that do not have primary enforcement
responsibility, exemptions may be
granted by the Administrator pursuant
to Subpart F of this part.
(1) A State must document all find-
ings that are required under Section
1416 of the Act:
(i) Before finding that management
and restructuring changes cannot be
made, a State must consider the fol-
lowing measures, and the availability
of State Revolving Loan Fund assist-
ance, or any other Federal or State
program, that is reasonably likely to
be available within the period of the
exemption to implement these meas-
ures:
(A) Consideration of rate increases,
accounting changes, the appointment
of a State-certified operator under the
State's Operator Certification pro-
gram, contractual agreements for joint
operation with one or more public
water systems;
(B) Activities consistent with the
State's Capacity Development Strat-
egy to help the public water system ac-
quire and maintain technical, finan-
cial, and managerial capacity to come
into compliance with the Act; and
(C) Ownership changes, physical con-
solidation with another public water
system, or other feasible and appro-
priate means of consolidation which
would result in compliance with the
Act;
(ii) The State must consider the
availability of an alternative source of
water, including the feasibility of part-
nerships with neighboring public water
systems, as identified by the public
water system or by the State con-
sistent with the Capacity Development
Strategy.
(2) In the case of a public water sys-
tem serving a population of not more
than 3,300 persons and which needs fi-
nancial assistance for the necessary
improvements under the initial compli-
ance schedule, an exemption granted
by the State under section
1416(b)(2)(B)(i) or (ii) of the Act may be
renewed for one or more additional 2-
year periods, but not to exceed a total
of 6 additional years, only if the State
establishes that the public water sys-
tem is taking all practicable steps to
meet the requirements of Section
1416(b)(2)(B) of the Act and the estab-
lished compliance schedule to achieve
full compliance with the contaminant
level or treatment technique for which
the exemption was granted. A State
must document its findings in granting
an extension under this paragraph.
[63 PR 43847, Aug. 14, 1998]
592
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Environmental Protection Agency
§142.23
§142.21 State consideration of a vari-
ance or exemption request.
A State with primary enforcement
responsibility shall act on any variance
or exemption request submitted to it,
within 90 days of receipt of the request.
§ 142.22 Review? of State variances, ex-
emptions and schedules.
(a) Not, later than 18 months after the
effective date of the interim national
primary drinking water regulations the
Administrator shall complete a com-
prehensive review of the variances and
exemptions granted (and schedules pre-
scribed pursuant thereto) by the States
with primary enforcement responsi-
bility during the one-year period begin-
ning on such effective date. The Ad-
ministrator shall conduct such subse-
quent reviews of exemptions and sched-
ules as he deems necessary to carry out
the purposes of this title, but at least
one review shall be completed within
each 3-year period following the com-
pletion of the first review under this
paragraph.
(b) Notice of a proposed review shall
be published in the FEDERAL REGISTER.
Such notice shall (1) provide informa-
tion respecting the location of data and
other information respecting the
variances and exemptions to be re-
viewed (including data and other infor-
mation concerning new scientific mat-
ters bearing on such variances and ex-
emptions), and (2) advise of the oppor-
tunity to submit comments on the
variances and exemptions reviewed and
on the need for continuing them. Upon
completion of any such review, the Ad-
ministrator shall publish in the FED-
ERAL REGISTER the results of his re-
view, together with findings responsive
to any comments submitted in connec-
tion with such review.
§ 142.23 Notice to State.
(a) If the Administrator finds that a
State has, in a substantial number of
instances, abused its discretion in
granting: variances or exemptions
under section 1415(a) or section 1416(a)
of the Act or failed to prescribe sched-
ules in accordance with section 1415(a)
or section 1416(b) of the Act, he shall
notify the State of his findings. Such
notice shall:
(1) Identify each public water system
for which the finding was made;
(2) Specify the reasons for the find-
ing; and
(3) As appropriate, propose revoca-
tion of specific variances or exemp-
tions, or propose revised schedules for
specific public water systems.
(b) The Administrator shall also no-
tify the State of a public hearing to be
held on the provisions of the notice re-
quired by paragraph (a) of this section.
Such notice shall specify the time and
location for the hearing. If, upon noti-
fication of a finding by the Adminis-
trator, the State takes adequate cor-
rective action, the Administrator shall
rescind his notice to the State of a pub-
lic hearing, provided that the Adminis-
trator is notified of the corrective ac-
tion prior to the hearing.
(c) The Administrator shall publish
notice of the public hearing in the FED-
ERAL REGISTER and in a newspaper or
newspapers of general circulation in
the involved State including a sum-
mary of the findings made pursuant to
paragraph (a) of this section, a state-
ment of the time and location for the
hearing, and the address and telephone
number of an office at which interested
persons may obtain further informa-
tion concerning the hearing.
(d) Hearings convened pursuant to
paragraphs (b) and (c) of this section
shall be conducted before a hearing of-
ficer to be designated by the Adminis-
trator. The hearing shall be conducted
by the hearing officer in an informal,
orderly and expeditious manner. The
hearing officer shall have authority to
call witnesses, receive oral and written
testimony and take such other action
as may be necessary to assure the fair
and efficient conduct of the hearing.
Following the conclusion of the hear-
ing, the hearing officer shall forward
the record of the hearing to the Admin-
istrator,
(e) Within 180 days after the date no-
tice is given pursuant to paragraph (b)
of this section, the Administrator
shall:
(1) Rescind the finding for which the
notice was given and promptly notify
the State of such rescission, or
(2) Promulgate with any modifica-
tions as appropriate such revocation
and revised schedules proposed in such
593
-------
§142,24
40 CFR Ch. I (7-1-04 Edition)
notice and promptly notify the State of
such action.
(f) A revocation or revised schedule
shall take effect 90 days after the State
is notified under paragraph (e)(2) of
this section.
§ 142.24 Administrator's rescission.
If, upon notification of a finding by
the Administrator under §142.23, the
State takes adequate corrective action
before the effective date of the revoca-
tion or revised schedule, the Adminis-
trator shall rescind the application of
his finding to that variance, exemption
or schedule.
Subpart D—Federal Enforcement
§142,30 Failure by State to assure en-
forcement,
(a) The Administrator shall notify a
State and the appropriate supplier of
water whenever he finds during a pe-
riod in which the State has primary en-
forcement responsibility for public
water systems that a public water sys-
tem within such State is not in compli-
ance with any primary drinking water
regulation contained in part 141 of this
chapter or with any schedule or other
requirements imposed pursuant to a
variance or exemption granted under
section 1415 or 1416 of the Act: Provided,
That the State will be deemed to have
been notified of a violation referred to
in a report submitted by the State.
(b) The Administrator shall provide
advice and technical assistance to such
State and public water system as may
be appropriate to bring the system into
compliance by the earliest feasible
time.
[41 FR 2918, Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987]
§ 142.31 [Reserved]
§ 142.32 Petition for public hearing.
(a) If the Administrator makes a
finding of noncompliance pursuant to
§142.30 with respect to a public water
system in a State which has primary
enforcement responsibility, the Admin-
istrator may, for the purpose of assist-
ing that State in carrying out such re-
sponsibility and upon the petition of
such State or public water system or
persons served by such system, hold,
after appropriate notice, public hear-
ings for the purpose of gathering infor-
mation as described in §142.33.
(b) A petition for a public hearing
pursuant to paragraph (a) of this sec-
tion shall be filed with the Adminis-
trator and shall include the following
information:
(1) The name, address and telephone
number of the individual or other enti-
ty requesting a hearing.
(2) If the petition is filed by a person
other than the State or public water
system, a statement that the person is
served by the system.
(3) A brief statement of information
that the requesting person intends to
submit at the requested hearing,
(4) The signature of the individual
submitting the petition; or, if the peti-
tion is filed on behalf of a State, public
water system or other entity, the sig-
nature of a responsible official of the
State or other entity.
§ 142.83 Public hearing.
(a) If the Administrator grants the
petition for public hearing, he shall
give appropriate public notice of such
hearing. Such notice shall be by publi-
cation in the FEDERAL REGISTER and in
a newspaper of general circulation or
by other appropriate communications
media covering the area served by such
public water system.
(b) A hearing officer designated by
the Administrator shall gather during
the public hearing information from
technical or other experts, Federal,
State, or other public officials, rep-
resentatives of the public water sys-
tem, persons served by the system, and
other interested persons on:
(1) The ways in which the system can
within the earliest feasible time be
brought into compliance, and
(2) The means for the maximum fea-
sible protection of the public health
during any period in which such sys-
tem is not in compliance.
(c) On the basis of the hearing and
other available information the Ad-
ministrator shall issue recommenda-
tions which shall be sent to the State
and public water system and shall be
made available to the public and com-
munications media.
594
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Environmental Protection Agency
§ 142.34 Entry and inspection of public
water systems,
(a) Any supplier of water or other
person subject to a national primary
drinking water regulation shall, at any
time, allow the Administrator, or a
designated representative of the Ad-
ministrator, upon presenting appro-
priate credentials and a written notice
of inspection, to enter any establish-
ment, facility or other property of such
supplier or other person to determine
whether such supplier or other person
has acted or is acting in compliance
with the requirements of the Act or
subchapter D of this chapter. Such in-
spection may include inspection, at
reasonable times, of records, files, pa-
pers, processes, controls and facilities,
or testing of any feature of a public
water system, including its raw water
source.
(b) Prior to entry into any establish-
ment, facility or other property within
a State which has primary enforcement
responsibility, the Administrator shall
notify, in writing, the State agency
charged with responsibility for safe
drinking water of his intention to
make such entry and shall include in
his notification a statement of reasons
for such entry. The Administrator
shall, upon a showing by the State
agency that such an entry will be det-
rimental to the administration of the
State's program of primary enforce-
ment responsibility, take such showing
into consideration in determining
whether to make such entry. The Ad-
ministrator shall in any event offer the
State agency the opportunity of having
a representative accompany the Ad-
ministrator or his representative on
such entry.
(c) No State agency which receives
notice under paragraph (b) of this sec-
tion may use the information con-
tained in the notice to inform the per-
son whose property is proposed to be
entered of the proposed entry; if a
State so uses such information, notice
to the agency under paragraph (b) of
this section is not required for subse-
quent inspections of public water sys-
tems until such time as the Adminis-
trator determines that the agency has
provided him satisfactory assurances
that it will no longer so use informa-
§142.41
tion contained in a notice received
under paragraph (b) of this section.
Subpart E—Variances Issued by
the Administrator Under Sec-
tion 1415(a) of the Act
§ 142.40 Requirements for a variance.
(a) The Administrator may grant one
or more variances to any public water
system within a State that does not
have primary enforcement responsi-
bility from any requirement respecting
a maximum contaminant level of an
applicable national primary drinking
water regulation upon a finding that:
(1) Because of characteristics of the
raw water sources which are reason-
ably available to the system, the sys-
tem cannot meet the requirements re-
specting the maximum contaminant
levels of such drinking water regula-
tions despite application of the best
technology, treatment techniques, or
other means, which the Administrator
finds are generally available (taking
costs into consideration); and
(2) The granting of a variance will
not result in an unreasonable risk to
the health of persons served by the sys-
tem.
(b) The Administrator may grant one
or more variances to any public water
system within a State that does not
have primary enforcement responsi-
bility from any requirement of a speci-
fied treatment technique of an applica-
ble national primary drinking water
regulation upon a finding that the pub-
lic water system applying for the vari-
ance has demonstrated that such treat-
ment technique is not necessary to pro-
tect the health of persons because of
the nature of the raw water source of
such system.
§ 142.41 Variance request.
A supplier of water may request the
granting of a variance pursuant to this
subpart for a public water system with-
in a State that does not have primary
enforcement responsibility by submit-
ting a request for a variance in writing
to the Administrator. Suppliers of
water may submit a joint request for
variances when they seek similar
variances under similar circumstances.
Any written request for a variance or
595
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§142.42
40 CFR Ch. I (7-1-04 Edition)
variances shall include the following
information:
(a) The nature and duration of vari-
ance requested.
(b) Relevant analytical results of
water quality sampling of the system,
including results of relevant tests con-
ducted pursuant to the requirements of
the national primary drinking water
regulations,
(c) For any request made under
§142.40(a):
(1) Explanation in full and evidence
of the best available treatment tech-
nology and techniques.
(2) Economic and legal factors rel-
evant to ability to comply.
(3) Analytical results of raw water
quality relevant to the variance re-
quest.
(4) A proposed compliance schedule,
including the date each step toward
compliance will be achieved. Such
schedule shall include as a minimum
the following dates:
(i) Date by which arrangement for al-
ternative raw water source or improve-
ment of existing raw water source will
be completed.
(ii) Date of initiation of the connec-
tion of the alternative raw water
source or improvement of existing raw
water source.
(iii) Date by which final compliance
is to be achieved.
(5) A plan for the provision of safe
drinking water in the case of an exces-
sive rise in the contaminant level for
which the variance is requested.
(6) A plan for additional interim con-
trol measures during the effective pe-
riod of variance.
(d) For any request made under
§142.40(b), a statement that the system
will perform monitoring and other rea-
sonable requirements prescribed by the
Administrator as a condition to the
variance.
(e) Other information, if any, be-
lieved to be pertinent by the applicant.
(f) Such other information as the Ad-
ministrator may require.
[41 PR 2918, Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987]
§ 142.42 Consideration of a variance
request.
(a) The Administrator shall act on
any variance request submitted pursu-
ant to §142.41 within 90 days of receipt
of the request.
(b) In his consideration of whether
the public water system is unable to
comply with a contaminant level re-
quired by the national primary drink-
ing water regulations because of the
nature of the raw water source, the Ad-
ministrator shall consider such factors
as the following:
(1) The availability and effectiveness
of treatment methods for the contami-
nant for which the variance is re-
quested.
(2) Cost and other economic consider-
ations such as implementing treat-
ment, improving the quality of the
source water or using an alternate
source.
(c) A variance may be issued to a
public water system on the condition
that the public water system install
the best technology, treatment tech-
niques, or other means, which the Ad-
ministrator finds are available (taking
costs into consideration) and based
upon an evaluation satisfactory to the
Administrator that indicates that al-
ternative sources of water are not rea-
sonably available to the public water
system.
(d) In his consideration of whether a
public water system should be granted
a variance to a required treatment
technique because such treatment is
unnecessary to protect the public
health, the Administrator shall con-
sider such factors as the following:
(1) Quality of the water source in-
cluding water quality data and perti-
nent sources of pollution.
(2) Source protection measures em-
ployed by the public water system.
[41 PR 2918. Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987: 63 FR 43847. Aug. 14,
1998]
§ 142.43 Disposition of a variance re-
quest.
(a) If the Administrator decides to
deny the application for a variance, he
shall notify the applicant of his inten-
tion to issue a denial. Such notice shall
include a statement of reasons for the
proposed denial, and shall offer the ap-
plicant an opportunity to present,
within 30 days of receipt of the notice,
additional information or argument to
the Administrator. The Administrator
596
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Environmental Protection Agency
§142.44
shall make a final determination on
the request within 30 days after receiv-
ing any such additional information or
argument. If no additional Information
or argument is submitted by the appli-
cant the application shall be denied.
(b) If the Administrator proposes to
grant a variance request submitted
pursuant to §142.41, he shall notify the
applicant of his decision in writing.
Such notice shall identify the variance,
the facility covered, and shall specify
the period of time for which the vari-
ance will be effective.
(1) For the type of variance specified
in §142.40(a) such notice shall provide
that the variance will be terminated
when the system comes into compli-
ance with the applicable regulation,
and may be terminated upon a finding
by the Administrator that the system
has failed to comply with any require-
ments of a final schedule issued pursu-
ant to §142.44.
(2) For the type of variance specified
in §142.40{b) such notice shall provide
that the variance may be terminated
at any time upon a finding that the na-
ture of the raw water source is such
that the specified treatment technique
for which the variance was granted is
necessary to protect the health of per-
sons or upon a finding that the public
water system has failed to comply with
monitoring and other requirements
prescribed by the Administrator as a
condition to the granting of the vari-
ance.
(c) For a variance specified in
§142.40(a)(l) the Administrator shall
propose a schedule for:
(1) Compliance (including increments
of progress) by the public water system
with each contaminant level require-
ment covered by the variance; and,
(2) Implementation by the public
water system of such additional con-
trol measures as the Administrator
may require for each contaminant cov-
ered by the variance.
(d) The proposed schedule for compli-
ance shall specify dates by which steps
towards compliance are to be taken, in-
cluding at the minimum, where appli-
cable:
(I) Date by which arrangement for an
alternative raw water source or im-
provement of existing raw water source
will be completed.
(2) Date of Initiation of the connec-
tion for the alternative raw water
source or improvement of the existing
raw water source.
(3) Date by which final compliance is
to be achieved,
(e) The proposed schedule may, If the
public water system has no access to
an alternative raw water source, and
can effect or anticipate no adequate
improvement of the existing raw water
source, specify an indefinite time pe-
riod for compliance until a new and ef-
fective treatment technology is devel-
oped at which time a new compliance
schedule shall be prescribed by the Ad-
ministrator,
(f) The proposed schedule for imple-
mentation of additional interim con-
trol measures during the period of vari-
ance shall specify interim treatment
techniques, methods and equipment,
and dates by which steps toward meet-
ing the additional interim control
measures are to be met.
(g) The schedule shall be prescribed
by the Administrator at the time of
granting of the variance, subsequent to
provision of opportunity for hearing
pursuant to §142.44.
[41 FR 2918, Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987]
§142.44 Public hearings on variances
and schedules.
(a) Before a variance and schedule
proposed by the Administrator pursu-
ant to §142.43 may take effect, the Ad-
ministrator shall provide notice and
opportunity for public hearing on the
variance and schedule. A notice given
pursuant to the preceding sentence
may cover the granting of more than
one variance and a hearing held pursu-
ant to such notice shall include each of
the variances covered by the notice.
(b) Public notice of an opportunity
for hearing on a variance and schedule
shall be circulated In a manner de-
signed to inform interested and poten-
tially interested persons of the pro-
posed variance and schedule, and shall
include at least the following:
(1) Posting of a notice in the prin-
cipal post office of each municipality
or area served by the public water sys-
tem, and publishing of a notice in a
597
-------
§142,45
40 CFR Ch. I (7-1-04 Edition)
newspaper or newspapers of general cir-
culation in the area served by the pub-
lic water system; and
(2) Mailing of a notice to the agency
of the State in which the system is lo-
cated which is responsible for the
State's water supply program, and to
other appropriate State or local agen-
cies at the Administrator's discretion.
(3) Such notice shall include a sum-
mary of the proposed variance and
schedule and shall inform interested
persons that they may request a public
hearing on the proposed variance and
schedule.
(c) Bequests for hearing may be sub-
mitted by any interested person other
than a Federal agency. Frivolous or in-
substantial requests for hearing may
be denied by the Administrator. Re-
quests must be submitted to the Ad-
ministrator within 30 days after
issuance of the public notices provided
for in paragraph (b) of this section.
Such requests shall include the fol-
lowing information:
(1) The name, address and telephone
number of the individual, organization
or other entity requesting a hearing;
(2) A brief statement of the interest
of the person making the request in the
proposed variance and schedule, and of
information that the requester intends
to submit at such hearing;
(3) The signature of the individual
making the request, or, if the request
is made on "behalf of an organization or
other entity, the signature of a respon-
sible official of the organization or
other entity.
(d) The Administrator shall give no-
tice in the manner set forth in para-
graph (b) of this section of any hearing
to be held pursuant to a request sub-
mitted by an interested person or on
his own motion. Notice of the hearing
shall also be sent to the persons re-
questing the hearing, if any. Notice of
the hearing shall include a statement
of the purpose of the hearing, informa-
tion regarding the time and location
for the hearing, and the address and
telephone number of an office at which
interested persons may obtain further
information concerning the hearing. At
least one hearing location specified in
the public notice shall be within the in-
volved State. Notice of hearing shall be
given not less than 15 days prior to the
time scheduled for the hearing.
(e) A hearing convened pursuant to
paragraph (d) of this section shall be
conducted before a hearing officer to be
designated by the Administrator. The
hearing shall be conducted by the hear-
ing officer in an informal, orderly and
expeditious manner. The hearing offi-
cer shall have authority to call wit-
nesses, receive oral and written testi-
mony and take such other action as
may be necessary to assure the fair and
efficient conduct of the hearing. Fol-
lowing the conclusion of the hearing,
the hearing officer shall forward the
record of the hearing to the Adminis-
trator.
(f) The variance and schedule shall
become effective 30 days after notice of
opportunity for hearing is given pursu-
ant to paragraph (b) of this section if
no timely request for hearing is sub-
mitted and the Administrator does not
determine to hold a public hearing on
Ms own motion.
[41 PR 2918, Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987]
§ 142.45 Action after hearing,
Within 30 days after the termination
of the public hearing held pursuant to
§142.44. the Administrator shall, taking
into consideration information ob-
tained during such hearing and rel-
evant information, confirm, revise or
rescind the proposed variance and
schedule.
[52 PR 20675, June 2, 1987]
§ 142.46 Alternative treatment tech-
niques.
The Administrator may grant a vari-
ance from any treatment technique re-
quirement of a national primary drink-
ing water regulation to a supplier of
water, whether or not the public water
system for which the variance is re-
quested is located in a State which has
primary enforcement responsibility,
upon a showing from any person that
an alternative treatment technique not
included in such requirement Is at
least as efficient in lowering the level
of the contaminant with respect to
598
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Environmental Protection Agency
§142.51
which such requirements was pre-
scribed. A variance under this para-
graph shall be conditioned on the use
of the alternative treatment technique
which is the basis of the variance.
Subpart F—Exemptions Issued by
the Administrator
§ 142.50 Requirements for an exemp-
tion.
(a) The Administrator may exempt
any public water system within a State
that does not have primary enforce-
ment responsibility from any require-
ment regarding a maximum contami-
nant level or any treatment technique
requirement, or from both, of an appli-
cable national primary drinking water
regulation upon a finding that—
(1) Due to compelling factors (which
may include economic factors, includ-
ing qualification of the public water
system as a system serving a disadvan-
taged community pursuant to section
1452(d) of the Act), the public water
system Is unable to comply with such
contaminant level or treatment tech-
nique requirement or to implement
measures to develop an alternative
source of water supply;
(2) The public water system was in
operation on the effective date of such
contaminant level or treatment tech-
nique requirement, or for a public
water system that was not in operation
"by that date, no reasonable alternative
source of drinking water is available to
such new public water system;
(3) The granting of the exemption
will not result in an unreasonable risk
to health; and
(4) Management or restructuring
changes (or both), as provided in
§142.20(b)(l)(i), cannot reasonably be
made that will result in compliance
with the applicable national primary
drinking water regulation or, if com-
pliance cannot be achieved, improve
the quality of the drinking water.
(b) No exemption shall be granted un-
less the public water system estab-
lishes that the public water system is
taking all practicable steps to meet
the standard; and
(1) The public water system cannot
meet the standard without capital im-
provements which cannot be completed
prior to the date established pursuant
to Section 1412(b)(10) of the Act;
(2) In the case of a public water sys-
tem which needs financial assistance
for the necessary improvements, the
public water system has entered into
an agreement to obtain such financial
assistance or assistance pursuant to
Section 1452 of the Act, or any other
Federal or State program that is rea-
sonably likely to be available within
the period of the exemption; or
(3) The public water system has en-
tered into an enforceable agreement to
become a part of a regional public
water system.
(c) A public water system may not
receive an exemption under this sub-
part if the public water system was
granted a variance under Section
1415(e) of the Act.
[63 FR 43847, Aug'. 14. 1998]
§ 142.51 Exemption request.
A supplier of water may request the
granting of an exemption pursuant to
this subpart for a public water system
within a State that does not have pri-
mary enforcement responsibility by
submitting a request for exemption in
writing to the Administrator. Sup-
pliers of water may submit a joint re-
quest for exemptions when they seek
similar exemptions under similar cir-
cumstances. Any written request for an
exemption or exemptions shall include
the following information:
(a) The nature and duration of ex-
emption requested.
(b) Relevant analytical results of
water quality sampling of the system,
including results of relevant tests con-
ducted pursuant to the requirements of
the national primary drinking water
regulations.
(c) Explanation of the compelling
factors such as time or economic fac-
tors which prevent such system from
achieving compliance.
(d) Other information, if any, be-
lieved by the applicant to be pertinent
to the application.
(e) A proposed compliance schedule,
including the date when each step to-
ward compliance will be achieved.
(f) Such other information as the Ad-
ministrator may require.
599
203-160 D-20
-------
§142.52
40 CFR Ch. I (7-1-04 Edition)
§ 142.52 Consideration of an exemption
request.
(a) The Administrator shall act on
any exemption request submitted pur-
suant to §142.51 within 90 days of re-
ceipt of the request,
(b) In his consideration of whether
the public water system is unable to
comply due to compelling factors, the
Administrator shall consider such fac-
tors as the following:
(1) Construction, installation, or
modification of the treatment equip-
ment or systems,
(2) The time needed to put into oper-
ation a new treatment facility to re-
place an existing system which is not
in compliance.
(3) Economic feasibility of compli-
ance,
§142.53 Disposition of an exemption
request.
(a) If the Administrator decides to
deny the application for an exemption,
he shall notify the applicant of his in-
tention to issue a denial. Such notice
shall include a statement of reasons for
the proposed denial, and shall offer the
applicant an opportunity to present,
within 30 days of receipt of the notice,
additional information or argument to
the Administrator. The Administrator
shall make a final determination on
the request within 30 days after receiv-
ing any such additional information or
argument. If no additional information
or argument is submitted by the appli-
cant, the application shall be denied.
(b) If the Administrator grants an ex-
emption request submitted pursuant to
§142.51, he shall notify the applicant of
his decision in writing. Such notice
shall identify the facility covered, and
shall specify the termination date of
the exemption. Such notice shall pro-
vide that the exemption will be termi-
nated when the system comes into
compliance with the applicable regula-
tion, and may be terminated upon a
finding by the Administrator that the
system has failed to comply with any
requirements of a final schedule issued
pursuant to § 142.55.
(c) The Administrator shall propose a
schedule for:
(1) Compliance (including increments
of progress or measures to develop an
alternative source of water supply) by
the public water system with each con-
taminant level requirement or treat-
ment technique requirement with re-
spect to which the exemption was
granted; and
(2) Implementation by the public
water system of such control measures
as the Administrator may require for
each contaminant covered by the ex-
emption.
(d) The schedule shall be prescribed
by the Administrator at the time the
exemption is granted, subsequent to
provision of opportunity for hearing
pursuant to §142.54.
[41 PR 2918, Jan, 20, 1976, as amended at 52
FB 20675, June 2, 1987; 63 FR 43848, Aug. 14,
1998]
§142.54 Public hearings on exemption
schedules.
(a) Before a schedule proposed by the
Administrator pursuant to §142.53 may
take effect, the Administrator shall
provide notice and opportunity for pub-
lic hearing on the schedule. A notice
given pursuant to the preceding sen-
tence may cover the proposal of more
than one such schedule and a hearing
held pursuant to such notice shall in-
clude each of the schedules covered by
the notice.
(b) Public notice of an opportunity
for hearing on an exemption schedule
shall be circulated in a manner de-
signed to inform interested and poten-
tially interested persons of the pro-
posed schedule, and shall include at
least the following:
(1) Posting of a notice in the prin-
cipal post office of each municipality
or area served by the public water sys-
tem, and publishing of a notice in a
newspaper or newspapers of general cir-
culation in the area served by the pub-
lic water system.
(2) Mailing of a notice to the agency
of the State in which the system is lo-
cated which is responsible for the
State's water supply program and to
other appropriate State or local agen-
cies at the Administrator's discretion.
(3) Such notices shall include a sum-
mary of the proposed schedule and
shall inform interested persons that
they may request a public hearing on
the proposed schedule.
600
-------
Environmental Protection Agency
§ 142.57
(c) Bequests for hearing may be sub-
mitted by any interested person other
than a Federal agency. Frivolous or in-
substantial requests for hearing may
be denied by the Administrator. Re-
quests must be submitted to the Ad-
ministrator within 30 days after
issuance of the public notices provided
for in paragraph (b) of this section.
Such requests shall include the fol-
lowing information:
(1) The name, address and telephone
number of the individual, organization
or other entity requesting a hearing;
(2) A brief statement of the interest
of the person making the request in the
proposed schedule and of information
that the requesting person intends to
submit at such hearing; and
(3) The signature of the individual
making the request, or, if the request
is made on behalf of an organization or
other entity, the signature of a
responsibile official of the organization
or other entity.
(d) The Administrator shall give no-
tice in the manner set forth in para-
graph (to) of this section of any hearing
to be held pursuant to a request sub-
mitted by an interested person or on
his own motion. Notice of the hearing
shall also be sent to the person re-
questing the hearing, if any. Notice of
the hearing shall include a statement
of the purpose of the hearing, informa-
tion regarding the time and location of
the hearing, and the address and tele-
phone number of an office at which in-
terested persons may obtain further in-
formation concerning the hearing. At
least one hearing location specified in
the public notice shall be within the in-
volved State. Notice of the hearing
shall be given not less than 15 days
prior to the time scheduled for the
hearing.
(e) A hearing convened pursuant to
paragraph (d) of this section shall be
conducted before a hearing officer to be
designated by the Administrator. The
hearing shall be conducted by the hear-
ing officer in an informal, orderly and
expeditious manner. The hearing offi-
cer shall have authority to call wit-
nesses, receive oral and written testi-
mony and take such action as may be
necessary to assure the fair and effi-
cient conduct of the hearing. Following
the conclusion of the hearing, the hear-
ing officer shall forward the record of
the hearing to the Administrator.
[41 FR 2918, Jan. 20, 1976, as amended at 52
PR 20675, June 2, 1987]
§ 142.SS Final schedule.
(a) Within 30 days after the termi-
nation of the public hearing pursuant
to §142.54, the Administrator shall,
taking into consideration information
obtained during such hearing, revise
the proposed schedule as necessary and
prescribe the final schedule for compli-
ance and interim measures for the pub-
lic water system granted an exemption
under §142.52.
(b) Such schedule must require com-
pliance with each contaminant level
and treatment technique requirement
with respect to which the exemption
was granted as expeditiously as prac-
ticable but not later than 3 years after
the otherwise applicable compliance
date established in section 1412(b)(10) of
the Act.
(c) [Reserved]
[41 FR 2918, Jan. 20, 1976, as amended at 52
FR 20675. June 2, 1987: 63 PR 43848, Aug. 14.
1998]
§ 142,56 Extension of date for compli-
ance.
In the case of a public water system
which serves a population of not more
than 3,300 persons and which needs fi-
nancial assistance for the necessary
improvements, an exemption granted
under §142,50(b) (1) or (2) may be re-
newed for one or more additional 2-
year periods, but not to exceed a total
of 6 additional years, if the public
water system establishes that the pub-
lic water system is taking all prac-
ticable steps to meet the requirements
of section 1416(b)(2)(B) of the Act and
the established compliance schedule.
[63 FR 43848, Aug. 14,
§142.57 Bottled water, point-of-use,
and point-of-entry devices.
(a) A State may require a public
water system to use bottled water,
point-of-use devices, or point-of-entry
devices as a condition of granting an
exemption from the requirements of
§§141.61 (a) and (c), and 141.62 of this
chapter.
601
-------
§142.60
40 CFR Ch. I (7-1-04 Edition)
(b) Public water systems using bot-
tled water as a condition of obtaining
an exemption from the requirements of
§§141.61 (a) and (c) and 141.62(b) must
meet the requirements in §142.62(g).
(c) Public water systems that use
point-of-use or polnt-of-entry devices
as a condition for receiving an exemp-
tion must meet the requirements in
1141.6200.
[56 PR 3596, Jan. 30, 1991, as amended at 56
PR 30280, July 1, 1991]
Subpart G—Identification of Best
Technology, Treatment Tech-
niques or Other Means Gen-
erally Available
§142.60 Variances from the maximum
contaminant level for total
trihalomethancs.
(a) The Administrator, pursuant to
section 1415(a)(l)(A) of the Act, hereby
identifies the following' as the best
technology, treatment techiques or
other means generally available for
achieving compliance with the max-
imum contaminant level for total
trlhalomethanes (§141.12(c)):
(1) Use of chloramines as an alternate
or supplemental disinfectant or oxi-
dant.
(2) Use of chlorine dioxide as an al-
ternate or supplemental disinfectant or
oxidant.
(3) Improved existing clarification for
THM precursor reduction.
(4) Moving the point of chlorination
to reduce TTHM formation and, where
necessary, substituting for the use of
chlorine as a pre-oxidant chloramines,
chlorine dioxide or potassium per-
manganate.
(5) Use of powdered activated carbon
for THM precursor or TTHM reduction
seasonally or intermittently at dosages
not to exceed 10 mg/L on an annual av-
erage basis.
(b) The Administrator in a state that
does not have primary enforcement re-
sponsibility or a state with primary en-
forcement responsibility (primacy
state) that issues variances shall re-
quire a community water system to in-
stall and/or use any treatment method
Identified in §142.60(a) as a condition
for granting a variance unless the Ad-
ministrator or primacy state deter-
mines that such treatment method
identified in §142.60(a) is not available
and effective for TTHM control for the
system. A treatment method shall not
be considered to be "available and ef-
fective" for an individual system if the
treatment method would not be tech-
nically appropriate and technically
feasible for that system or would only
result in a marginal reduction in
TTHM for the system. If, upon applica-
tion by a system for a variance, the
Administrator or primacy state that
issues variances determines that none
of the treatment methods identified in
§142.60(a) is available and effective for
the system, that system shall be enti-
tled to a variance under the provisions
of section 1415(a)(l)(A) of the Act. The
Administrator's or primacy state's de-
termination as to the availability and
effectiveness of such treatment meth-
ods shall be based upon studies by the
system and other relevant information.
If a system submits information in-
tending to demonstrate that a treat-
ment method is not available and effec-
tive for TTHM control for that system,
the Administrator or primacy state
shall make a finding whether this in-
formation supports a decision that
such treatment method is not available
and effective for that system "before re-
quiring installation and/or use of such
treatment method.
(c) Pursuant to § 142.43 (c) through (g)
or corresponding state regulations, the
Administrator or primacy state that
issues variances shall issue a schedule
of compliance that may require the
system being granted the variance to
examine the following treatment meth-
ods (1) to determine the probability
that any of these methods will signifi-
cantly reduce the level of TTHM for
that system, and (2) if such probability
exists, to determine whether any of
these methods are technically feasible
and economically reasonable, and that
the TTHM reductions obtained will be
commensurate with the costs incurred
with the installation and use of such
treatment methods for that system:
Introduction of off-line water storage for
THM precursor reduction.
Aeration for TTHM reduction, where geo-
graphically and environmentally appro-
priate.
602
-------
Environmental Protection Agency
§ 142.61
Introduction of clarification where not
currently practiced.
Consideration of alternative sources of raw
water.
Use of ozone as an alternate or supple-
mental disinfectant or oxidant.
(d) If the Administrator or primacy
state that issues variances determines
that a treatment method identified in
§142.60{c) is technically feasible, eco-
nomically reasonable and will achieve
TTHM reductions commensurate with
the costs incurred with the installation
and/or use of such treatment method
for the system, the Administrator or
primacy state shall require the system
to install and/or use that treatment
method in connection with a compli-
ance schedule issued under the provi-
sions of section 1415(a)(l)(A) of the Act.
The Administrator's or primacy state's
determination shall be based upon
studies by the system and other rel-
evant information. In no event shall
the Administrator require a system to
install and/or use a treatment method
not described in § 142.60 (a) or (c) to ob-
tain or maintain a variance from the
TTHM Rule or in connection with any
variance compliance schedule.
[48 FR 8414, Feb. 28, 1983]
§142.61 Variances from the maximum
contaminant level for fluoride.
(a) The Administrator, pursuant to
section 1415(aKl)(A) of the Act, hereby
identifies the following as the best
technology, treatment techniques or
other means generally available for
achieving compliance with the Max-
imum Contaminant Level for fluoride.
(1) Activated alumina absorption,
centrally applied
(2) Reverse osmosis, centrally applied
(b) The Administrator in a state that
does not have primary enforcement re-
sponsibility or a state with primary en-
forcement responsibility (primacy
state) that issues variances shall re-
quire a community water system to in-
stall and/or use any treatment method
identified in §142.61(a) as a condition
for granting a variance unless the Ad-
ministrator or the primacy state deter-
mines that such treatment method
identified in §142.61(a) as a condition
for granting a variance is not available
and effective for fluoride control for
the system. A treatment method shall
not be considered to be "available and
effective" for an individual system if
the treatment method would not be
technically appropriate and tech-
nically feasible for that system. If,
upon application by a system for a
variance, the Administrator or pri-
macy state that issues variances deter-
mines that none of the treatment
methods identified in §142.61(a) are
available and effective for the system,
that system shall be entitled to a vari-
ance under the provisions of section
1415(a)(l)(A) of the Act. The Adminis-
trator's or primacy state's determina-
tion as to the availability and effec-
tiveness of such treatment methods
shall be based upon studies by the sys-
tem and other relevant information. If
a system submits information to dem-
onstrate that a treatment method is
not available and effective for fluoride
control for that system, the Adminis-
trator or primacy state shall make a
finding whether this information sup-
ports a decision that such treatment
method is not available and effective
for that system before requiring instal-
lation and/or use of such treatment
method.
(c) Pursuant to §142.43 (cHg) or cor-
responding state regulations, the Ad-
ministrator or primacy state that
issues variances shall issue a schedule
of compliance that may require the
system being granted the variance to
examine the following treatment meth-
ods (1) to determine the probability
that any of these methods will signifi-
cantly reduce the level of fluoride for
that system, and (2) if such probability
exists, to determine whether any of
these methods are technically feasible
and economically reasonable, and that
the fluoride reductions obtained will be
commensurate with the costs incurred
with the installation and use of such
treatment methods for that system:
(1) Modification of lime softening;
(2) Alum coagulation;
(3) Electrodialysis;
(4) Anion exchange resins;
(5) Well field management;
(6) Alternate source;
(7) Reglonalization,
(d) If the Administrator or primary
state that issues variances determines
that a treatment method identified in
§ 142.61(c) or other treatment method is
603
-------
§142.62
40 CFR Ch. i (7-1-04 Edition)
technically feasible, economically rea-
sonable, and will achieve fluoride re-
ductions commensurate with the costs
incurred with the installation and/or
use of such treatment method for the
system, the Administrator or primacy
state shall require the system to in-
stall and/or use that treatment method
in connection with a compliance sched-
ule issued under the provisions of sec-
tion 1415(a)(l)(A) of the Act. The Ad-
ministrator's or primacy state's deter-
mination shall be based upon studies
by the system and other relevant infor-
mation.
[51 PR 11411, Apr. 2, 1986]
Contaminant
§ 142.62 Variances and exemptions
from the maximum contaminant
levels for organic and inorganic
chemicals.
(a) The Administrator, pursuant to
section 1415(a)(l)(A) of the Act hereby
identifies the technologies listed in
paragraphs (a)(l) through (a)(54) of this
section as the best technology, treat-
ment techniques, or other means avail-
able for achieving compliance with the
maximum contaminant levels for or-
ganic chemicals listed in §141.61 (a) and
(c):
Best available technologies
PTA'
GAG 2
OX'
(1) Benzene X
(2) Carbon tetrachloride X
(3) 1,2-Dichloroethane , X
(4) Trichloroethylene X
(S) para-Dtehlorobenzene X
(6) 1,1-Dichloroethylene X
(7) 1,1,1-Trichloroethane X
(8) Vinyl chloride X
(9) cis-1,2-Dichloroethylene X
(10) 1,2-Oichloropropane X
(11) Ethylbenzene X
(12) Monochlorobanzene X
(13) o-Dichlarobenzene X
(14) Slyrene X
(15) Tetrachloroethylene X
(16) Toluene X
(17) trans-1,2-Diehloroethylene X
(18) Xyiense (total) X
(19) Alachlor
(20) Aldtaarb
{21) Aldiearb sulfoxide
(22) Aldiearb sulfone
(23) Atrazlne
(24) Carbofuran
(25) CNordane
(26) Dibromochlofopropane X
(27)2,4-0
(28) Ethylene dibromide X
(29) Heptachlor
(30) Heptachlor epoxide
(31) Lindane
(32) Methoxyohlor
(33)PCBs
(34) Pentachlorophenol
(35) Toxaphene
(36)2,4,5-TP
(37) Senzo(a]pyrene
(38) Dalapon
(38) Diohloromethane X
(40) Di(2-ethyihexyl)adipat8 X
(41) Di(2-ethythexyl)phthalate
(42)Dinoseb
(43)Diquat
(44) Endothall
(45) Endrin
(46) Glyphosate
(47) Hexachtorobenzene
(46) Hexaohtarocyolopentadlene X
(49) Oxamyl (Vydate)
(50) Picloram
(51) Simazine
604
-------
Environmental Protection Agency
§ 142.62
Contaminant
(52) 1,2,4-Trichlorobenzene
(53) 1,1,2-Trichloroethane
(54) 2,3,7,8-TCDD (Dloxin)
Best available technologies
PTA"
OX'
1 Packed Tower Aeration
2 Granular Activated Carbon
3 Oxidation (Chlorination or Ozonation)
(b) The Administrator, pursuant to
section 1415(a)(D(A) of the Act, hereby
identifies the following as the best
technology, treatment techniques, or
other means available for achieving
compliance with the maximum con-
taminant levels for the inorganic
chemicals listed in §141.62:
BAT FOR INORGANIC COMPOUNDS LISTED IN
§141.62(8)
Chemical name
Antimony
Arsenic4
Barium
Chromium
Cyanide
Mercury
Nickel
Nitrite
Nitrate
Thallium
BAT($)
2,7
5 1,2, 5, 6, 7.
9, 12
2,3,8
5,6,7,9
1 25,6,7
2567
2,5,6 =,7
5,7,10
2',4,6>,7"
5,6,7
5,7,9
5,7
1,2 ',6.7,9
1.5
' BAT only if influent Hg concentrations
2 BAT for Chromium ill only.
*BAT for Selenium IV only.
4 8ATs for Arsenic V. Pre-oxidation may be required to con-
vert Arsenic 111 to Arsenic V.
sTo obtain high removals, iron to arsenic ratio must be at
least 20:1.
Key to BATS in Table
l=Activated Alumina
2=Coagulatlon/FiltratIon (not BAT for sys-
tems <500 service connections)
3=Direct and Diatomite Filtration
4=Granular Activated Carbon
5=Ion Exchange
6=Lime Softening (not BAT for systems <500
service connections)
7=Reverse Osmosis
8=Corrosion Conti'ol
9=Electrodialysis
10=Ctlorine
ll=Ultra violet
12=Oxidation/Filtration
(c) A State shall require community
water systems and non-transient, non-
community water systems to install
and/or use any treatment method iden-
tified in §142.62 (a) and (b) as a condi-
tion for granting a variance except as
provided in paragraph (d) of this sec-
tion. If, after the system's installation
of the treatment method, the system
cannot meet the MOL, that system
shall be eligible for a variance under
the provisions of section 1415(a)(l)(A) of
the Act.
(d) If a system can demonstrate
through comprehensive engineering as-
sessments, which may include pilot
plant studies, that the treament meth-
ods identified in §142.62 (a) and (b)
would only achieve a de minimis reduc-
tion In contaminants, the State may
issue a schedule of compliance that re-
quires the system being granted the
variance to examine other treatment
methods as a condition of obtaining
the variance.
(e) If the State determines that a
treatment method identified In para-
graph (d) of this section is technically
feasible, the Administrator or primacy
State may require the system to in-
stall and/or use that treatment method
in connection with a compliance sched-
ule issued under the provisions of sec-
tion 1415(a)(l)(A) of the Act. The
State's determination shall be based
upon studies by the system and other
relevant information.
(f) The State may require a public
water system to use bottled water,
point-of-use devices, point-of-entry de-
vices or other means as a condition of
granting a variance or an exemption
from the requirements of §§141.61 (a)
and (c) and 141.62, to avoid an unrea-
sonable risk to health. The State may
require a public water system to use
bottled water and point-of-use devices
or other means, but not point-of-entry
devices, as a condition for granting an
exemption from corrosion control
treatment requirements for lead and
copper in §§141.81 and 141.82 to avoid an
unreasonable risk to health. The State
605
-------
§142.62
40 CFR Ch. I (7-1-04 Edition)
may require a public water system to
use point-of-entry devices as a condi-
tion for granting an exemption from
the source water and lead service line
replacement requirements for lead and
copper under §§141.83 or 141.84 to avoid
an unreasonable risk to health.
(g) Public water systems that use
bottled water as a condition for receiv-
ing a variance or an exemption from
the requirements of §§141.61 (a) and (c)
and 141.62, or an exemption from the
requirements of §§141.81-141.84 must
meet the requirements specified in ei-
ther paragraph (g)(l) or (g)(2) and para-
graph (g)(3) of this section:
(1) The Administrator or primacy
State must require and approve a mon-
itoring program for bottled water. The
public water system must develop and
put in place a monitoring program that
provides reasonable assurances that
the bottled water meets all MCLs. The
public water system must monitor a
representative sample of the bottled
water for all contaminants regulated
under §§ 141.61 (a) and (c) and 141.62 dur-
ing the first three-month period that it
supplies the bottled water to the pub-
lic, and annually thereafter. Results of
the monitoring program shall be pro-
vided to the State annually.
(2) The public water system must re-
ceive a certification from the bottled
water company that the bottled water
supplied has been taken from an "ap-
proved source" as defined in 21 CFR
129.3(a); the bottled water company has
conducted monitoring in accordance
with 21 CFR 129.60(9) (1) through (3);
and the bottled water does not exceed
any MOLs or quality limits as set out
in 21 CFR 103.35, part 110, and part 129.
The public water system shall provide
the certification to the State the first
quarter after it supplies bottled water
and annually thereafter. At the State's
option a public water system may sat-
isfy the requirements of this sub-
section if an approved monitoring pro-
gram is already in place in another
State.
(3) The public water system is fully
responsible for the provision of suffi-
cient quantities of bottled water to
every person supplied by the public
water system via door-to-door bottled
water delivery.
(h) Public water systems that use
point-of-use or point-of-entry devices
as a condition for obtaining a variance
or an exemption from NPDWRs must
meet the following requirements:
(1) It is the responsibility of the pub-
lic water system to operate and main-
tain the point-of-use and/or point-of-
entry treatment system.
(2) Before point-of-use or point-of-
entry devices are installed, the public
water system must obtain the approval
of a monitoring plan which ensures
that the devices provide health protec-
tion equivalent to that provided by
central water treatment.
(3) The public water system must
apply effective technology under a
State-approved plan. The micro-
biological safety of the water must be
maintained at all times.
(4) The State must require adequate
certification of performance, field test-
ing, and, if not included in the certifi-
cation process, a rigorous engineering
design review of the point-of-use and/or
point-of-entry devices.
(5) The design and application of the
point-of-use and/or point-of-entry de-
vices must consider the potential for
increasing concentrations of hetero-
trophic bacteria in water treated with
activated carbon. It may be necessary
to use frequent backwashing, post-con-
tactor disinfection, and Heterotrophie
Plate Count monitoring to ensure that
the microbiological safety of the water
is not compromised.
(6) The State must be assured that
buildings connected to the system have
sufficient point-of-use or point-of-entry
devices that are properly installed,
maintained, and monitored such that
all consumers will be protected.
(7) In requiring the use of a point-of-
entry device as a condition for grant-
ing an exemption from the treatment
requirements for lead and copper under
§§141.83 or 141.84, the State must be as-
sured that use of the device will not
cause increased corrosion of lead and
copper bearing materials located be-
tween the device and the tap that could
increase contaminant levels at the tap.
[56 FE 3596, Jan. 30, 1991, as amended at 56
PR 26563, June 7, 1991; 57 PR 31848, July 17,
1992; 59 PR 33864, June 30, 1994; 59 FR 34325,
July 1, 1994; 66FB 7066, Jan. 22, 2001]
606
-------
Environmental Protection Agency
§142.65
EFFECTIVE DATE NOTE: At 69 PR 38857, June
29, 2004. § 142.62 was amended by removing the
citation "103.35" and adding In its place
"165.110", effective July 29. 2004.
§ 142.63 Variances and exemptions
from the maximum contaminant
level for total coliforms.
(a) No variances or exemptions from
the maximum contaminant level in
§141.63 of this chapter are permitted.
(b) EPA has stayed the effective date
of this section relating to the total
coliform MOL of §141.63(a) of this chap-
ter for systems that demonstrate to
the State that the violation of the
total coliform MCL is due to a per-
sistent growth of total coliforms in the
distribution system rather than fecal
or pathogenic contamination, a treat-
ment lapse or deficiency, or a problem
in the operation or maintenance of the
distribution system.
[54 FB 27568, June 29, 1989, as amended at 56
FR 1557, Jan. 15, 1991]
§ 142.64 Variances and exemptions
from the requirements of part 141,
subpart H—Filtration and Disinfec-
tion.
fa) No variances from the require-
ments in part 141, subpart H are per-
mitted,
(b) No exemptions from the require-
ments in §141.72 (a)(3) and (b)(2) to pro-
vide disinfection are permitted,
[54 FR. 27540, June 29, 1989]
§ 142.63 Variances and exemptions
from the maximum contaminant
levels for radionuclides.
(a)(l) Variances and exemptions from
the maximum contaminant levels for
combined radium-226 and radium-228.
uranium, gross alpha particle activity
(excluding Radon and Uranium), and
beta particle and photon radioactivity.
(i) The Administrator, pursuant to
section 1415(a)(l)(A) of the Act, hereby
identifies the following as the best
available technology, treatment tech-
niques, or other means available for
achieving compliance with the max-
imum contaminant levels for the radio-
nuclides listed in §141.66(b), (c). (d), and
(e) of this chapter, for the purposes of
issuing variances and exemptions, as
shown in Table A to this paragraph.
TABLE A—BAT FOR RADIONUCLIDES LISTED IN
§141.66
Contaminant
Combined radium-226 and ra-
dium-228.
Uranium
Gross alpha particle activity
(excluding radon and ura-
nium).
Beta particle and photon ra-
dioactivity.
BAT
Ion exchange, reverse osmo-
sis, lime softening.
Ion exchange, reverse osmo-
sis, lime softening, coagu-
lation/filtration,
Reverse osmosis.
Ion exchange, reverse osmo-
sis.
(ill In addition, the Administrator
hereby identifies the following as the
best available technology, treatment
techniques, or other means available
for achieving compliance with the
maximum contaminant levels for the
radionuclides listed in §141.66Cb), (c).
(d), and (e) of this chapter, for the pur-
poses of issuing variances and exemp-
tions to small drinking water systems,
defined here as those serving 10,000 per-
sons or fewer, as shown in Table C to
this paragraph.
TABLE B—LIST OF SMALL SYSTEMS COMPLIANCE TECHNOLOGIES FOR RADIONUCLIDES AND
LIMITATIONS TO USE
Unit technologies
1. Ion exchange (IE)
2, Point of use (.POD2) IE
3. Reverse osmosis (RO) ..
4. POU2RO
5. Lime softening ., :
6, Green sand filtration I
1', Co-precipitation with barium sulfate ... j
B. Electrodtalysis/electrodialysis reversal \
9. Pre-forrned hydrous manganese
oxide filtration.
Limitations
(see foot-
notes)
: Operator skill level required 1
Raw water quality rang
considerations *
; Intermediate
| Basic
I Advanced
, Basic
Advanced
Basic.
Intermediate to Advanced .
Basic to intermediate
Intermediate
All ground waters.
All ground wafers.
Surface waters usually require pre-til-
tration.
Surface waters usually require pre-fil-
tration.
All waters.
Ground waters with suitable water
quality.
All ground waters.
All ground waters.
607
-------
§142.65
40 CFR Ch. 1 (7-1-04 Edition)
TABLE B—LIST OF SMALL SYSTEMS COMPLIANCE TECHNOLOGIES FOR RADIONUCLIDES AND
LIMITATIONS TO USE—Continued
Unit technologies
Limitations
(see foot-
notes)
(a) (H)
(!)
Operator skill level required1
Raw water quality range &
conside rations1
concentrations may affect regenera-
tion frequency.
ties.
1 National Research Council (NRC). Safe Water from Every Tap; Improving Water Service to Small Communities. National
Academy Press, Washington, D.C. 1997.
2 A POU, or "point-of-use" technology is a treatment device installed at a single tap used for the purpose of reducing contami-
nants in drinking water at that one tap. POU devices are typically installed at the kitchen tap. See the April 21, 2000 NGDA for
more details.
Limitations Footnotes: Technologies for Radionuclides;
aThe regeneration solution contains high concentrations of the contaminant tons. Disposal options should be carefully consid-
ered before choosing this technology,
DWhen POU devices are used tor compliance, programs for long-term operation, maintenance, and monitoring must be pro-
vided by water utility to ensure proper performance.
c Reject water disposal options should be carefully considered before choosing this technology. See other RO limitations de-
scribed in the SWTR compliance technologies table.
dThe combination of variable source water qualrty and the complexity of the water chemistry involved may make this tech-
nology too complex for small surface water systems.
9 Removal efficiencies can vary depending on water quality.
'This technology may be very limited in application to small systems. Since the process requires static mixing, detention ba-
sins, and fiilration, it is most applicable to systems with sufficiently high sulfate levels that already have a suitable filtration treat-
ment train in place,
sThis technology is most applicable to smali systems that already have filtration in place,
h Handling of chemicals required during regeneration and pH adjustment may be too difficult for small systems without an ade-
quately trained operator.
'Assumes modification to a coagulation/filtration process already in place,
TABLE C—BAT FOR SMALL COMMUNITY WATER SYSTEMS FOR THE RADIONUCLIDES LISTED IN
§141.66
Compliance technologies1 for system size categories (population served)
Combined radium-226 and radium-228
Uranium
1 25-500
1,2,3,4,3,6,7,8,9 .,
I 3, 4
.,, 1, 2, 3 4 ...
I 1,2,4, 10, 11
501-3,300
1,2, 3,4,5,6,7,8, 9 ..
3, 4
1234.
1,2, 3,4,5, 10, 11
3,300-10,000
1 2, 3, 4, 5, 6 7, 8, 9.
3, 4
1 2 3, 4
1,2, 3,4,5, 10, 11.
1 Note; Numbers correspond to those technologies found listed in the table B to this paragraph.
(2) A State shall require community
water systems to install and/or use any
treatment technology identified in
Table A to this section, or in the case
of small water systems (those serving
10,000 persons or fewer), Table B and
Table C of this section, as a condition
for granting a variance except as pro-
vided in paragraph (a)(3) of this sec-
tion. If, after the system's installation
of the treatment technology, the sys-
tem cannot meet the MCL, that system
shall be eligible for a variance under
the provisions of section 1415(a)(l)(A) of
the Act,
(3) If a community water system can
demonstrate through comprehensive
engineering assessments, which may
include pilot plant studies, that the
treatment technologies identified in
this section would only achieve a de
minimus reduction in the contaminant
level, the State may issue a schedule of
compliance that requires the system
being granted the variance to examine
other treatment technologies as a con-
dition of obtaining the variance.
(4) If the State determines that a
treatment technology identified under
paragraph (a)(3) of this section is tech-
nically feasible, the Administrator or
primacy State may require the system
to install and/or use that treatment
technology in connection with a com-
pliance schedule issued under the pro-
visions of section 1415(a)(l)(A) of the
Act. The State's determination shall be
based upon studies by the system and
other relevant information.
(5) The State may require a commu-
nity water system to use bottled water,
608
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Environmental Protection Agency
§142.76
point-of-use devices, point-of-entry de-
vices or other means as a condition of
granting a variance or an exemption
from the requirements of § 141.66 of this
chapter, to avoid an unreasonable risk
to health.
(6) Community water systems that
use bottled water as a condition for re-
ceiving- a variance or an exemption
from the requirements of §141.66 of this
chapter must meet the requirements
specified in either §142.62(g)(l) or
§142,62(g)(2)and(g)(3).
(7) Community water systems that
use point-of-use or point-of-entry de-
vices as a condition for obtaining a
variance or an exemption from the
radionuclides NPDWRs must meet the
conditions in §142.62(h)(l) through
(b) [Reserved]
[65 FR 78751, Dec. 7, 2000]
Subpart H— Indian Tribe$
SOURCE: 53 FR 37411, Sept. 26. 1988, unless
otherwise noted.
§142.72 Requirements for Tribal eligi-
bility.
The Administrator is authorized to
treat an Indian tribe as eligible to
apply for primary enforcement for the
Public Water System Program and the
authority to waive the mailing' require-
ments of §141.155(a) if it meets the fol-
lowing criteria:
(a) The Indian Tribe is recognized by
the Secretary of the Interior.
(b! The Indian Tribe has a tribal gov-
erning body which is currently "car-
rying out substantial governmental du-
ties and powers" over a defined area,
(i.e., is currently performing govern-
mental functions to promote the
health, safety, and welfare of the af-
fected population within a defined geo-
graphic area).
(c) The Indian Tribe demonstrates
that the functions to be performed in
regulating the public water systems
that the applicant intends to regulate
are within the area of the Indian Tribal
government's jurisdiction.
(d) The Indian Tribe is reasonably ex-
pected to be capable, in the Adminis-
trator's judgment, of administering (in
a manner consistent with the terms
and purposes of the Act and all applica-
ble regulations) an effective Public
Water System program.
[53 FR 37411, Sept, 26, 1988. as amended at 59
FE 643«. Dec. 14. 1994; 63 FR 44535. Aug. 19.
1998]
§142.76 Bequest by an Indian Tribe
for a determination of eligibility.
An Indian Tribe may apply to the Ad-
ministrator for a determination that it
meets the criteria of section 1451 of the
Act. The application shall be concise
and describe how the Indian Tribe will
meet each of the requirements of
§142.72. The application shall consist of
the following information:
(a) A statement that the Tribe is rec-
ognized by the Secretary of the Inte-
rior.
(b) A descriptive statement dem-
onstrating that the Tribal governing
body is currently carrying out substan-
tial governmental duties and powers
over a defined area. The statement
should:
(1) Describe the form of the Tribal
government;
(2) Describe the types of govern-
mental functions currently performed
by the Tribal governing body such as,
but not limited to, the exercise of po-
lice powers affecting (or relating to)
the health, safety, and welfare of the
affected population; taxation; and the
exercise of the power of eminent do-
main; and
(3) Identify the sources of the Tribal
government's authority to carry out
the governmental functions currently
being performed.
(c) A map or legal description of the
area over which the Indian Tribe as-
serts jurisdiction; a statement by the
Tribal Attorney General (or equivalent
official) which describes the basis for
the Tribe's jurisdictional assertion (in-
cluding the nature or subject matter of
the asserted jurisdiction); a copy of
those documents such as Tribal con-
stitutions, by-laws, charters, executive
orders, codes, ordinances, and/or reso-
lutions which the Tribe believes are
relevant to its assertions regarding ju-
risdiction; and a description of the lo-
cations of the public water systems the
Tribe proposes to regulate.
(d) A narrative statement describing
the capability of the Indian Tribe to
609
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§142.78
40 CFR Ch. I (7-1-04 Edition)
administer an effective Public Water
System program. The narrative state-
ment should include:
(1) A description of the Indian Tribe's
previous management experience
which may include, the administration
of programs and services authorized by
the Indian Self-Determination and
Education Assistance Act (25 TJ.S.C. 450
et seq.), the Indian Mineral Develop-
ment Act (25 U.S.C. 2101 et seq,), or the
Indian Sanitation Facilities Construc-
tion Activity Act (42 U.S.C. 2004a).
(2) A list of existing environmental
or public health programs adminis-
tered by the Tribal governing body and
a copy of related Tribal laws, regula-
tions and policies.
(3) A description of the Indian Tribe's
accounting and procurement systems.
(4) A description of the entity (or en-
tities) which exercise the executive,
legislative, and judicial functions of
the Tribal government.
(5) A description of the existing, or
proposed, agency of the Indian Tribe
which will assume primary enforce-
ment responsibility, including a de-
scription of the relationship between
owners/operators of the public water
systems and the agency.
(6) A description of the technical and
administrative capabilities of the staff
to administer and manage an effective
Public Water System Program or a
plan which proposes how the Tribe will
acquire additional administrative and/
or technical expertise. The plan must
address how the Tribe will obtain the
funds to acquire the additional admin-
istrative and technical expertise.
(e) The Administrator may, in his
discretion, request further documenta-
tion necessary to support a Tribe's eli-
gibility.
(f) If the Administrator has pre-
viously determined that a Tribe has
met the prerequisites that make it eli-
gible to assume a role similar to that
of a state as provided by statute under
the Safe Drinking Water Act, the Clean
Water Act, or the Clean Air Act, then
that Tribe need provide only that in-
formation unique to the Public Water
System program (paragraphs (c), (d)(5)
and (6) of this section).
[53 FR 37411, Sept. 26, 1988, as amended at 59
FR 64344, Dec. 14, 1994]
§142,78 Procedure for processing an
Indian Tribe's application.
(a) The Administrator shall process a
completed application of an Indian
Tribe in a timely manner. He shall
promptly notify the Indian Tribe of re-
ceipt of the application.
(b) A tribe that meets the require-
ments of §141.72 of this chapter is eligi-
ble to apply for development grants
and primacy enforcement responsi-
bility for a Public Water System Pro-
gram and associated funding under sec-
tion 1443(a) of the Act and for primary
enforcement responsibility for public
water systems under section 1413 of the
Act and for the authority to waive the
mailing requirement of §141.155(a) of
this chapter.
[53 FR 37411 Sept. 26, 1988, as amended at 59
FR 64345, Dec. 14, 1994; 63 FR 71376, Dec. 28,
1998]
Subpart I—Administrator's Review
of State Decisions that imple-
ment Criteria Under Which Fil-
tration Is Required
SOURCE: 54 FR 27540, June 29, 1989, unless
otherwise noted.
1142.80 Review procedures.
(a) The Administrator may initiate a
comprehensive review of the decisions
made by States with primary enforce-
ment responsibility to determine, in
accordance with § 141.71 of this chapter,
if public water systems using surface
water sources must provide filtration
treatment. The Administrator shall
complete this review within one year of
its initiation and shall schedule subse-
quent reviews as (s)he deems necessary.
(b) EPA shall publish notice of a pro-
posed review in the FEDERAL REGISTER.
Such notice must:
(1) Provide information regarding the
location of data and other information
pertaining to the review to be con-
ducted and other information including
new scientific matter bearing on the
application of the criteria for avoiding
filtration; and
(2) Advise the public of the oppor-
tunity to submit comments.
(c) Upon completion of any such re-
view, the Administrator shall notify
each State affected by the results of
610
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Environmental Protection Agency
§ 142.81
the review and shall make the results
available to the public.
§ 142.81 Notice to the State.
(a) If the Administrator finds
through periodic review or other avail-
able information that a State (1) has
abused its discretion in applying the
criteria for avoiding filtration under
§141.71 of this chapter in determining
that a system does not have to provide
filtration treatment, or (2) has failed to
prescribe compliance schedules for
those systems which must provide fil-
tration in accordance with section
1412(b)(7)(C)(ii) of the Act, (s)he shall
notify the State of these findings. Such
notice shall:
(1) Identify each public water system
for which the Administrator finds the
State has abused its discretion;
(2) Specify the reasons for the find-
ing;
(3) As appropriate, propose that the
criteria of §141.71 of this chapter be ap-
plied properly to determine the need
for a public water system to provide
filtration treatment or propose a re-
vised schedule for compliance by the
public water system with the filtration
treatment requirements;
(b) The Administrator shall also no-
tify the State that a public hearing is
to be held on the provisions of the no-
tice required by paragraph (a) of this
section. Such notice shall specify the
time and location of the hearing. If,
upon notification of a finding by the
Administrator that the State has
abused its discretion under §141.71 of
this chapter, the State takes corrective
action satisfactory to the Adminis-
trator, the Administrator may rescind
the notice to the State of a public
hearing.
(c) The Administrator shall publish
notice of the public hearing in the FED-
ERAL REGISTER and in a newspaper of
general circulation in the involved
State, including a summary of the find-
ings made pursuant to paragraph (a) of
this section, a statement of the time
and location for the hearing, and the
address and telephone number of an of-
fice at which interested persons may
obtain further information concerning
the hearing.
(d) Hearings convened pursuant to
paragraphs (b) and (c) of this section
shall be conducted before a hearing of-
ficer to be designated by the Adminis-
trator. The hearing shall be conducted
by the hearing officer in an informal,
orderly, and expeditious manner. The
hearing officer shall have the authority
to call witnesses, receive oral and writ-
ten testimony, and take such other ac-
tion as may be necessary to ensure the
fair and efficient conduct of the hear-
ing. Following the conclusion of the
hearing, the hearing officer may make
a recommendation to the Adminis-
trator based on the testimony pre-
sented at the hearing and shall forward
any such recommendation and the
record of the hearing to the Adminis-
trator.
(e) Within 180 days after the date no-
tice is given pursuant to paragraph (b)
of this section, the Administrator
shall:
(1) Rescind the notice to the State of
a public hearing if the State takes cor-
rective action satisfactory to the Ad-
ministrator; or
(2) Rescind the finding for which the
notice was given and promptly notify
the State of such rescission; or
(3) Uphold the finding for which the
notice was given. In this event, the Ad-
ministrator shall revoke the State's
decision that filtration was not re-
quired or revoke the compliance sched-
ule approved by the State, and promul-
gate, as appropriate, with any appro-
priate modifications, a revised filtra-
tion decision or compliance schedule
and promptly notify the State of such
action.
(f) Revocation of a State's filtration
decision or compliance schedule and/or
promulgation of a revised filtration de-
cision or compliance schedule shall
take effect 90 days after the State is
notified under paragraph (e)(3) of this
section,
Subpart J [Reserved]
Subpart K—Variances for Small
System
SOURCE: 63 FR 43848, Au.gr. 14, 1998, unless
otherwise noted.
611
-------
§142.301
40 CFR Ch. 1 (7-1-04 Edition)
GENERAL PROVISIONS
§142.301 What is a small system vari-
ance?
Section 1415(e) of the Act authorizes
the issuance of variances from the re-
quirement to comply with a maximum
contaminant level or treatment tech-
nique to systems serving fewer than
10,000 persons. The purpose of this sub-
part is to provide the procedures and
criteria for obtaining these variances.
The regulations in this subpart shall
take effect on September 14, 1998.
i 142.302 Who can issue a small system
variance?
A small system variance under this
subpart may only be Issued by either:
(a) A State that is exercising primary
enforcement responsibility under Sub-
part B for public water systems under
the State's jurisdiction; or
(b) The Administrator, for a public
water system in a State which does not
have primary enforcement responsi-
bility.
§ 142.303 Which size public water sys-
tems can receive a small system
variance?
(a) A State exercising primary en-
forcement responsibility for public
water systems (or the Administrator
for other systems) may grant a small
system variance to public water sys-
tems serving 3,300 or fewer persons.
(b) With the approval of the Adminis-
trator pursuant to §142.312, a State ex-
ercising primary enforcement responsi-
bility for public water systems may
grant a small system variance to pub-
lic water systems serving more than
3,300 persons but fewer than 10,000 per-
sons.
(c) In determining the number of per-
sons served by the public water system,
the State or Administrator must in-
clude persons served by consecutive
systems. A small system variance
granted to a public water system would
also apply to any consecutive system
served by it.
§ 142.304 For which of the regulatory
requirements is a small system vari-
ance available?
(a) A small system variance is not
available under this subpart for a na-
tional primary drinking water regula-
tion for a microbial contaminant (in-
cluding a bacterium, virus, or other or-
ganism) or an indicator or treatment
technique for a microbial contaminant.
(b) A small system variance under
this subpart is otherwise only available
for compliance with a requirement
specifying a maximum contaminant
level or treatment technique for a con-
taminant with respect to which;
(1) a national primary drinking water
regulation was promulgated on or after
January 1,1986; and
(2) the Administrator has published a
small system variance technology pur-
suant to Section 1412(b)(15) of the Act,
NOTE TO PARAGRAPH (B)(l): Small system
variances are not available for public water
systems above the pre-1986 maximum con-
taminant level even if subsequently revised.
If the Agency revises a pre-1986 maximum
contaminant level and makes it more strin-
gent, then a variance would be available for
that contaminant, but only up to the pre-
1986 maximum contaminant level,
§142.305 When can a small system
variance be granted by a State?
No small system variance can be
granted by a State until the later of
the following:
(a) 90 days after the State proposes to
grant the small system variance;
(b) If a State is proposing to grant a
small system variance to a public
water system serving 3,300 or fewer per-
sons and the Administrator objects to
the small system variance, the date on
which the State makes the rec-
ommended modifications or responds
in writing to each objection; or
(c) If a State is proposing to grant a
small system variance to a public
water system serving a population
more than 3,300 and fewer than 10,000
persons, the date the Administrator ap-
proves the small system variance. The
Administrator must approve or dis-
approve the variance within 90 days
after it is submitted to the Adminis-
trator for review.
612
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Environmental Protection Agency
§ 142.307
REVIEW OF SMALL SYSTEM VARIANCE
APPLICATION
§ 142.306 What are the responsibilities
of the public water system, State
and the Administrator in ensuring
that sufficient information is avail-
able and for evaluation of a small
system variance application?
(a) A public water system requesting
a small system variance must provide
accurate and correct information to
the State or the Administrator to issue
a small system variance in accordance
with this subpart. A State may assist a
public water system in compiling infor-
mation required for the State or the
Administrator to issue a small system
variance in accordance with this sub-
part.
(b) Based upon an application for a
small system variance and other infor-
mation, and before a small system
variance may be proposed under this
subpart, the State or the Adminis-
trator must find and document the fol-
lowing:
(1) The public water system is eligi-
ble for a small system variance pursu-
ant to §§142.303 (i.e., the system serves
a population of fewer than 10,000 per-
sons) and 142.304 (i.e., the contaminant
for which the small system variance is
sought is not excluded from variance
eligibility);
(2) The public water system cannot
afford to comply, in accordance with
the ai'fordability criteria established
by the State (or by the Administrator
in States which do not have primary
enforcement responsibility), with the
national primary drinking water regu-
lation for which a small system vari-
ance is sought, including by:
(i) Treatment:
(ii) Alternative sources of water sup-
ply;
(Hi) Restructuring- or consolidation
changes, including ownership change
and/or physical consolidation with an-
other public water system; or
(iv) Obtaining financial assistance
pursuant to Section 1452 of the Act or
any other Federal or State program;
(3) The public water system meets
the source water quality requirements
for installing the small system vari-
ance technology developed pursuant to
guidance published under section
1412(b)(15) of the Act;
(4) The public water system is finan-
cially and technically capable of in-
stalling, operating and maintaining the
applicable small system variance tech-
nology; and
(5) The terms and conditions of the
small system variance, as developed
through compliance with §142.307, en-
sure adequate protection of human
health, considering the following:
(i) The quality of the source water
for the public water system; and
(ii) Removal efficiencies and expected
useful life of the small system variance
technology.
§ 142.307 What terms and conditions
must be included in a small system
variance?
(a) A State or the Administrator
must clearly specify enforceable terms
and conditions of a small system vari-
ance,
(b) The terms and conditions of a
small system variance issued under
this subpart must include, at a min-
imum, the following requirements:
(1) Proper and effective installation,
operation and maintenance of the ap-
plicable small system variance tech-
nology in accordance with guidance
published by the Administrator pursu-
ant to section 1412(b)(15) of the Act,
taking into consideration any relevant
source water characteristics and any
other site-specific conditions that may
affect proper and effective operation
and maintenance of the technology;
(2) Monitoring requirements, for the
contaminant for which a small system
variance is sought, as specified in 40
CPR part 141; and
(3) Any other terms or conditions
that are necessary to ensure adequate
protection of public health, which may
include:
(i) Public education requirements;
and
(ii) Source water protection require-
ments.
(c) The State or the Administrator
must establish a schedule for the pub-
lic water system to comply with the
terms and conditions of the small sys-
tem variance which must include, at a
minimum, the following requirements;
(1) Increments of progress, such as
milestone dates for the public water
613
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§142,308
40 CFR Ch. I (7-1-04 Edition)
system to apply for financial assist-
ance and begin capital improvements;
(2) Quarterly reporting to the State
or Administrator of the public water
system's compliance with the terms
and conditions of the small system
variance;
(3) Schedule for the State or the Ad-
ministrator to review the small system
variance under paragraph (d) of this
section; and
(4) Compliance with the terms and
conditions of the small system vari-
ance as soon as practicable but not
later than 3 years after the date on
which the small system variance is
granted. The Administrator or State
may allow up to 2 additional years if
the Administrator or State determines
that additional time is necessary for
the public water system to:
(i) Complete necessary capital im-
provements to comply with the small
system variance technology, secure an
alternative source of water, or restruc-
ture or consolidate; or
(ii) Obtain financial assistance pro-
vided pursuant to section 1452 of the
Act or any other Federal or State pro-
gram.
(d) The State or the Administrator
must review each small system vari-
ance granted not less often than every
5 years after the compliance date es-
tablished in the small system variance
to determine whether the public water
system continues to meet the eligi-
bility criteria and remains eligible for
the small system variance and is com-
plying with the terms and conditions of
the small system variance. If the pub-
lic water system would no longer be el-
igible for a small system variance, the
State or the Administrator must deter-
mine whether continuing the variance
is in the public interest. If the State or
the Administrator finds that con-
tinuing the variance is not in the pub-
lic interest, the variance must be with-
drawn.
PUBLIC PARTICIPATION
§142.308 What public notice is re-
quired before a State or the Admin-
istrator proposes to issue a small
system variance?
(a) At least fifteen (15) days before
the date of proposal, and at least thirty
(30) days prior to a public meeting to
discuss the proposed small system vari-
ance, the State, Administrator, or pub-
lic water system as directed by the
State or Administrator, must provide
notice to all persons served by the pub-
lic water system. For billed customers,
identified in paragraph (a)(l) of this
section, this notice must include the
information listed in paragraph (c) of
this section. For other persons regu-
larly served by the system, identified
in paragraph (a)(2) of this section, the
notice shall include the information
identified in paragraph (d) of this sec-
tion. Notice must be provided to all
persons served by;
(1) Direct mail or other home deliv-
ery to billed customers or other service
connections, and
(2) Any other method reasonably cal-
culated to notify, in a brief and concise
manner, other persons regularly served
by the system. Such methods may in-
clude publication in a local newspaper,
posting in public places or delivery to
community organizations.
(b) At the time of proposal, the State
must publish a notice in the State
equivalent to the FEDERAL REGISTER or
a newspaper or newspapers of wide cir-
culation in the State, or, in the case of
the Administrator, in the FEDERAL
REGISTER, This notice shall include the
information listed in paragraph (c) of
this section.
(c) The notice in paragraphs (a)(l)
and (b) of this section must include, at
a minimum, the following:
(1) Identification of the
contaminant[s] for which a small sys-
tem variance is sought;
(2) A brief statement of the health ef-
fects associated with the
contaminant[s] for which a small sys-
tem variance is sought using language
in Appendix C of Part 141 Subpart O of
this chapter;
(3) The address and telephone number
at which interested persons may obtain
further information concerning the
contaminant and the small system
variance;
(4) A brief summary, in easily under-
standable terms, of the terms and con-
ditions of the small system variance;
(5) A description of the consumer pe-
tition process under §142.310 and infor-
mation on contacting the EPA Re-
gional Office;
614
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Environmental Protection Agency
§142.311
(6) a brief statement announcing the
public meeting required under
§142.309(a), including a statement of
the purpose of the meeting, informa-
tion regarding the time and location
for the meeting, and the address and
telephone number at which interested
persons may obtain further informa-
tion concerning the meeting; and
(7) In communities with a large pro-
portion of non-English-speaking resi-
dents, as determined by the primacy
agency, information in the appropriate
language regarding the content and im-
portance of the notice.
(d) The notice in paragraph (a)(2) of
this section must provide sufficient in-
formation to alert readers to the pro-
posed variance and direct them where
to receive additional information.
(e) At its option, the State or the Ad-
ministrator may choose to issue sepa-
rate notices or additional notices re-
lated to the proposed small system
variance, provided that the require-
ments in paragraphs (a) through (d) of
this section are satisfied.
(f) Prior to promulgating the final
variance, the State or the Adminis-
trator must respond in writing to all
significant public comments received
relating to the small system variance.
Response to public comment and any
other documentation supporting the
issuance of a variance must be made
available to the public after final pro-
mulgation.
§142.309 What are the public meeting
requirements associated with the
proposal of a small system vari-
ance?
(a) A State or the Administrator
must provide for at least one (1) public
meeting on the small system variance
no later than 15 days after the small
system variance is proposed.
(b) At the time of the public meeting,
the State or Administrator must pre-
pare and make publicly available, in
addition to the information listed in
§142.308(c), either:
(1) The proposed small system vari-
ance, if the public meeting occurs after
proposal of the small system variance;
or
(2) A draft of the proposed small sys-
tem variance, if the public meeting oc-
curs prior to proposal of the proposed
small system variance.
(c) Notice of the public meeting must
be provided in the manner required
under §142.308 at least 30 days in ad-
vance of the public meeting. This no-
tice must be provided by the State, the
Administrator, or the public water sys-
tem as directed by the State or Admin-
istrator.
§142.310 How can a person served by
the public water system obtain EPA
review of a State proposed small
system variance?
(a) Any person served by the public
water system may petition the Admin-
istrator to object to the granting of a
small system variance within 30 days
after a State proposes to grant a small
system variance for a public water sys-
tem,
(b) The Administrator must respond
to a petition filed by any person served
by the public water system and deter-
mine whether to object to the small
system variance under §142.311, no
later than 60 days after the receipt of
the petition.
EPA REVIEW AND APPROVAL OF SMALL
SYSTEM VARIANCES
§142.311 What procedures allow the
Administrator to object to a pro-
posed small system variance or
overturn a granted small system
variance for a public water system
serving 3,300 or fewer persons?
(a) At the time a State proposes to
grant a small system variance under
this subpart, the State must submit to
the Administrator the proposed small
system variance and all supporting in-
formation, including' any written pub-
lic comments received prior to pro-
posal.
(b) The Administrator may review
and object to any proposed small sys-
tem variance within 90 days of receipt
of the proposed small system variance.
The Administrator must notify the
State in writing of each basis for the
objection and propose a modification
to the small system variance to resolve
the concerns of the Administrator. The
State must make the recommended
modification, respond in writing to
615
-------
§142.312
40 CFR Ch. I (7-1-04 Edition)
each objection, or withdraw the pro-
posal to grant the small system vari-
ance.
(c) If the State issues the small sys-
tem variance without resolving the
concerns of the Administrator, the Ad-
ministrator may overturn the State de-
cision to grant the variance if the Ad-
ministrator determines that the State
decision does not comply with the Act
or this rule.
§ 142.312 What EPA action is necessary
when a State proposes to grant a
small system variance to a public
water system serving a population
of more than 3,300 and fewer than
10,000 persons?
(a) At the time a State proposes to
grant a small system variance to a
public water system serving a popu-
lation of more than 3,300 and fewer
than 10,000 persons, the State must
submit the proposed small system vari-
ance and all supporting information,
including public comments received
prior to proposal, to the Adminis-
trator.
(b) The Administrator must approve
or disapprove the small system vari-
ance within 90 days of receipt of the
proposed small system variance and
supporting information. The Adminis-
trator must approve the small system
variance if it meets each requirement
within the Act and this rule.
(c) If the Administrator disapproves
the small system variance, the Admin-
istrator must notify the State in writ-
ing of the reasons for disapproval and
the small system variance does not be-
come effective. The State may resub-
mit the small system variance for re-
view and approval with modifications
to address the objections stated by the
Administrator.
§142,313 How will the Administrator
review a State's program under this
subpart?
(a) The Administrator must periodi-
cally review each State program under
this subpart to determine whether
small system variances granted by the
State comply with the requirements of
the Act, this rule and the affordability
criteria developed by the State.
(b) If the Administrator determines
that small system variances granted by
a State are not in compliance with the
requirements of the Act, this rule or
the affordability criteria developed by
the State, the Administrator shall no-
tify the State in writing of the defi-
ciencies and make public the deter-
minations.
(c) The Administrator's review will
be based in part on quarterly reports
prepared by the States pursuant to
§142.15(a)(l) relating to violations of in-
crements of progress or other violated
terms or conditions of small system
variances.
PART 143—NATIONAL SECONDARY
DRINKING WATER REGULATIONS
Sec.
143.1 Purpose.
143.2 Definitions.
143.3 Secondary maximum contaminant lev-
els.
143.4 Monitoring.
AUTHORITY: 42 U.S.C. 300f et aeq.
SOUBCB: 44 PR 42198, July 19, 1978, unless
otherwise noted.
§ 143.1 Purpose.
This part establishes National Sec-
ondary Drinking Water Regulations
pursuant to section 1412 of the Safe
Drinking Water Act, as amended (42
U.S.C. 300gr-l). These regulations con-
trol contaminants in drinking water
that primarily affect the aesthetic
qualities relating to the public accept-
ance of drinking water. At consider-
ably higher concentrations of these
contaminants, health implications
may also exist as well as aesthetic deg-
radation. The regulations are not Fed-
erally enforceable but are intended as
guidelines for the States.
§ 143.2 Definitions.
(a) Act means the Safe Drinking
Water Act as amended (42 U.S.C. 300f et
seq.).
(b) Contaminant means any physical,
chemical, biological, or radiological
substance or matter in water.
(c) Public water system means a sys-
tem for the provision to the public of
piped water for human consumption, if
such a system has at least fifteen serv-
ice connections or regularly serves an
average of at least twenty-five individ-
uals daily at least 60 days out of the
616
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Environmental Protection Agency
§143,4
year. Such term Includes (1) any collec-
tion, treatment, storage, and distribu-
tion facilities under control of the op-
erator of such system and used pri-
marily in connection with such system,
and (2) any collection or pretreatment
storage facilities not under such con-
trol which are used primarily in con-
nection with such system. A public
water system is either a "community
water system" or a "non-community
water system."
(d) State means the agency of the
State or Tribal government which has
jurisdiction over public water systems.
During any period when a State does
not have responsibility pursuant to
section 1443 of the Act, the term
"State" means the Regional Adminis-
trator, U.S. Environmental Protection
Agency.
(e) Supplier of water means any person
who owns or operates a public water
system.
(f) Secondary maximum contaminant
levels means SMOLs which apply to
public water systems and which, in the
judgement of the Administrator, are
requisite to protect the public welfare.
The SMCL means the maximum per-
missible level of a contaminant in
water which is delivered to the free
flowing outlet of the ultimate user of
public water system. Contamimants
added to the water under cir-
cumstances controlled by the user, ex-
cept those resulting from corrosion of
piping and plumbing' caused by water
quality, are excluded from this defini-
tion.
[44 FB 42198, July 19, 1979, as amended at 53
FB 37412, Sept. 26, 1988]
§143.3 Secondary maximum contami-
nant levels,
The secondary maximum contami-
nant levels for public water systems
are as follows:
Contaminant
Contaminant
Aluminum ...
Chloride
Color
Copper
Corrosivity ,,
Fluoride
Level
0.05 to 0.2 mg/l.
250 mg/1.
15 color units.
1.0 mg/l.
Non-corrosive,
2-0 mg/l.
Foaming agents
Iron
Manganese
Odor
pH
Silver
Sulfate
Total dissolved solids (IDS)
Zinc
Level
0.5 mg/l.
0.3 mg/l.
0.05 mg/l.
3 threshold odor number.
6.5-8.5.
0.1 mgfl.
250 mg/l.
500 mg/l.
5 mg/l.
These levels represent reasonable goals
for drinking water quality. The States
may establish higher or lower levels
which may be appropriate dependent
upon local conditions such as unavail-
ability of alternate source waters or
other compelling factors, provided that
public health and welfare are not ad-
versely affected.
[44 PR 42198, July 19, 1979, as amended at 51
PR 11412, Apr. 2, 1986: 56 FR 3597, Jan. 30,
1991]
§ 143.4 Monitoring.
(a) It is recommended that the pa-
rameters in these regulations should be
monitored at intervals no less frequent
than the monitoring performed for in-
organic chemical contaminants listed
in the National Interim Primary
Drinking Water Regulations as applica-
ble to community water systems. More
frequent monitoring would be appro-
priate for specific parameters such as
pH, color, odor or others under certain
circumstances as directed by the State.
(b) Measurement of pH, copper and
fluoride to determine compliance under
§143.3 may be conducted with one of
the methods in §141.23(k)(l). Analyses
of aluminum, chloride, foaming agents,
iron, manganese, odor, silver, sulfate,
total dissolved solids (TDS) and zinc to
determine compliance under § 143.3 may
be conducted with the methods in the
following table. Criteria for analyzing
aluminum, copper, iron, manganese,
silver and zinc samples with digestion
or directly without digestion, and
other analytical test procedures are
contained in Technical Notes on Drink-
ing Water Methods, EPA-600/B-94-173,
October 1994, which is available at
NTIS PB95-104766.
Contaminant
1. Aluminum
EPA
200.72
ASTM3
SM4
18th and 19th
ed.
3120 B
SM4
20th ed.
3120 B.
Other
617
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Pt. 144
40 CFR Ch. I (7-1-04 Edition)
Contaminant
2 Chloride
3 Color .. .....
5, Iron
7 Odor ...
8. Silver
9 Sulfate
10 Tata! Dissolved Solids
11 Zinc
EPA
200 B2
200.9=
300 O1
200.7=
200.92
2007s
200 82 ..
200. 92
200.72
200.82
200.92
300 O1
375.21
200 7 2
200.82
ASTM3
D4327-97
D512-89B
D4327-97
D516-90
SM-
18th and 19th
ed.
3113 B
3111 D.
4110 B
4500-CI" D
4500-CI- B
2120 B
5540 C
3120 B
3111 B.
3113 B.
3120 B
3111 B
3113 B.
2150 B
3120 B
3111 B.
3113 B
4110 B
4SOO-SQ,2- F
4500-SCV-C,
D.
4500-SCV- E
2540 C
3120 B
3111 B.
SM"
20th ed.
4110 B
4500 — C|- D
4500-CI- B.
2120 B
5540 C
3120 B.
3120 B
2150 B
3120 B
4110 B
4500-SOi'- F.
4500-SCM^C,
D.
4500-SO,,2" E.
2540 C
3120 B
Other
I-3720-855
The procedures shall be done In accordance with the documents listed below. The incorporation by reference of the following
documents was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies
of the documents may be obtained from the sources listed below. Information regarding obtaining these documents can be ob-
tained from the Safe Drinking Water Hotline at 800-426-4781. Documents may be inspected at EPA's Drinking Water Docket,
EPA West, 1301 Constitution Avenue, NW, Room B135, Washington, DC (Telephone: 202-566-2426); or at the National Ar-
chives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or
goto: http://www.2rchjves.gov/federal_register/code_of_federa/ mgulatsons/ibr locations.html.
1 "Methods for the Determination of Inorganic Substances irPEnvironmentarSamples", EPA/600/R-93-100, August 1993.
Available at NTIS, PB94-120821.
2 "Methods for the Determination of Metals in Environmental Samples—Supplement P, EPA/600/R-04-111, May 1994. Avail-
able at NTIS, PB 95-126472.
3 Annual Book of ASTM Standards, 1994, 1996, or 1999, Vols. 11.01 and 11.02, ASTM International; any year containing the
cited version of the method may be used. Copies may be obtained from ASTM International, 100 Barr Harbor Drive, West
Conshohocken, PA 19428. sa
••Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition
(1998), American Public Health Association, 1015 Fifteenth Street, NW, Washington, DC 20005. The cited methods published in
any of these three editions may be used, except that the versions of 3111 B, 3111 D, and 3113 B in the 20fh edrtion may not be
used.
5 Method I-372G-85, Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd
ed., 1989; Available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.
[44 PB 42198. July 19, 1979, as amended at 53 PR 5147, Feb. 19, 1988; 58 FR 30281, July 1, 1991;
59 PR 62470, Bee. 5, 1994; 64 PB 67466, Deo. 1, 1999; 67 FR 65252. Oct. 23, 2002: 69 PR 18803, Apr.
9, 2004]
PART 144—UNDERGROUND
INJECTION CONTROL PROGRAM
Subpart A—General Provisions
Sec.
144.1 Purpose and scope of part 144.
144.2 Promulgation of Class II programs for
Indian lands.
144.3 Definitions.
144.4 Considerations under Federal law.
144.5 Confidentiality of information.
144.6 Classification of wells.
144.7 Identification of underground sources
of drinking water and exempted aquifers.
144.8 Noncompliance and program reporting
by the Director.
Subpart B—General Program Requirements
144.11 Prohibition of unauthorized injec-
tion.
144.12 Prohibition of movement of fluid into
underground sources of drinking water.
144.13 Prohibition of Class IV wells.
144.14 Requirements for wells injecting haz-
ardous waste.
144.15 [Reserved]
144.16 Waiver of requirement by Director.
144.17 Records.
Subpart C—Authorization of Underground
Injection by Rule
144.21 Existing Class I, II (except enhanced
recovery and hydrocarbon storage) and
III wells.
618
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Environmental Protection Agency
§144.1
144,22 Existing Class II enhanced recovery
and hydrocarbon storage wells.
144,23 Class IV wells.
144.24 Class V wells.
144.25 Requiring a permit.
144.26 Inventory requirements.
144.27 Requiring other information.
144.28 Requirements for Class I, II, and III
wells authorized by rule.
Subpart D—Authorization by Permit
144.31 Application for a permit; authoriza-
tion by permit.
144.32 Signatories to permit applications
and reports.
144.33 Area permits.
144.34 Emergency permits.
144.35 Effect of a. permit.
144.36 Duration of permits.
144.37 Continuation of expiring permits,
144.38 Transfer of permits.
144.39 Modification or revocation and
reissuance of permits.
144.40 Termination of permits.
144.41 Minor modifications of permits.
Subpart E—Permit Conditions
144,51 Conditions applicable to all permits,
144.52 Establishing permit conditions.
144.53 Schedule of compliance.
144.54 Requirements for recording and re-
porting of monitoring results.
144.55 Corrective action.
Subpart F—Financial Responsibility: Class I
Hazardous Waste Injection Weils
144.60 Applicability,
144.61 Definitions of terms as used in this
subpart.
144.62 Cost estimate for plugging and aban-
donment.
144.63 Financial assurance for plugging and
abandonment.
144.64 Incapacity of owners or operators,
guarantors, or financial institutions.
144.65 Use of State-required mechanisms.
144.66 State assumption of responsibility,
144,70 Wording of the instruments.
Subpart G—Requirements (or Owners and
Operators ot Class V Injection Wells
144.79 General.
DEFINITION OP CLASS V INJECTION WILLS
144.80 What is a Class V injection well?
144.81 Does this subpart apply to me?
REQUIREMENTS FOE ALL CLASS V INJECTION
WELLS
144.82 What must I do to protect under-
ground sources of drinking water?
144.83 Do I need to notify anyone about my
Class V injection well?
144.84 Do I need to get a permit?
ADDITIONAL REQUIREMENTS FOR CLASS V
LARGE-CAPACITY CESSPOOLS AND MOTOB
VEHICLE WASTE DISPOSAL WELLS
144.85 Do these additional requirements
apply to me?
144,86 What are the definitions I need to
know?
144.87 How does the identification of ground
water protection areas and other sen-
sitive areas affect me?
144.88 What are the additional require-
ments?
144.89 How do I close my Class V injection
well?
AUTHORITY: Safe Drinking Water Act, 42
U.S.C. 300f et seq; Resource Conservation and
Recovery Act, 42 U.S.C. 6901 et seq.
SOURCE: 48 FR 14189, Apr. 1, 1983, unless
otherwise noted.
Subpart A—General Provisions
§ 144.1 Purpose and scope of part 144.
(a) Contents of part 144. The regula-
tions in this part set forth require-
ments for the Underground Injection
Control (UIC) program promulgated
under Part C of the Safe Drinking
Water Act (SDWA) (Pub. L. 93-523, as
amended; 42 U.S.C. 300f et seq,) and, to
the extent that they deal with haz-
ardous waste, the Resource Conserva-
tion and Recovery Act (RCRA) (Pub. L.
94-580 as amended; 42 U.S.C. 6901 et
seq.},
(b) Applicability. (1) The regulations
in this part establish minimum re-
quirements for UIC programs. To the
extent set forth in part 145, each State
must meet these requirements in order
to obtain primary enforcement author-
ity for the UIC program in that State.
(2) In addition to serving as min-
imum requirements for UIC programs,
the regulations in this part constitute
a part of the UIC program for States
listed in part 147 to be administered di-
rectly by EPA.
(c) The information requirements lo-
cated in the following sections have
been cleared by the Office of Manage-
ment and Budget: Sections 144.11,
144.28(c)(d)(i), 144.31, 14.33, 144.51(j)(m)
(n), 144.52(a), 144.54, 144.55, 144.15. 144.23,
144.26, 144.27, 144.28(i)(k), 144.51(o),
146.52. The OMB clearance number is
2040-0042.
619
-------
§144.1
40 CFR Ch. 1 (7-1-04 Edition)
(d) Authority. (1) Section 1421 of
SDWA requires the Administrator to
promulgate regulations establishing
minimum requirements for effective
UIC programs,
(2) Section 1422 of SDWA requires the
Administrator to list in the FEDERAL
REGISTER "each State for which in his
judgment a State underground injec-
tion control program may be necessary
to assure that underground injection
will not endanger drinking water
sources" and to establish by regulation
a program for EPA administration of
TJIO programs in the absence of an ap-
proved State program in a listed State,
(3) Section 1423 of SDWA provides
procedures for EPA enforcement of UIC
requirements.
(4) Section 1431 authorizes the Ad-
ministrator to take action to protect
the health of persons when a contami-
nant which is present in or may enter
a public water system or underground
source of drinking water may present
an imminent and substantial endanger-
ment to the health of persons.
(5) Section 1445 of SDWA authorizes
the promulgation of regulations for
such recordkeeping, reporting, and
monitoring requirements "as the Ad-
ministrator may reasonably require
* * * to assist him in establishing regu-
lations under this title," and a "right of
entry and inspection to determine com-
pliance with this title, including for
this purpose, inspection, at reasonable
time, or records, files, papers, proc-
esses, controls, and facilities * * *,"
(6) Section 1450 of SDWA authorizes
the Administrator "to prescribe such
regulations as are necessary or appro-
priate to carry out his functions" under
SDWA.
(e) Overview of the UIC program. An
TJIO program is necessary in any State
listed by EPA under section 1422 of the
SDWA. Because all States have been
listed, the SDWA requires all States to
submit an UIC program within 270 days
after July 24, 1980, the effective date of
40 CFR part 146, which was the final
element of the UIC minimum require-
ments to be originally promulgated.
unless the Administrator grants an ex-
tension, which can be for a period not
to exceed an additional 270 days. If a
State fails to submit an approvable
program, EPA will establish a program
for that State. Once a program is es-
tablished, SDWA provides that all un-
derground injections in listed States
are unlawful and subject to penalties
unless authorized by a permit or a rule.
This part sets forth the requirements
governing all UIC programs, authoriza-
tions by permit or rule and prohibits
certain types of injection. The tech-
nical regulations governing these au-
thorizations appear in 40 CFR part 146.
(f) Structure of the UIC program—(1)
Part 144. This part sets forth the per-
mitting and other program require-
ments that must be met by UIC Pro-
grams, whether run by a State or by
EPA. It is divided into the following
subparts:
(i) Subpart A describes general ele-
ments of the program, including defini-
tions and classifications.
(ii) Subpart B sets forth the general
program requirements, including the
performance standards applicable to all
injection activities, basic elements
that all UIC programs must contain,
and provisions for waiving permit of
rule requirements under certain cir-
cumstances.
(iii) Subpart C sets forth require-
ments for wells authorized by rule.
(iv) Subpart D sets forth permitting
procedures.
(v) Subpart E sets forth specific con-
ditions, or types of conditions, that
must at a minimum be included in all
permits.
(vi) Subpart F sets forth the financial
responsibility requirements for owners
and operators of all existing and new
Class I hazardous waste injection wells,
(vii) Subpart G of this part sets forth
requirements for owners and operators
of Class V injection wells.
(2) Part 145. While part 144 sets forth
minimum requirements for all UIC
Programs, these requirements are spe-
cifically identified as elements of a
State application for primacy to ad-
minister an UIC Program in part 145.
Part 145 also sets forth the necessary
elements of a State submission and the
procedural requirements for approval
of State programs.
(3) Part 124. The public participation
requirements that must be met by UIC
Programs, whether administered by
the State or by EPA, are set forth in
part 124, EPA must comply with all
620
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§144.2
40 CFR Ch. 1 (7-1-04 Edition)
apply to injections of hazardous wastes
into aquifers or portions thereof which
have been exempted pursuant to
§146.04.
(h) Interim Status under RCRA for
Class I Hazardous Waste Injection Wells.
The minimum national standards
which define acceptable injection of
hazardous waste during the period of
interim status under RCRA are set out
in the applicable provisions of this
part, parts 146 and 147, and §265.430 of
this chapter. The issuance of a UIC per-
mit does not automatically terminate
BORA interim status. A Class I well's
interim status does, however, auto-
matically terminate upon issuance to
that well of a RCRA permit, or upon
the well's receiving a BORA permit-by-
rule under §270.60(b) of this chapter.
Thus, until a Class I well injecting haz-
ardous waste receives a RCRA permit
or RCRA permit-by-rale, the well's
interim status requirements are the
applicable requirements imposed
pursuant to this part and parts 146, 147,
and 265 of this chapter, including any
requirements imposed in the UIC per-
mit.
[48 FR 14189, Apr. 1, 1983. as amended at 49
FR 20181, May 11, 1984; 52 PR 20676, June 2,
1987; 52 PR 45797, Dec. 1. 1887; 53 PK 28147,
July 26, 1988: 64 PR 68565, Dec. 7, 1999: 67 FR
39592, June 7, 2002]
§144.2 Promulgation of Class II pro-
grams for Indian lands.
Notwithstanding the requirements of
this part or parts 124 and 146 of this
chapter, the Administrator may pro-
mulgate an alternate UIC Program for
Class II wells on any Indian reservation
or Indian lands. In promulgating such a
program the Administrator shall con-
sider the following factors:
(a) The interest and preferences of
the tribal government having responsi-
bility for the given reservation or In-
dian lands;
{b> The consistency between the al-
ternate program and any program in
effect in an adjoining jurisdiction; and
(c) Such other factors as are nec-
essary and appropriate to carry out the
Safe Drinking Water Act.
§ 144.3 Definitions.
Terms not defined in this section
have the meaning given by the appro-
priate Act. When a defined term ap-
pears in a definition, the defined term
is sometimes placed within quotation
marks as an aid to readers,
Administrator means the Adminis-
trator of the United States Environ-
mental Protection Agency, or an au-
thorized representative.
Application means the EPA standard
national forms for applying for a per-
mit, including any additions, revisions
or modifications to the forms; or forms
approved by EPA for use in approved
States, including any approved modi-
fications or revisions.
Appropriate Act and regulations means
the Solid Waste Disposal Act, as
amended by the Resource Conservation
and Recovery Act (RCBA); or Safe
Drinking Water Act (SDWA), which-
ever is applicable; and applicable
regulations promulgated under those
statutes.
Approved State Program means a UIC
program administered by the State or
Indian Tribe that has been approved by
EPA according to SDWA sections 1422
and,'or 1425.
Aquifer means a geological "forma-
tion," group of formations, or part of a
formation that is capable of yielding a
significant amount of water to a well
or spring.
Area of review means the area sur-
rounding an injection well described
according1 to the criteria set forth in
§146.06 or in the case of an area permit,
the project area plus a circumscribing
area the width of which is either 1A of
a mile or a number calculated accord-
ing to the criteria set forth in §146.06.
Cesspool means a "drywell" that re-
ceives untreated sanitary waste con-
taining human excreta, and which
sometimes has an open bottom and/or
perforated sides.
Contaminant means any physical,
chemical, biological, or radiological
substance or matter in water.
Director means the Regional Adminis-
trator, the State director or the Tribal
director as the context requires, or an
authorized representative. When there
is no approved State or Tribal pro-
gram, and there is an EPA adminis-
tered program, "Director" means the
Begional Administrator. When there is
an approved State or Tribal program,
"Director" normally means the State or
622
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Environmental Protection Agency
§144.1
part 124 requirements; State adminis-
tered programs must comply with part
124 as required by part 145. These re-
quirements carry out the purposes of
the public participation requirement of
40 OPE part 25 (Public Participation),
and supersede the requirements of that
part as they apply to the UIC Program,
(4) Part 146. This part sets forth the
technical criteria and standards that
must be met in permits and authoriza-
tions by rule as required by part 144.
(g) Scope of the permit or rule require-
ment. The UIC Permit Program regu-
lates underground injections by five
classes of wells (see definition of "well
injection," §144.3). The five classes of
wells are set forth in §144.6. All owners
or operators of these injection wells
must be authorized either by permit or
rule by the Director. In carrying out
the mandate of the SOW A, this subpart
provides that no injection shall be au-
thorized by permit or rule if it results
in the movement of fluid containing
any contaminant into Underground
Sources of Drinking Water (USDWs—
see §144.3 for definition), if the pres-
ence of that contaminant may cause a
violation of any primary drinking
water regulation under 40 CFB part 141
or may adversely affect the health of
persons (§144.12). Existing Class IV
wells which inject hazardous waste di-
rectly into an underground source of
drinking water are to be eliminated
over a period of six months and new
such Class IV wells are to be prohibited
(§144.13). For Class V wells, if remedial
action appears necessary, a permit may
be required (§144.25) or the Director
must require remedial action or clo-
sure by order (§144.12(c)). During UIC
Program development, the Director
may identify aquifers and portions of
aquifers which are actual or potential
sources of drinking water. This will
provide an aid to the Director in car-
rying out his or her duty to protect all
USDWs. An aquifer is a USDW if it fits
the definition, even if it has not been
"identified." The Director may also des-
ignate "exempted aquifers" using the
criteria in 40 CFR 146.4. Such aquifers
are those which would otherwise qual-
ify as "underground sources of drinking
water" to be protected, but which have
no real potential to be used as drinking
water sources. Therefore, they are not
USDWs. No aquifer is an "exempted aq-
uifer" until it has been affirmatively
designated under the procedures in
§144.7. Aquifers which do not fit the
definition of "underground source of
drinking water" are not "exempted
aquifers." They are simply not subject
to the special protection afforded
USDWs.
(1) Specific inclusions. The following
wells are included among those types
of injection activities which are cov-
ered by the UIC regulations. (This list
is not intended to be exclusive but is
for clarification only.)
(i) Any injection well located on a
drilling platform inside the State's ter-
ritorial waters.
(ii) Any dug hole or well that is
deeper than its largest surface dimen-
sion, where the principal function of
the hole is emplacement of fluids.
(iii) Any well used by generators of
hazardous waste, or by owners or oper-
ators of hazardous waste management
facilities, to dispose of fluids con-
taining hazardous waste. This includes
the disposal of hazardous waste into
what would otherwise be septic sys-
tems and cesspools, regardless of their
capacity.
(iv) Any septic tank, cesspool, or
other well used by a multiple dwelling,
community, or Regional system for the
injection of wastes.
(2) Specific exclusions. The following
are not covered by these regulations:
(i) Injection wells located on a drill-
ing platform or other site that is be-
yond the State's territorial waters.
(ii) Individual or single family resi-
dential waste disposal systems such as
domestic cesspools or septic systems.
(iii) Non-residential cesspools, septic
systems or similar waste disposal sys-
tems if such systems (A) Are used sole-
ly for the disposal of sanitary waste,
and (B) have the capacity to serve
fewer than 20 persons a day.
(iv) Injection wells used for injection
of hydrocarbons which are of pipeline
quality and are gases at standard tem-
perature and pressure for the purpose
of storage.
(v) Any dug hole, drilled hole, or
bored shaft which is not used for the
subsurface emplacement of fluids.
(3) The prohibition applicable to
Class IV wells under §144.13 does not
621
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Environmental Protection Agency
§144.3
Tribal director. In some circumstances,
however, EPA retains the authority to
take certain actions even when there is
an approved State or Tribal program.
In such cases, the term "Director"
means the Regional Administrator and
not the State or Tribal director.
Draft permit means a document pre-
pared under §124.6 indicating the Direc-
tor's tentative decision to issue or
deny, modify, revoke and reissue, ter-
minate, or reissue a "permit." A notice
of intent to terminate a permit, and a
notice of intent to deny a permit, as
discussed in §124.5 are types of "draft
permits." A denial of a request for
modification, revocation and
reissuance, or termination, as dis-
cussed in §124.5 is not a "draft permit."
Drilling mud means a heavy suspen-
sion used in drilling an "injection well,"
introduced down the drill pipe and
through the drill bit.
Dry well means a well, other than an
improved sinkhole or subsurface fluid
distribution system, completed above
the water table so that its bottom and
sides are typically dry except when re-
ceiving fluids.
Eligible Indian Tribe is a Tribe that
meets the statutory requirements es-
tablished at 42 U.S.C. 30Qj-ll(b)(l).
Emergency permit means a UIC "per-
mit" issued in accordance with §144.34.
Environmental Protection Agency
("EPA") means the United States Envi-
ronmental Protection Agency.
EPA means the United States "Envi-
ronmental Protection Agency."
Exempted aquifer means an "aquifer"
or its portion that meets the criteria in
the definition of "underground source
of drinking water" but which has been
exempted according to the procedures
in §144.7.
Existing injection well means an "in-
jection well" other than a "new injec-
tion well."
Facility or activity means any UIC
"injection well," or an other facility or
activity that is subject to regulation
under the UIC program.
Fluid means any material or sub-
stance which flows or moves whether
in a semisolid, liquid, sludge, gas, or
any other form or state.
Formation means a body of consoli-
dated or unconsolidated rock charac-
terized by a degree of lithologic homo-
geneity which is prevailingly, but not
necessarily, tabular and is mappable on
the earth's surface or traceable in the
subsurface.
Formation fluid means "fluid" present
in a "formation" under natural condi-
tions as opposed to introduced fluids,
such as "drilling mud."
Generator means any person, by site
location, whose act or process produces
hazardous waste identified or listed in
40 CFB part 261.
Ground water means water below the
land surface in a zone of saturation.
Hazardous waste means a hazardous
waste as defined in 40 CPE 261.3.
Hazardous waste management facility
("HWM facility") means all contiguous
land, and structures, other appur-
tenances, and improvements on the
land used for treating, storing, or dis-
posing of hazardous waste. A facility
may consist of several treatment, stor-
age, or disposal operational units (for
example, one or more landfills, surface
impoundments, or combination of
them).
HWM facility means "Hazardous
Waste Management facility"
Improved sinkhole means a naturally
occurring karst depression or other
natural crevice found in volcanic ter-
rain and other geologic settings which
have been modified by man for the pur-
pose of directing and emplacing fluids
into the subsurface.
Indian lands means "Indian country"
as defined in 18 U.S.C. 1151. That sec-
tion defines Indian country as:
(a) All land within the limits of any
Indian reservation under the jurisdic-
tion of the United States government,
notwithstanding the issuance of any
patent, and, including rights-of-way
running through the reservation;
(b) All dependent Indian commu-
nities within the borders of the United
States whether within the original or
subsequently acquired territory there-
of, and whether within or without the
limits of a State; and
(c) All Indian allotments, the Indian
titles to which have not been extin-
guished, including rights-of-way run-
ning through the same.
Indian Tribe means any Indian Tribe
having a Federally recognized gov-
erning body carrying out substantial
623
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§144.3
40 CFR Ch. ! (7-1-04 Edition)
governmental duties and powers over a
defined area.
Injection well means a "well" into
which "fluids" are being injected.
Injection zone means a geological
"formation" group of formations, or
part of a formation receiving fluids
through a "well."
Interstate Agency means an agency of
two or more States established by or
under an agreement or compact ap-
proved by the Congress, or any other
agency of two or more States or Indian
Tribes having substantial powers or du-
ties pertaining to the control of pollu-
tion as determined and approved by the
Administrator under the "appropriate
Act and regulations."
Major facility means any UIC "facility
or activity" classified as such by the
Regional Administrator, or, in the case
of approved State programs, the Re-
gional Administrator in conjunction
with the State Director.
Manifest means the shipping docu-
ment originated and signed by the
"generator" which contains the infor-
mation required by subpart B of 40 CPR
part 262.
New injection wells means an "injec-
tion well" which began injection after a
UIC program for the State applicable
to the well is approved or prescribed.
Owner or operator means the owner or
operator of any "facility or activity"
subject to regulation under the UIC
.program.
Permit means an authorization, li-
cense, or equivalent control document
issued by EPA or an approved State to
implement the requirements of this
part, parts 145, 146 and 124. "Permit" in-
cludes an area permit (§144.33) and an
emergency permit (§144.34). Permit
does not include UIC authorization by
rule (§144.21), or any permit which has
not yet been the subject of final agency
action, such as a "draft permit."
Person means an individual, associa-
tion, partnership, corporation, munici-
pality, State, Federal, or Tribal agen-
cy, or an agency or employee thereof.
Plugging means the act or process of
stopping the flow of water, oil or gas
into or out of a formation through a
borehole or well penetrating that for-
mation.
Point of injection means the last ac-
cessible sampling point prior to waste
fluids being released into the sub-
surface environment through a Class V
injection well. For example, the point
of injection of a Class V septic system
might be the distribution box—the last
accessible sampling point before the
waste fluids drain into the underlying
soils. For a dry well, it is likely to be
the well bore itself.
Project means a group of wells in a
single operation.
Radioactive Waste means any waste
which contains radioactive material in
concentrations which exceed those list-
ed in 10 CFR part 20, appendix B, table
II, column 2.
RCRA means the Solid Waste Dis-
posal Act as amended by the Resource
Conservation and Recovery Act of 1976
(Pub. L, 94-580, as amended by Pub. L.
95-609, Pub. L. 96-510, 42 U.S.C. 6901 et
seq.).
Regional Administrator means the Re-
gional Administrator of the appro-
priate Regional Office of the Environ-
mental Protection Agency or the au-
thorized representative of the Regional
Administrator.
Sanitary waste means liquid or solid
wastes originating solely from humans
and human activities, such as wastes
collected from toilets, showers, wash
basins, sinks used for cleaning domes-
tic areas, sinks used for food prepara-
tion, clothes washing operations, and
sinks or washing machines where food
and beverage serving dishes, glasses,
and utensils are cleaned. Sources of
these wastes may include single or
multiple residences, hotels and motels,
restaurants, bunkhouses, schools, rang-
er stations, crew quarters, guard sta-
tions, campgrounds, picnic grounds,
day-use recreation areas, other com-
mercial facilities, and industrial facili-
ties provided the waste is not mixed
with industrial waste.
Schedule of compliance means a sched-
ule of remedial measures included in a
"permit," including an enforceable se-
quence of interim requirements (for ex-
ample, actions, operations, or mile-
stone events) leading to compliance
with the "appropriate Act and regula-
tions."
SDWA means the Safe Drinking
Water Act (Pub. L. 93-523, as amended;
42 U.S.C. 300f etseq.).
624
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Environmental Protection Agency
§144,4
Septic system means a "well" that is
used to emplace sanitary waste below
the surface and is typically comprised
of a septic tank and subsurface fluid
distribution system or disposal system.
Site means the land or water area
where any "facility or activity" is phys-
ically located or conducted, including
adjacent land used in connection with
the facility or activity.
State means any of the 50 States, the
District of Columbia, Guam, the Com-
monwealth of Puerto Rico, the Virgin
Islands, American Samoa, the Trust
Territory of the Pacific Islands, the
Commonwealth of the Northern Mar-
iana Islands, or an Indian Tribe treated
as a State.
State Director means the chief admin-
istrative officer of any State, inter-
state, or Tribal agency operating an
"approved program," or the delegated
representative of the State director. If
the responsibility is divided among two
or more States, interstate, or Tribal
agencies, "State Director" means the
chief administrative officer of the
State, interstate, or Tribal agency au-
thorized to perform the particular pro-
cedure or function to which reference
is made.
State/EPA agreement means an agree-
ment between the Regional Adminis-
trator and the State which coordinates
EPA and State activities, responsibil-
ities and programs.
Stratum (plural strata) means a single
sedimentary bed or layer, regardless of
thickness, that consists of generally
the same kind of rock material.
Subsurface fluid distribution system
means an assemblage of perforated
pipes, drain tiles, or other similar
mechanisms intended to distribute
fluids below the surface of the ground.
Total dissolved solids means the total
dissolved (filterable) solids as deter-
mined by use of the method specified in
40 CFR part 136.
Transferee means the owner or oper-
ator receiving ownership and/or oper-
ational control of the well.
Transferor means the owner or oper-
ator transferring ownership and/or
operational control of the well.
UIC means the Underground Injec-
tion Control program under Part C of
the Safe Drinking Water Act, including
an "approved State program."
Underground injection means a "well
injection."
Underground source of drinking water
(USDW) means an aquifer or its por-
tion:
(a)(l) Which supplies any public
water system; or
(2) Which contains a sufficient quan-
tity of ground water to supply a public
water system; and
(i) Currently supplies drinking water
for human consumption; or
(ii) Contains fewer than 10,000 mg/1
total dissolved solids; and
(b) Which is not an exempted aquifer.
USDW means "underground source of
drinking water."
Well means: A bored, drilled, or driv-
en shaft whose depth is greater than
the largest surface dimension; or, a dug
hole whose depth is greater than the
largest surface dimension; or, an im-
proved sinkhole; or, a subsurface fluid
distribution system.
Well injection means the subsurface
emplacement of fluids through a well.
[48 FR 14189, Apr. 1, 1983, as amended at 49
FR 45305, Nov. 15, 1984: 52 FR 20676, June 2,
1987; 53 FR 37412, Sept. 26, 1988; 58 FR 63895,
Dec. 3, 1993; 59 FR 64345, Dec. 14, 1994; 64 FR
68565, Deo. 7, 1999]
§ 144.4 Considerations under Federal
law.
The following is a list of Federal laws
that may apply to the issuance of per-
mits under these rules. When any of
these laws is applicable, its procedures
must be followed. When the applicable
law requires consideration or adoption
of particular permit conditions or re-
quires the denial of a permit, those re-
quirements also must be followed.
(a) The Wild and Scenic Rivers Act, 16
U.S.C. 1273 et seq. Section 7 of the Act
prohibits the Regional Administrator
from assisting by license or otherwise
the construction of any water re-
sources project that would have a di-
rect, adverse effect on the values for
which a national wild and scenic river
was established.
(b) The National Historic Preservation
Act of 1966, 16 U.S.C. 470 et seq. Section
106 of the Act and implementing regu-
lations (36 CFR part 800) require the
Regional Administrator, before issuing
625
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§144.5
40 CFR Ch. I (7-1-04 Edition)
a license, to adopt measures when fea-
sible to mitigate potential adverse ef-
fects of the licensed activity and prop-
erties listed or eligible for listing in
the National Register of Historic
Places. The Act's requirements are to
be implemented in cooperation with
State Historic Preservation Officers
and upon notice to, and when appro-
priate, in consultation with the Advi-
sory Council on Historic Preservation.
(c) The Endangered Species Act, 16
U.S.C. 1531 et seq. Section 1 of the Act
and implementing regulations (50 CFR
part 402) require the Regional Adminis-
trator to ensure, in consultation with
the Secretary of the Interior or Com-
merce, that any action authorized by
EPA is not likely to jeopardize the con-
tinued existence of any endangered or
threatened species or adversely affect
its critical habitat.
(d) The Coastal Zone Management Act,
16 U.S.C. 1451 et seq. Section 307(c) of
the Act and implementing regulations
(15 CPR part 930) prohibit EPA from
issuing a permit for an activity affect-
ing land or water use in the coastal
zone until the applicant certifies that
the proposed activity complies with
the State Coastal Zone Management
program, and the State or its des-
ignated agency concurs with the cer-
tification (or the Secretary of Com-
merce overrides the States noneoneur-
rence).
(e) The Pish, and Wildlife Coordination
Act, 16 U.S.C. 661 et seq., requires the
Regional Administrator, before issuing
a permit proposing or authorizing the
impoundment (with certain exemp-
tions), diversion, or other control or
modification of any body of water, con-
sult with the appropriate State agency
exercising jurisdiction over wildlife re-
sources to conserve these resources.
(f) Executive orders. [Reserved]
(Clean Water Act (33 U.S.C. 1251 et seq.). Safe
Drinking Water Act (42 U.S.C. 300f et seq.),
Clean Air Act (42 U.S.C. 7401 et seq.), Re-
source Conservation and Recovery Act (42
U.S.C. 6901 et seq.))
[48 PR 14189, Apr. 1, 1983, as amended at 48
FR 39621, Sept. 1, 1983]
§ 144.5 Confidentiality of information.
(a) In accordance with 40 CPR part 2,
any information submitted to EPA
pursuant to these regulations may be
claimed as confidential by the sub-
mitter. Any such claim must be as-
serted at the time of submission in the
manner prescribed on the application
form or instructions or, in the case of
other submissions, by stamping the
words "confidential business informa-
tion" on each page containing such in-
formation. If no claim is made at the
time of submission, EPA may make the
information available to the public
without further notice. If a claim is as-
serted, the information will be treated
in accordance with the procedures in 40
CPR part 2 (Public Information).
(b) Claims of confidentiality for the
following information will be denied:
(1) The name and address of any per-
mit applicant or permittee;
(2) Information which deals with the
existence, absence, or level of contami-
nants in drinking water.
§ 144,6 Classification of wells.
Injection wells are classified as fol-
lows;
(a) Class I. (1) Wells used by genera-
tors of hazardous waste or owners or
operators of hazardous waste manage-
ment facilities to inject hazardous
waste beneath the lowermost forma-
tion containing', within one-quarter
mile of the well bore, an underground
source of drinking water.
(2) Other industrial and municipal
disposal wells which inject fluids be-
neath the lowermost formation con-
taining, within one quarter mile of the
well bore, an underground source of
drinking water.
(3) Radioactive waste disposal wells
which inject fluids below the lower-
most formation containing an under-
ground source of drinking water within
one quarter mile of the well bore.
(b) Class II. Wells which inject fluids:
(1) Which are brought to the surface
in connection with natural gas storage
operations, or conventional oil or nat-
ural gas production and may be com-
mingled with waste waters from gas
plants which are an intergral part of
production operations, unless those wa-
ters are classified as a hazardous waste
at the time of injection.
(2) For enhanced recovery of oil or
natural gas; and
626
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Environmental Protection Agency
§144.7
(3) For storage of hydrocarbons
which are liquid at standard tempera-
ture and pressure.
(c) Class ///. Wells which inject for
extraction of minerals including:
(1) Mining of sulfur by the Fraseh
process;
(2) In situ production of uranium or
other metals; this category includes
only in-situ production from ore bodies
which have not been conventionally
mined. Solution mining of conven-
tional mines such as stopes leaching is
included in Class V.
(3) Solution mining of salts or pot-
ash.
(d) Class IV. (1) Wells used by genera-
tors of hazardous waste or of radio-
active waste, by owners or operators of
hazardous waste management facili-
ties, or by owners or operators of radio-
active waste disposal sites to dispose of
hazardous waste or radioactive waste
into a formation which within one-
quarter (l/4) mile of the well contains
an underground source of drinking
water.
(2) Wells used by generators of haz-
ardous waste or of radioactive waste,
by owners or operators of hazardous
waste management facilities, or by
owners or operators of radioactive
waste disposal sites to dispose of haz-
ardous waste or radioactive waste
above a formation which within one-
quarter (3/«) mile of the well contains
an underground source of drinking
water.
(3) Wells used by generators of haz-
ardous waste or owners or operators of
hazardous waste management facilities
to dispose of hazardous waste, which
cannot be classified under paragraph
(a)(l) or (d) (1) and (2) of this section
(e.g., wells used to dispose of hazardous
waste into or above a formation which
contains an aquifer which has been ex-
empted pursuant to §146.04).
(e) Class V. Injection wells not in-
cluded in Class I, II, III, or IV. Specific
types of Class V injection wells are de-
scribed in § 144.81.
[48 PR 14189, Apr. 1, 1983, as amended at 52
FR 20676, June 2, 1987; 64 PR 68565, Dec. 7,
1999]
§144.7 Identification of underground
sources of drinking water and ex-
empted aquifers.
(a) The Director may identify (by
narrative description, illustrations,
maps, or other means) and shall pro-
tect, except where exempted under
paragraph (b) of this section, as an un-
derground source of drinking water, all
aquifers or parts of aquifers which
meet the definition of an "underground
source of drinking water" in §144.3.
Even if an aquifer has not been specifi-
cally identified by the Director, it is an
underground source of drinking water
if it meets the definition in §144.3.
(b)(l) The Director may identify (by
narrative description, illustrations,
maps, or other means) and describe in
geographic and/or geometric terms
(such as vertical and lateral limits and
gradient) which are clear and definite,
all aquifers or parts thereof which the
Director proposes to designate as ex-
empted aquifers using the criteria in 40
CFR 146.04.
(2) No designation of an exempted aq-
uifer submitted as part of a TJIC Pro-
gram shall be final until approved by
the Administrator as part of a UIC pro-
gram.
(3) Subsequent to program approval
or promulgation, the Director may,
after notice and opportunity for a pub-
lic hearing, identify additional exempt-
ed aquifers. For approved State pro-
grams exemption of aquifers identifed
(i) under § 146.04(b) shall be treated as a
program revision under §145.32; (ii)
under §146.04(c) shall become final if
the State Director submits the exemp-
tion in writing to the Administrator
and the Administrator has not dis-
approved the designation within 45
days. Any disapproval by the Adminis-
trator shall state the reasons and shall
constitute final Agency action for pur-
poses of judicial review.
(c)(l) For Class III wells, the Director
shall require an applicant for a permit
which necessitates an aquifer exemp-
tion under §146,04(b)(l) to furnish the
data necessary to demonstrate that the
aquifer is expected to be mineral or hy-
drocarbon producing. Information con-
tained in the mining plan for the pro-
posed project, such as a map and gen-
eral description of the mining zone,
general information on the mineralogy
627
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§144.8
40 CFR Ch. I (7-1-04 Edition)
and geochemistry of the mining zone,
analysis of the amenability of the min-
ing zone to the proposed mining meth-
od, and a time-table of planned devel-
opment of the mining zone shall be
considered by the Director in addition
to the information required by
§144.31(gr).
(2) For Class II wells, a demonstra-
tion of commercial producibility shall
be made as follows:
(i) For a Class II well to be used for
enhanced oil recovery processes in a
field or project containing aquifers
from which hydrocarbons were pre-
viously produced, commercial
producibility shall be presumed by the
Director upon a demonstration by the
applicant of historical production hav-
ing occurred in the project area or
field,
(ii) For Class II wells not located in a
field or project containing aquifers
from which hydrocarbons were pre-
viously produced, information such as
logs, core data, formation description,
formation depth, formation thickness
and formation parameters such as per-
meability and porosity shall be consid-
ered by the Director, to the extent
such information is available.
S 144.8 Noneomplianee and program
reporting by the Director.
The Director shall prepare quarterly
and annual reports as detailed below.
When the State is the permit-issuing
authority, the State Director shall sub-
mit any reports required under this
section to the Regional Administrator.
When EPA is the permit-issuing au-
thority, the Regional Administrator
shall submit any report required under
this section to EPA Headquarters.
(a) Quarterly reports. The Director
shall submit quarterly narrative re-
ports for major facilities as follows:
(1) Format, The report shall use the
following format:
(i) Provide an alphabetized list of
permittees. When two or more permit-
tees have the same name, the lowest
permit number shall be entered first.
(ii) For each entry on the list, in-
clude the following information in the
following order:
(A) Name, location, and permit num-
ber of the noncomplying permittees.
(B) A brief description and date of
each Instance of noncompliance for
that permittee. Instances of non-
compliance may include one or more
the kinds set forth in paragraph (a)(2)
of this section. When a permittee has
noncompliance of more than one kind,
combine the information into a single
entry for each such permittee.
(C) The date(s) and a brief descrip-
tion of the action(s) taken by the Di-
rector to ensure compliance.
(D) Status of the instance(s) of non-
compliance with the date of the review
of the status or the date of resolution.
(B) Any details which tend to explain
or mitigate the instance(s) of non-
compliance.
(2) Instances of noncompliance to be re-
ported. Any instances of noncompliance
within the following categories shall be
reported in successive reports until the
noncompliance is reported as resolved.
Once noncompliance is reported as re-
solved it need not appear in subsequent
reports.
(i) Failure to complete construction ele-
ments. When the permittee has failed to
complete, by the date specified in the
permit, an element of a compliance
schedule involving either planning for
construction or a construction step (for
example, begin construction, attain op-
eration level); and the permittee has
not returned to compliance by accom-
plishing the required elements of the
schedule within 30 days from the date a
compliance schedule report is due
under the permit.
(ii) Modifications to schedules of com-
pliance. When a schedule of compliance
in the permit has been modified under
§§ 144.39 or 144.41 because of the permit-
tee's noncompliance.
(iii) Failure to complete or provide com-
pliance schedule or monitoring reports.
When the permittee has failed to com-
plete or provide a report required in a
permit compliance schedule (for exam-
ple, progress report or notice of non-
compliance or compliance) or a moni-
toring report; and the permittee has
not submitted the complete report
within 30 days from the date it is due
under the permit for compliance sched-
ules, or from the date specified in the
permit for monitoring reports.
628
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Environmental Protection Agency
§144.11
(iv) Deficient reports. When the re-
quired reports provided by the per-
mittee are so deficient as to cause mis-
understanding by the Director and thus
impede the review of the status of com-
pliance.
(v) Noncompliance with other permit re-
quirements, Noncompliance shall be re-
ported in the following circumstances:
(A) Whenever the permittee has vio-
lated a permit requirement (other than
reported under paragraph (a)(2) (i) or
(ii) of this section), and has not re-
turned to compliance within 45 days
from the date reporting of noncompli-
ance was due under the permit; or
(B) When the Director determines
that a pattern of noncompliance exists
for a major facility permittee over the
most recent four consecutive reporting
periods. This pattern includes any vio-
lation of the same requirement in two
consecutive reporting periods, and any
violation of one or more requirements
in each of four consecutive reporting
periods: or
(C) When the Director determines
significant permit noncompliance or
other significant event has occurred,
such as a migration of fluids into a
USDW.
(vi) All other. Statistical information
shall be reported quarterly on all other
instances of noncompliance by major
facilities with permit requirements not
otherwise reported under paragraph (a)
of this section.
(b) Annual reports—(1) Annual non-
compliance report. Statistical reports
shall be submitted by the Director on
nonmajor UIC permittees indicating
the total number reviewed, the number
of noncomplying nonmajor permittees,
the number of enforcement actions,
and number of permit modifications
extending compliance deadlines. The
statistical information shall be orga-
nized to follow the types of noncompli-
ance listed in paragraph (a) of this
section.
(2) For State-administered UIC Pro-
grams only. In addition to the annual
noncompliance report, the State Direc-
tor shall:
(i) Submit each year a program re-
port to the Administrator (in a manner
and form prescribed by the Adminis-
trator) consisting of:
(A) A detailed description of the
State's implementation of its program;
(B) Suggested changes, if any to the
program description (see §145.23(f))
which are necessary to reflect more ac-
curately the State's progress in issuing
permits;
(C) An updated inventory of active
underground injection operations in
the State.
(ii) In addition to complying with the
requirements of paragraph (b)(2)(i) of
this section, the Director shall provide
the Administrator, on February 28th
and August 31st of each of the first two
years of program operation, the infor-
mation required in 40 CFR 148.15, 146.25.
and 146.35.
(c) Schedule. (1) For all quarterly re-
ports. On the last working day of May,
August, November, and February, the
State Director shall submit to the Re-
gional Administrator information con-
cerning noncompliance with permit re-
quirements by major facilities in the
State in accordance with the following
schedule. The Regional Administrator
shall prepare and submit information
for EPA-issued permits to EPA Head-
quarters in accordance with the same
schedule.
QUARTERS COVERED BY REPORTS ON
NONCOMPLIANCE BY MAJOR FACILITIES
[Date for completion of reports]
January, February, and March , 1 May 31
April, May, and June 1 Aug. 31
July, August, and September "* Nov. 30
October, November, and December 1 Feb. 28
1 Reports must be made available to the public for inspec-
tion and copying on this date.
(2) For all annual reports. The period
for annual reports shall be for the cal-
endar year ending December 31, with
reports completed and available to the
public no more than 60 days later.
Subpart B—General Program
Requirements
§ 144,11 Prohibition of unauthorized
injection.
Any underground injection, except
into a well authorized by rule or except
as authorized by permit issued under
the UIC program, is prohibited. The
construction of any well required to
629
-------
§144.12
40 CFR Ch. I {7-1-04 Edition)
have a permit is prohibited until the
permit has been issued.
[48 PR 14189, Apr. 1, 1983, as amended at 58
PR 63895, Dec. 3, 1993]
§ 144.12 Prohibition of movement of
fluid into underground sources of
drinking water.
(a) No owner or operator shall con-
struct, operate, maintain, convert,
plug, abandon, or conduct any other in-
jection activity in a manner that al-
lows the movement of fluid containing
any contaminant into underground
sources of drinking water, if the pres-
ence of that contaminant may cause a
violation of any primary drinking
water regulation under 40 CPE part 142
or may otherwise adversely affect the
health of persons. The applicant for a
permit shall have the burden of show-
ing that the requirements of this para-
graph are met.
(b) For Class I, II and III wells, if any
water quality monitoring of an under-
ground source of drinking water indi-
cates the movement of any contami-
nant into the underground source of
drinking water, except as authorized
under part 146, the Director shall pre-
scribe such additional requirements for
construction, corrective action, oper-
ation, monitoring, or reporting (includ-
ing closure of the injection well) as are
necessary to prevent such movement.
In the case of wells authorized by per-
mit, these additional requirements
shall be imposed by modifying the per-
mit in accordance with §144.39, or the
permit may be terminated under
§144.40 if cause exists, or appropriate
enforcement action may be taken if the
permit has been violated. In the case of
wells authorized by rule, see §§ 144.21
through 144.24. For EPA administered
programs, such enforcement action
shall be taken in accordance with ap-
propriate sections of the SDWA.
(c) For Class V wells, if at any time
the Director learns that a Class V well
may cause a violation of primary
drinking water regulations under 40
CPR part 142, he or she shall:
(1) Require the injector to obtain an
individual permit;
(2) Order the injector to take such ac-
tions (including, where required, clo-
sure of the injection well) as may be
necessary to prevent the violation. For
EPA administered programs, such or-
ders shall be issued in accordance with
the appropriate provisions of the
SDWA; or
(3) Take enforcement action.
(d) Whenever the Director learns that
a Class V well may be otherwise ad-
versely affecting the health of persons,
he or she may prescribe such actions as
may be necessary to prevent the ad-
verse effect, including any action au-
thorized under paragraph (c) of this
section.
(e) Notwithstanding any other provi-
sion of this section, the Director may
take emergency action upon receipt of
information that a contaminant which
is present in or likely to enter a public
water system or underground source of
drinking water may present an immi-
nent and substantial endangerment to
the health of persons. If the Director is
an EPA official, he must first deter-
mine that the appropriate State and
local authorities have not taken appro-
priate action to protect the health of
such persons, before taking emergency
action.
[48 PR 14189, Apr. 1. 1983, as amended at 52
PR 20676, June 2, 1987]
§ 144.13 Prohibition of Class IV wells.
(a) The following: are prohibited, ex-
cept as provided in paragraph (c) of
this section:
(1) The construction of any Class IV
well.
(2) The operation or maintenance of
any Class IV well not in operation
prior to July 18, 1980.
(3) The operation or maintenance of
any Class IV well that was in operation
prior to July 18, 1980, after six months
following the effective date of a UIC
program approved or promulgated for
the state.
(4) Any increase in the amount of
hazardous waste or change in the type
of hazardous waste injected into a
Class IV well.
(b) The owner or operator of a Class
IV well shall comply with the require-
ments of §144.14, and with the require-
ments of §144.23 regarding closure of
Class IV wells.
(c) Wells used to inject contaminated
ground water that has been treated and
is being reinjected into the same for-
mation from which it was drawn are
630
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Environmental Protection Agency
§144.16
not prohibited by this section if such
injection is approved by EPA, or a
State, pursuant to provisions for clean-
up of releases under the Comprehensive
Environmental Response, Compensa-
tion, and Liability Act of 1980
(CBRCLA), 42 U.S.C. 9601-9657, or pur-
suant to requirements and provisions
under the Resource Conservation and
Recovery Act (RCRA), 42 U.S.C. 6901
through 6987.
(d) Clarification. The following wells
are not prohibited by this action:
(1) Wells used to inject hazardous
waste into aquifers or portions thereof
that have been exempted pursuant to
§146.4, if the exempted aquifer into
which waste is injected underlies the
lowermost formation containing a
USDW. Such wells are Class I wells as
specified in §144.6(a)(l), and the owner
or operator must comply with the re-
quirements applicable to Class I wells.
(2) Wells used to inject hazardous
waste where no USDW exists within
one quarter mile of the well bore in
any underground formation, provided
that the Director determines that such
injection is into a formation suffi-
ciently isolated to ensure that injected
fluids do not migrate from the injec-
tion zone. Such wells are Class I wells
as specified in §144,6(a)(l), and the
owner or operator must comply with
the requirements applicable to Class I
wells.
[49 FR 20181, May 11, 1984, as amended at 67
FR 39593, June 7, 2002]
§ 144,14 Requirements for wells inject-
ing hazardous waste,
(a) Applicability. The regulations in
this section apply to all generators of
hazardous waste, and to the owners or
operators of all hazardous waste man-
agement facilities, using any class of
well to inject hazardous wastes accom-
panied by a manifest. (See also §144.13.)
(b) Authorization. The owner or oper-
ator of any well that is used to inject
hazardous waste required to be accom-
panied by a manifest or delivery docu-
ment shall apply for authorization to
inject as specified in §144.31 within 6
months after the approval or promul-
gation of the State UIC program.
(c) Requirements. In addition to com-
plying with the applicable require-
ments of this part and 40 CFR part 146,
the owner or operator of each facility
meeting the requirements of paragraph
(b) of this section, shall comply with
the following:
(1) Notification. The owner or operator
shall comply with the notification re-
quirements of section 3010 of Public
Law 94-580.
(2) Identification number. The owner
or operator shall comply with the re-
quirements of 40 CPR 264.11.
(3) Manifest system. The owner or op-
erator shall comply with the applicable
recordkeeping and reporting require-
ments for manifested wastes in 40 CFR
264.71.
(4) Manifest discrepancies. The owner
or operator shall comply with 40 CPR
264.72.
(5) Operating record. The owner or op-
erator shall comply with 40 CFR
264,73(a), (b)(l), and (b)(2),
(6) Annual report. The owner or oper-
ator shall comply with 40 CFR 264.75.
(7) Unmanifested waste report. The
owner or operator shall comply with 40
CFR 264.75.
(8) Personnel training. The owner or
operator shall comply with the applica-
ble personnel training requirements of
40 CFR 264.16.
(9) Certification of closure. When aban-
donment is completed, the owner or op-
erator must submit to the Director cer-
tification by the owner or operator and
certification by an independent reg-
istered professional engineer that the
facility has been closed in accordance
with the specifications in § 144.52(a)(6).
(d) Additional requirements for Class IV
wells. [Reserved]
§144.15 {Reserved]
§144.16 Waiver of requirement by Di-
rector,
(a) When injection does not occur into,
through or above an underground source
of drinking water, the Director may au-
thorize a well or project with less
stringent requirements for area of re-
view, construction, mechanical integ-
rity, operation, monitoring, and re-
porting than required in 40 CFR part
146 or §144.52 to the extent that the re-
duction in requirements will not result
in an increased risk of movement of
fluids into an underground source of
drinking water.
631
203-160 D-21
-------
§144.17
40 CFR Ch. I (7-1-04 Edition)
(b) When injection occurs through or
above an underground source of drink-
ing water, but the radius of endan-
gering influence when computed under
§146.06(a) is smaller or equal to the ra-
dius of the well, the Director may au-
thorize a well or project with less
stringent requirements for operation,
monitoring, and reporting- than re-
quired in 40 CFR part 146 or §144.52 to
the extent that the reduction in re-
quirements will not result in an in-
creased risk of movement of fluids into
an underground source of drinking
water.
(c) When reducing requirements
under paragraph (a) or (b) of this sec-
tion, the Director shall prepare a fact
sheet under §124.8 explaining the rea-
sons for the action.
§ 144.17 Records.
The Director or the Administrator
may require, by written notice on a se-
lective well-by-well basis, an owner or
operator of an injection well to estab-
lish and maintain records, make re-
ports, conduct monitoring, and provide
other information as is deemed nec-
essary to determine whether the owner
or operator has acted or is acting in
compliance with Part C of the SDWA
or its implementing1 regulations.
[58 FE 63895, Dec. 3, 1993]
Subpart C—Authorization of
Underground Injection by Rule
§ 144.21 Existing Class I, II (except en-
hanced recovery and hydrocarbon
storage) and III wells.
(a) An existing- Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III injection well is authorized
by rule if the owner or operator injects
into the existing well within one year
after the date at which a UIC program
authorized under the SDWA becomes
effective for the first time or inven-
tories the well pursuant to the require-
ments of §144.26. An owner or operator
of a well which is authorized by rule
pursuant to this section shall rework,
operate, maintain, convert, plug, aban-
don or inject into the well in compli-
ance with applicable regulations.
(b) Duration of well authorization by
rule. Well authorization under this sec-
tion expires upon the effective date of
a permit issued pursuant to §§144.25,
144.31, 144.33 or 144.34; after plugging
and abandonment in accordance with
an approved plugging and abandonment
plan pursuant to §§144.28(e) and 146.10,
and upon submission of a plugging and
abandonment report pursuant to
|144.28(k); or upon conversion in com-
pliance with §144.28(j).
(c) Prohibitions on injection. An owner
or operator of a well authorized by rule
pursuant to this section is prohibited
from injecting into the well:
(1) Upon the effective date of an ap-
plicable permit denial;
(2) Upon failure to submit a permit
application in a timely manner pursu-
ant to §§144.25 or 144.31;
(3) Upon failure to submit inventory
information in a timely manner pursu-
ant to § 144.26;
(4) Upon failure to comply with a re-
quest for information in a timely man-
ner pursuant to § 144.27;
(5) Upon failure to provide alter-
native financial assurance pursuant to
§144.28(d)(7);
(6) Forty-eight hours after receipt of
a determination by the Director pursu-
ant to §144.28(f)(3) that the well lacks
mechanical integrity, unless the Direc-
tor requires immediate cessation;
(7) Upon receipt of notification from
the Director pursuant to §144.28(1) that
the transferee has not demonstrated fi-
nancial responsibility pursuant to
§144.28(d);
(8) For Class I and III wells:
(i) In States with approved programs,
five years after the effective date of
the UIC program unless a timely and
complete permit application is pending
the Director's decision; or
(ii) In States with programs adminis-
tered by EPA, one year after the effec-
tive date of the UIC program unless a
timely and complete permit applica-
tion is pending the Director's decision;
or
(9) For Class II wells (except en-
hanced recovery and hydrocarbon stor-
age), five years after the effective date
of the UIC program unless a timely and
complete permit application is pending
the Director's decision.
(d) Class II and III wells in existing
fields or projects. Notwithstanding the
632
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Environmental Protection Agency
§ 144.23
prohibition in §144,11, this section au-
thorizes Class II and Class III wells or
projects in existing fields or projects to
continue normal operations until per-
mitted, including construction, oper-
ation, and plugging and abandonment
of wells as part of the operation, pro-
vided the owner or operator maintains
compliance with all applicable require-
ments.
(e) Requirements. The owner or oper-
ator of a well authorized under this
section shall comply with the applica-
ble requirements of §144.28 and part 147
of this chapter no later than one year
after authorization.
[48 FR 14189, Apr. 1, 1983, as amended at 49
FB 20181, May 11, 1984: 58 PR 63895, Dec. 3,
1993]
§ 144.22 Existing Class II enhanced re-
covery and hydrocarbon storage
wells.
(a) An existing Class II enhanced re-
covery or hydrocarbon storage injec-
tion well is authorized by rule for the
life of the well or project, if the owner
or operator injects into the existing
well within one year after the date
which a UIC program authorized under
the SDWA becomes effective for the
first time or inventories the well pur-
suant to the requirements of § 144.26.
An owner or operator of a well which is
authorized by rule pursuant to this sec-
tion shall rework, operate, maintain,
convert, plug, abandon or inject into
the well in compliance with applicable
regulations.
(b) Duration of well authorization by
rule. Well authorization under this sec-
tion expires upon the effective date of
a permit issued pursuant to §§144.25,
144.31, 144.33 or 144.34; after plugging
and abandonment in accordance with
an approved plugging and abandonment
plan pursuant to §§144.28(c) and 146.10
of this chapter, and upon submission of
a plugging and abandonment report
pursuant to §144.28(k); or upon conver-
sion in compliance with § 144,28(j).
(c) Prohibitions on injection. An owner
or operator of a well authorized by rule
pursuant to this section is prohibited
from injecting into the well:
(1) Upon the effective date of an ap-
plicable permit denial;
(2) Upon failure to submit a permit
application in a timely manner pursu-
ant to §§144.25 or 144.31;
(3) Upon failure to submit inventory
information in a timely manner pursu-
ant to § 144.26;
(4) Upon failure to comply with a re-
quest for information in a timely man-
ner pursuant to §144.27;
(5) Upon failure to provide alter-
native financial assurance pursuant to
§144.28(d)(7);
(6) Forty-eight hours after receipt of
a determination by the Director pursu-
ant to §144.28(f)(3) that the well lacks
mechanical integrity, unless the Direc-
tor requires immediate cessation; or
(7) Upon receipt of notification from
the Director pursuant to §144.28(1) that
the transferee has not demonstrated fi-
nancial responsibility pursuant to
§144.28(d).
(d) Requirements. The owner or oper-
ator of a well authorized under this
section shall comply with the applica-
ble requirements of § 144.28 and part 147
of this chapter. Such owner or operator
shall comply with the casing and ce-
menting requirements no later than 3
years and other requirements no later
than 1 year after authorization.
[49 FE 20181, May 11, 1984, as amended at 58
FE 63896, Dec. 3,
§ 144.23 Class IV wells.
(a) Injection into existing Class IV
wells is authorized for up to six months
after approval or promulgation of the
UIC Program. Such wells are subject to
the requirements of §§144.13 and
144.14(c).
(b) Closure. For EPA administered
programs only,
(1) Prior to abandoning any Class IV
well, the owner or operator shall plug
or otherwise close the well in a manner
acceptable to the Regional Adminis-
trator.
(2) [Reserved]
(3) The owner or operator of a Class
IV well must notify the Regional Ad-
ministrator of intent to abandon the
well at least thirty days prior to aban-
donment.
(c) Notwithstanding the require-
ments of paragraphs (a) and (b) of this
section, injection wells used to inject
contaminated ground water that has
been treated and is being injected into
633
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§144.24
40 CFR Ch.! (7-1-04 Edition)
the same formation from which it was
drawn are authorized by rule for the
life of the well if such subsurface em-
placement of fluids is approved by
EPA, or a State, pursuant to provisions
for cleanup of releases under the Com-
prehensive Environmental Response,
Compensation, and Liability Act of
1980 (CERCLA), 42 U.S.C. 9601^9675, or
pursuant to requirements and provi-
sions under the Resource Conservation
and Recovery Act (RCRA), 42 U.S.C.
6901-6992k.
[49 FR 20181, May 11, 1984, as amended at 60
FB 33932, June 29, 1995; 64 FR 68566, Dec. 7,
1999]
§144.24 Class V wells.
(a) A Class V injection well is author-
ized by rule, subject to the conditions
in §144.84
(b) Duration of well authorization by
rule. Well authorization under this sec-
tion expires upon the effective date of
a permit issued pursuant to §§144.25,
144.31, 144.33 or 144.34, or upon proper
closure of the well.
(c) Prohibition of injection. An owner
or operator of a well which is author-
ized by rule pursuant to this section is
prohibited from injecting into the well:
(1) Upon the effective date of an ap-
plicable permit denial;
(2) Upon failure to submit a permit
application in a timely manner pursu-
ant to §§144.25 or 144.31;
(3) Upon failure to submit inventory
information in a timely manner pursu-
ant to § 144.26; or
(4) Upon failure to comply with a re-
quest for information in a timely man-
ner pursuant to § 144.27.
[58 FB 63896, Dec. 3, 1993, as amended at 64
FR 68566, Dec. 7, 1999]
§ 144.25 Requiring a permit.
(a) The Director may require the
owner or operator of any Class I, II, III
or V injection well which is authorized
by rule under this subpart to apply for
and obtain an individual or area UIC
permit. Cases where individual or area
UIC permits may be required include:
(1) The injection well is not in com-
pliance with any requirement of the
rule;
NOTE: Any underground injection whioli
violates any authorization by rule is subject
to appropriate enforcement action.
(2) The injection well is not or no
longer is within the category of wells
and types of well operations authorized
In the rule;
(3) The protection of USDWs requires
that the injection operation be regu-
lated by requirements, such as for cor-
rective action, monitoring and report-
ing, or operation, which are not con-
tained in the rule.
(4) When the injection well is a Class
I, II (except existing enhanced recovery
and hydrocarbon storage) or III well, in
accordance with a schedule established
by the Director pursuant to §144.31(c).
(b) For EPA-administered programs,
the Regional Administrator may re-
quire an owner or operator of any well
which is authorized by rule under this
subpart to apply for an individual or
area UIC permit under this paragraph
only if the owner or operator has been
notified in writing that a permit appli-
cation is required. The owner or oper-
ator of a well which is authorized by
rule under this subpart is prohibited
from injecting into the well upon the
effective date of permit denial, or upon
failure by the owner or operator to sub-
mit an application in a timely manner
as specified in the notice. The notice
shall include: a brief statement of the
reasons for requiring a permit; an ap-
plication form; a statement setting a
time for the owner or operator to file
the application; and a statement of the
consequences of denial or issuance of
the permit, or failure to submit an ap-
plication, as described in this para-
graph,
(c) An owner or operator of a well au-
thorized by rule may request to be ex-
cluded from the coverage of this sub-
part by applying for an individual or
area UIC permit. The owner or oper-
ator shall submit an application under
§144.31 with reasons supporting the re-
quest, to the Director. The Director
may grant any such requests.
[48 PR 14189, Apr. 1, 1988, as amended at 49
FB 20182, May 11, 1984; 58 FB 63896. Dec. 3,
1993]
§ 144.26 Inventory requirements.
The owner or operator of an injection
well which is authorized by rule under
this subpart shall submit inventory in-
formation to the Director. Such an
owner or operator is prohibited from
634
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Environmental Protection Agency
§144.27
injecting into the well upon failure to
submit inventory information for the
well within the time frame specified in
paragraph (d) of this section.
(a) Contents. As part of the inventory,
the Director shall require and the
owner/operator shall provide at least
the following information:
(1) Facility name and location;
(2) Name and address of legal con-
tact;
(3) Ownership of facility;
(4) Nature and type of injection wells;
and
(5) Operating status of injection
wells.
NOTE: This information is requested on na-
tional form "Inventory of Injection Wells,"
OMB No, 158-B0170.
(b) Additional contents. For EPA ad-
ministered programs only, the owner
or operator of a well listed in para-
graph (b)(l) of this section shall pro-
vide the information listed in para-
graph (b)(2) of this section.
(1) This section applies to the fol-
lowing wells:
Ci) Class II enhanced recovery wells;
(ii) Class rv wells;
(iii) The following Class V wells;
(A) Sand or other backfill wells
[§146.5(e)(8)];
(B) Radioactive waste disposal wells
that are not Class I wells (40 CFR 146.5
(C) Geothermal energy recovery wells
[§146.5(e)(12)];
(D) Brine return flow wells
[§146.5(e)(14)];
(E) Wells used in experimental tech-
nologies [§146.5(e)(15)];
(F) Municipal and industrial disposal
wells other than Class I; and
(O) Any other Class V wells at the
discretion of the Regional Adminis-
trator.
(2) The owner or operator of a well
listed in paragraph (b)(l) shall provide
a listing of all wells owned or operated
setting forth the following information
for each well. (A single description of
wells at a single facility with substan-
tially the same characteristics is ac-
ceptable).
(i) For Class II only, the field
name(s);
(ii) Location of each well or project
given by Township, Range, Section,
and Quarter-Section, or by latitude and
longitude to the nearest second, ac-
cording to the conventional practice in
the State;
(iii) Date of completion of each well;
(iv) Identification and depth of the
formation(s) into which each well is in-
jecting;
(v) Total depth of each well;
(vi) Casing and cementing record,
tubing size, and depth of packer;
(vii) Nature of the injected fluids;
(viii) Average and maximum injec-
tion pressure at the wellhead;
(ix) Average and maximum injection
rate; and
(x) Date of the last mechanical integ-
rity test, if any.
(c) Notice. Upon approval of the UIC
Program in a State, the Director shall
notify owners or operators of injection
wells of their duty to submit inventory
information. The method of notifica-
tion selected by the Director must as-
sure that the owners or operators will
be made aware of the inventory re-
quirement.
(d) Deadlines. (1) The owner or oper-
ator of an injection well shall submit
inventory information no later than
one year after the date of approval or
effective date of the UIC program for
the State. The Director need not re-
quire inventory information from any
facility with interim status under
RCRA.
(2) For EPA administered programs
the information need not be submitted
if a complete permit application is sub-
mitted within one year of the effective
data of the UIC program. The owner or
operator of Class IV well shall submit
inventory information no later than 60
days after the effective date of the pro-
gram.
[48 FR 14189, Apr. 1. 1983. as amended at 49
PR 20182, May 11, 1984; 58 PR 63896, Dec. 3,
1993: 64 FR 68566, Dec. 7, 1999; 6? FR
June 7, 2002]
§ 144.27 Requiring other information.
(a) For EPA administered programs
only, in addition to the inventory re-
quirements of §144.26, the Regional Ad-
ministrator may require the owner or
operator of any well authorized by rule
under this subpart to submit informa-
tion as deemed necessary by the Re-
gional Administrator to determine
whether a well may be endangering an
635
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§144.28
40 CFR Ch. I (7-1-04 Edition)
underground source of drinking water
in violation of § 144.12 of this part.
(b) Such information requirements
may include, but are not limited to:
(1) Performance of ground-water
monitoring and the periodic submis-
sion of reports of such monitoring;
(2) An analysis of injected fluids, in-
cluding periodic submission of such
analyses; and
(3) A description of the geologic stra-
ta through and into which injection is
taking place.
(c) Any request for information under
this section shall be made in writing,
and include a brief statement of the
reasons for requiring the information.
An owner or operator shall submit the
information within the time period(s)
provided in the notice.
(d) An owner or operator of an injec-
tion well authorized by rule under this
subpart is prohibited from injecting
into the well upon failure of the owner
or operator to comply with a request
for information within the time pe-
riod(s) specified by the Director pursu-
ant to paragraph (c) of this section. An
owner or operator of a well prohibited
from injection under this section shall
not resume injection except under a
permit issued pursuant to §§144.25,
144.31, 144.33 or 144.34.
[49 PR 20182, May 11, 1984, as amended at 58
PR 63896, Dec. 3,1993]
§144.28 Requirements for Class I, II,
and III •wells authorized by rule.
The following requirements apply to
the owner or operator of a Class I, II or
III well authorized by rule under this
subpart, as provided by §§144.21(e) and
144.22(d).
(a) The owner or operator shall com-
ply with all applicable requirements of
this subpart and subpart B of this part.
Any noncompliance with these require-
ments constitutes a violation of the
Safe Drinking Water Act and is
grounds for enforcement action, except
that the owner or operator need not
comply with these requirements to the
extent and for the duration such non-
compliance is authorized by an emer-
gency permit under §144.34.
(b) Twenty-four hour reporting. The
owner or operator shall report any non-
compliance which may endanger health
or the environment, including:
(1) Any monitoring or other informa-
tion which indicates that any contami-
nant may cause an endangerment to a
USDW; or
(2) Any noncompliance or malfunc-
tion of the injection system which may
cause fluid migration into or between
USDWs.
Any information shall be provided oral-
ly within 24 hours from the time the
owner or operator becomes aware of
the circumstances. A written submis-
sion shall also be provided within five
days of the time the owner or operator
becomes aware of the circumstances.
The written submission shall contain a
description of the noncompliance and
its cause, the period of noncompliance,
including exact dates and times, and if
the noncompliance has not been cor-
rected, the anticipated time it is ex-
pected to continue; and steps taken or
planned to reduce, eliminate, and pre-
vent recurrence of the noncompliance.
(c) Plugging and abandonment plan. (1)
The owner or operator shall prepare,
maintain, and comply with a plan for
plugging and abandonment of the well
or project that meets the requirements
of §146.10 of this chapter and is accept-
able to the Director. For purposes of
this paragraph, temporary intermit-
tent cessation of Injection operations
is not abandonment.
(2) For EPA administered programs:
(i) The owner or operator shall sub-
mit the plan, on a form provided by the
Regional Administrator, no later than
one year after the effective date of the
UIC program in the state.
(ii) The owner or operator shall sub-
mit any proposed significant revision
to the method of plugging reflected in
the plan no later than the notice of
plugging required by §144.28(j)(2) (i.e.,
45 days prior to plugging unless shorter
notice is approved),
(ill) The plan shall Include the fol-
lowing information:
(A) The nature and quantity and ma-
terial to be used in plugging:
(B) The location and extent (by
depth) of the plugs;
(C) Any proposed test or measure-
ment to be made;
(D) The amount, size, and location
(by depth) of casing to be left in the
well;
636
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Environmental Protection Agency
§144.28
(E) Tlie method and location where
casing is to be parted; and
(P) [Reserved]
(O) The estimated cost of plugging
the well,
(iv) After a cessation of operations of
two years the owner or operator shall
plug and abandon the well in accord-
ance with the plan unless he:
(A) Provides notice to the Regional
Administrator;
(B) Describe actions or procedures,
satisfactory to the Regional Adminis-
trator, that the owner or operator will
take to ensure that the well will not
endanger USDWs during the period of
temporary abandonment. These actions
and procedures shall include compli-
ance with the technical requirements
applicable to active injection wells un-
less waived by the Regional Adminis-
trator.
(v) The owner or operator of any well
that has been temporarily abandoned
[ceased operations for more than two
years and has met the requirements of
paragraphs (c)(2) (A) and (B) of this sec-
tion] shall notify the Regional Admin-
istrator prior to resuming operation of
the well.
(d) Financial responsibility. (1) The
owner, operator and/or, for EPA-admin-
istered programs, the transferor of a
Class I, II or III well, is required to
demonstrate and maintain financial re-
sponsibility and resources to close,
plug and abandon the underground in-
jection operation in a manner pre-
scribed by the Director until:
(i) The well has been plugged and
abandoned in accordance with an ap-
proved plugging and abandonment plan
pursuant to §§144.28(c) and 146.10 and
submission of a plugging and abandon-
ment report has been made pursuant to
§144.28(k);
(ii) The well has been converted in
compliance with the requirements of
§144,28(j); or
(iii) For BPA-administered programs,
the transferor has received notice from
the Director that the transferee has
demonstrated financial responsibility
for the well. The owner or operator
shall show evidence of such financial
responsibility to the Director by the
submission of a surety bond, or other
adequate assurance, such as a financial
statement.
(2) For BPA-administered programs,
the owner or operator shall submit
such evidence no later than one year
after the effective date of the UIC pro-
gram in the State. Where the owner-
ship or operational control of the well
is transferred more than one year after
the effective date of the UIC program,
the transferee shall submit such evi-
dence no later than the date specified
in the notice required pursuant to
§144.28(1X2).
(3) For EPA administered programs
the Regional Administrator may re-
quire the owner or operator to submit
a revised demonstration of financial re-
sponsibility if the Regional Adminis-
trator has reason to believe that the
original demonstration is no longer
adequate to cover the cost of closing,
plugging and abandoning the well.
(4) For EPA administered programs
the owner or operator of a well inject-
ing hazardous waste must comply with
the financial responsibility require-
ments of subpart F of this part.
(5) For EPA-administered programs,
an owner or operator must notify the
Regional Administrator by certified
mail of the commencement of any vol-
untary or involuntary proceeding
under Title 11 (Bankruptcy) of the
United States Code which names the
owner or operator as debtor, within 10
business days after the commencement
of the proceeding. Any party acting as
guarantor for the owner or operator for
the purpose of financial responsibility
must so notify the Regional Adminis-
trator, if the guarantor is named as
debtor in any such proceeding.
(6) In the event of commencement of
a proceeding specified in paragraph
(d)(5) of this section, an owner or oper-
ator who has furnished a financial
statement for the purpose of dem-
onstrating financial responsibility
under this section shall be deemed to
be in violation of this paragraph until
an alternative financial assurance
demonstration acceptable to the Re-
gional Administrator is provided either
by the owner or operator or by its
trustee in bankruptcy, receiver, or
other authorized party. All parties
shall be prohibited from injecting into
the well until such alternate financial
assurance is provided.
637
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§ 144.28
40 CFR Ch. I (7-1-04 Edition)
(e) Casing and cementing requirements.
For enhanced recovery and hydro-
carbon storage wells:
(1) The owner or operator shall case
and cement the well to prevent move-
ment of fluids into or between under-
ground sources of drinking water. In
determining and specifying casing and
cementing requirements, the following
factors shall be considered:
(i) Depth to the injection zone;
(ii) Depth to the bottom of all
TJSDWs; and
(iii) Estimated maximum and aver-
age injection pressures.
(2) In addition, in determining and
specifying casing and cementing re-
quirements the Director may consider
information on:
(i) Nature of formation fluids;
(ii) Lithology of injection and con-
fining zones;
(iii) External pressure, internal pres-
sure, and axial loading;
(iv) Hole size;
(v) Size and grade of all casing
strings; and
(vi) Class of cement.
(3) The requirements in paragraphs
(e) (1) and (2) of this section need not
apply if:
(i) Regulatory controls for casing and
cementing existed at the time of drill-
ing of the well and the well is in com-
pliance with those controls; and
(ii) Well injection will not result in
the movement of fluids into an under-
ground source of drinking water so as
to create a significant risk to the
health of persons.
(4) When a State did not have regu-
latory controls for casing and cement-
ing prior to the time of the submission
of the State program to the Adminis-
trator, the Director need not apply the
casing and cementing requirements in
paragraph (e)(l) of this section if he
submits as a part of his application for
primacy, an appropriate plan for casing
and cementing of existing, newly con-
verted, and newly drilled wells in exist-
ing fields, and the Administrator ap-
proves the plan.
(f) Operating requirements. (1) Injec-
tion between the outermost casing pro-
tecting underground sources of drink-
ing water and the well bore is prohib-
ited.
(2) The owner or operator of a Class I,
II or III injection well authorized by
rule shall establish and maintain me-
chanical integrity as defined in §146.8
of this chapter until the well is prop-
erly plugged in accordance with an ap-
proved plugging and abandonment plan
pursuant to §§144.28(c) and 146.10, and a
plugging and abandonment report pur-
suant to §144.28(k) is submitted, or
until the well is converted in compli-
ance with §144.28(j). For EPA-adminis-
tered programs, the Regional Adminis-
trator may require by written notice
that the owner or operator comply
with a schedule describing when me-
chanical integrity demonstrations
shall be made.
(3) When the Director determines
that a Class I (non-hazardous), II or III
injection well lacks mechanical integ-
rity pursuant to §146.8 of this chapter,
the Director shall give written notice
of his determination to the owner or
operator. Unless the Director requires
immediate cessation, the owner or op-
erator shall cease injection into the
well within 48 hours of receipt of the
Director's determination. The Director
may allow plugging of the well in ac-
cordance with the requirements of
§146.10 of this chapter, or require the
owner or operator to perform such ad-
ditional construction, operation, moni-
toring, reporting and corrective action
as is necessary to prevent the move-
ment of fluid into or between UBDWs
caused by the lack of mechanical in-
tegrity. The owner or operator may re-
sume injection upon receipt of written
notification from the Director that the
owner or operator has demonstrated
mechanical integrity pursuant to §146.8
of this chapter.
(4) The Director may allow the owner
or operator of a well which lacks me-
chanical integrity pursuant to
§146.8(a)(l) of this chapter to continue
or resume injection if the owner or op-
erator has made a satisfactory dem-
onstration that there is no movement
of fluid into or between USDWs.
(5) For Class I wells, unless an alter-
native to a packer has been approved
under §146.12(c) of this chapter, the
owner or operator shall fill the annulus
between the tubing and the long string
of casings with a fluid approved by the
Director and maintain a pressure, also
638
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Environmental Protection Agency
§144.28
approved by the Director, on the annu-
lus. For EPA administered programs,
the owner or operator of a Class J well
completed with tubing and packer shall
fill the annulus between tubing and
casing with a noncorrosive fluid and
maintain a positive pressure on the an-
nulus. For other Class I wells, the
owner or operator shall insure that the
alternative completion method will re-
liably provide a comparable level of
protection to underground sources of
drinking water.
(6) Injection pressure.
(i) For Class I and III wells:
(A) Except during stimulation, the
owner or operator shall not exceed an
injection pressure at the wellhead
which shall be calculated so as to as-
sure that the pressure during injection
does not initiate new fractures or prop-
agate existing fractures in the injec-
tion zone; and
(B) The owner or operator shall not
inject at a pressure which will initiate
fractures in the confining zone or cause
the movement of injection or
formation fluids into an underground
source of drinking water.
(ii) For Class II wells:
(A) The owner or operator shall not
exceed a maximum injection pressure
at the wellhead which shall be cal-
culated so as to assure that the pres-
sure during injection does not initiate
new fractures of propagate existing
fractures in the confining zone adja-
cent to the USDWs; and
(B) The owner or operator shall not
inject at a pressure which will cause
the movement of injection or forma-
tion fluids into an underground source
of drinking water.
(g) Monitoring requirements. The
owner or operator shall perform the
monitoring as described in this para-
graph. For EPA administered pro-
grams, monitoring of the nature of the
injected fluids shall comply with appli-
cable analytical methods cited and de-
scribed in table I of 40 CFR 136.3 or in
appendix HI of 40 CFR part 261 or by
other methods that have been approved
by the Regional Administrator.
(1) The owner or operator of a Class I
well shall:
(i) Analyze the nature of the injected
fluids with sufficient frequency to
yield data representative of their char-
acteristics;
(ii) Install and use continuous record-
ing devices to monitor Injection pres-
sure, flow rate and volume, and the
pressure on the annulus between the
tubing and the long string of casing;
(iii) Install and use monitoring wells
within the area of review if required by
the Director, to monitor any migration
of fluids into and pressure in the under-
ground sources of drinking water. The
type, number and location of the wells,
the parameters to be measured, and the
frequency of monitoring must be ap-
proved by the Director.
(2) For Class II wells:
(i) The owner or operator shall mon-
itor the nature of the injected fluids
with sufficient frequency to yield data
representative of their characteristics.
For EPA administered programs, this
frequency shall be at least once within
the first year of the authorization and
thereafter when changes are made to
the fluid.
(ii) The owner or operator shall ob-
serve the injection pressure, flow rate,
and cumulative volume at least with
the following frequencies:
(A) Weekly for produced fluid dis-
posal operations;
(B) Monthly for enhanced recovery
operations;
(C) Daily during the injection of liq-
uid hydrocarbons and injection for
withdrawal of stored hydrocarbons; and
(D) Daily during the injection phase
of cyclic steam operations.
(iii) The owner or operator shall
record one observation of injection
pressure, flow rate and cumulative vol-
ume at reasonable intervals no greater
than thirty days.
(iv) For enhanced recovery and hy-
drocarbon storage wells:
(A) The owner or operator shall dem-
onstrate mechanical integrity pursu-
ant to §146.8 of this chapter at least
once every five years during the life of
the injection well,
(B) For EPA administered programs,
the Regional Administrator by written
notice may require the owner or oper-
ator to comply with a schedule describ-
ing when such demonstrations shall be
made.
639
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§144.28
40 CFR Ch. I (7-1-04 Edition)
(C) For EPA administered programs,
the owner or operator of any well re-
quired to be tested for mechanical in-
tegrity shall notify the Regional Ad-
ministrator at least 30 days prior to
any required mechanical integrity test.
The Regional Administrator may allow
a shorter notification period if it would
be sufficient to enable EPA to witness
the mechanical integrity testing if it
chose. Notification may be in the form
of a yearly or quarterly schedule of
planned mechanical integrity tests, or
it may be on an individual basis.
(v) The owner or operator of a hydro-
carbon storage or enhanced recovery
wells may monitor them by manifold
monitoring on a field or project basis
rather than on an individual well basis
if such facilities consist of more than
one injection well, operate with a com-
mon manifold, and provided the owner
or operator demonstrates to the Direc-
tor that manifold monitoring is com-
parable to individual well monitoring.
(3)(i) For Class III wells the owner or
operator shall provide to the Director a
qualitative analysis and ranges in con-
centrations of all constituents of in-
jected fluids at least once within the
first year of authorization and there-
after whenever the injection fluid is
modified to the extent that the initial
data are incorrect or incomplete. The
owner or operator may request Federal
confidentiality as specified in 40 CFR
part 2. If the information is proprietary
the owner or operator may in lieu of
the ranges in concentrations choose to
submit maximum concentrations
which shall not be exceeded. In such a
case the owner or operator shall retain
records of the undisclosed concentra-
tions and provide them upon request to
the Regional Administrator as part of
any enforcement investigation; and
(ii) Monitor injection pressure and ei-
ther flow rate or volume semi-monthly,
or meter and record daily injected and
produced fluid volumes as appropriate;
(iii) Monitor the fluid level in the in-
jection zone semi-monthly, where ap-
propriate;
(iv) All Class III wells may be mon-
itored on a field or project basis rather
than an individual well basis by mani-
fold monitoring. Manifold monitoring
may be used in cases of facilities con-
sisting of more than one injection well,
operating with a common manifold.
Separate monitoring systems for each
well are not required provided the
owner or operator demonstrates to the
Director that manifold monitoring is
comparable to individual well moni-
toring.
(h) Reporting requirements. The owner
or operator shall submit reports to the
Director as follows:
(1) For Class I wells, quarterly re-
ports on:
(i) The physical, chemical, and other
relevant characteristics of the injec-
tion fluids;
(ii) Monthly average, maximum, and
minimum values for injection pressure,
flow rate and volume, and annular
pressure;
(iii) The results from ground-water
monitoring wells prescribed in para-
graph (g)(l)(iii) of this section;
(iv) The results of any test of the in-
jection well conducted by the owner or
operator during the reported quarter if
required by the Director; and
(v) Any well work over performed
during the reported quarter,
(2) For Class II wells:
(i) An annual report to the Director
summarizing the results of all moni-
toring, as required in paragraph (gO(2)
of this section. Such summary shall in-
clude monthly records of injected
fluids, and any major changes in char-
acteristics or sources of injected fluids.
Previously submitted information may
be included by reference.
(ii) The owner or operator of hydro-
carbon storage and enhanced recovery
projects may report on a field or
project basis rather than on an indi-
vidual well basis where manifold moni-
toring is used.
(3) For Class III wells:
(i) Quarterly reporting on all moni-
toring, as required in paragraph (g)(3)
of this section;
(ii) Quarterly reporting of the results
of any periodic tests required by the
Director that are performed during the
reported quarter;
(iii) Monitoring may be reported on a
project or field basis rather than an in-
dividual well basis where manifold
monitoring is used.
(i) Retention of records. The owner or
operator shall retain records of all
640
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Environmental Protection Agency
§144.31
monitoring information, including the
following:
(1) Calibration and maintenance
records and all original strip chart re-
cordings for continuous monitoring in-
strumentation, and copies of all re-
ports required by this section, for a pe-
riod of at least three years from the
date of the sample, measurement, or
report. This period may be extended by
request of the Director at any time;
and
(2) The nature and composition of all
injected fluids until three years after
the completion of any plugging and
abandonment procedures specified
under §144.52(1)(6). The Director may
require the owner or operator to de-
liver the records to the Director at the
conclusion of the retention period. For
EPA administered programs, the owner
or operator shall continue to retain the
records after the three year retention
period unless he delivers the records to
the Regional Administrator or obtains
written approval from the Regional Ad-
ministrator to discard the records.
(j) Notice of abandonment. (1) The
owner or operator shall notify the Di-
rector, according to a time period re-
quired by the Director, before conver-
sion or abandonment of the well.
(2) For EPA-administered programs,
the owner or operator shall notify the
Regional Administrator at least 45
days before plugging and abandonment.
The Regional Administrator, at his dis-
cretion, may allow a shorter notice pe-
riod.
(k) Plugging and abandonment report,
For EPA-administered programs, with-
in 80 days after plugging a well or at
the time of the next quarterly report
(whichever is less) the owner or oper-
ator shall submit a report to the Re-
gional Administrator, If the quarterly
report is due less than 15 days before
completion of plugging, then the report
shall be submitted within 60 days. The
report shall be certified as accurate by
the person who performed the plugging
operation. Such report shall consist of
either:
(1) A statement that the well was
plugged in accordance with the plan
previously submitted to the Regional
Administrator; or
(2) Where actual plugging differed
from the plan previously submitted, an
updated version of the plan, on the
form supplied by the Regional Admin-
istrator, specifying the different proce-
dures used.
(1) Change of ownership or operational
control. For EPA-administered pro-
grams:
(1) The transferor of a Class I, II or
III well authorized by rule shall notify
the Regional Administrator of a trans-
fer of ownership or operational control
of the well at least 30 days in advance
of the proposed transfer.
(2) The notice shall include a written
agreement between the transferor and
the transferee containing a specific
date for transfer of ownership or oper-
ational control of the well; and a spe-
cific date when the financial responsi-
bility demonstration of §144.28(d) will
be met "by the transferee.
(3) The transferee is authorized to in-
ject unless he receives notification
from the Director that the transferee
has not demonstrated financial respon-
sibility pursuant to §144.28(d).
(m) Requirements for Class I hazardous
waste wells. The owner or operator of
any Class I well injecting hazardous
waste shall comply with §144.14(c). In
addition, for EPA-administered pro-
grams the owner or operator shall
properly dispose of, or decontaminate
by removing all hazardous waste resi-
dues, all injection well equipment.
[49 FR 20182, May 11. 1984, as amended at 58
PR 63897, Dec. 3, 1993]
Subpart D—Authorization by
Permit
§144.31 Application for a permit; au-
thorization by permit.
(a) Permit application. Unless an un-
derground injection well is authorized
by rule under subpart C of this part, all
injection activities including construc-
tion of an injection well are prohibited
until the owner or operator is author-
ized by permit. An owner or operator of
a well currently authorized by rule
must apply for a permit under this sec-
tion unless well authorization by rule
was for the life of the well or project.
Authorization by rule for a well or
project for which a permit application
has been submitted terminates for the
well or project upon the effective date
641
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§144.31
40 CFR Ch. 1 (7-1-04 Edition)
of the permit. Procedures for applica-
tions, issuance and administration of
emergency permits are found exclu-
sively in § 144.34, A BCRA permit apply-
ing the standards of part 264, subpart C
of this chapter will constitute a UIC
permit for hazardous waste injection
wells for which the technical standards
in part 146 of this chapter are not gen-
erally appropriate,
(b) Who applies? When a facility or ac-
tivity is owned by one person but is op-
erated by another person, it is the op-
erator's duty to obtain a permit.
(c) Time to apply. Any person who per-
forms or proposes an underground in-
jection for which a permit is or will be
required shall submit an application to
the Director in accordance with the
UIC program as follows:
(1) For existing wells, as expedi-
tiously as practicable and in accord-
ance with the schedule in any program
description under §145.23(f) or (for EPA
administered programs) on a schedule
established by the Regional Adminis-
trator, but no later than 4 years from
the approval or promulgation of the
UIC program, or as required under
§144,14Cb) for wells injecting hazardous
waste. For EPA administered programs
the owner or operator of Class I or III
wells shall submit a complete permit
application no later than 1 year after
the effective date of the program.
(2) For new injection wells, except
new wells in projects authorized under
§144.21(d) or authorized by an existing
area permit under §144.33(c), a reason-
able time before construction is ex-
pected to begin.
(d) Completeness. The Director shall
not issue a permit before receiving a
complete application for a permit ex-
cept for emergency permits. An appli-
cation for a permit is complete when
the Director receives an application
form and any supplemental informa-
tion which are completed to his or her
satisfaction. The completeness of any
application for a permit shall be judged
independently of the status of any
other permit application or permit for
the same facility or activity. For BPA-
administered programs, an application
which is reviewed under §124.3 is com-
plete when the Director receives either
a complete application or the informa-
tion listed in a notice of deficiency.
(e) Information requirements. All appli-
cants for permits shall provide the fol-
lowing information to the Director,
using the application form provided by
the Director.
(1) The activities conducted by the
applicant which require it to obtain
permits under RCRA, UIC, the Na-
tional Pollution Discharge Elimination
system (NPDBS) program under the
Clean Water Act, or the Prevention of
Significant Deterioration (PSD) pro-
gram under the Clean Air Act.
(2) Name, mailing address, and loca-
tion of the facility for which the appli-
cation is submitted.
(3) Up to four SIC codes which best
reflect the principal products or serv-
ices provided by the facility.
(4) The operator's name, address,
telephone number, ownership status,
and status as Federal, State, private,
public, or other entity.
(5) Whether the facility is located on
Indian lands.
(6) A listing of all permits or con-
struction approvals received or applied
for under any of the following pro-
grams:
(i) Hazardous Waste Management
program under RCRA.
(ii) UIC program under SDWA.
(iii) NPDES program under CWA.
(iv) Prevention of Significant Dete-
rioration (PSD) program under the
Clean Air Act.
(v) Nonattainment program under
the Clean Air Act.
(vi) National Emission Standards for
Hazardous Pollutants (NESHAPS)
preconstruction approval under the
Clean Air Act.
(vii) Ocean dumping permits under
the Marine Protection Research and
Sanctuaries Act.
(viii) Dredge and fill permits under
section 404 of CWA.
(ix) Other relevant environmental
permits, including State permits.
(7) A topographic map (or other map
if a topographic map is unavailable) ex-
tending one mile beyond the property
boundaries of the source depicting the
facility and each of its intake and dis-
charge structures; each of its haz-
ardous waste treatment, storage, or
disposal facilities; each well where
fluids from the facility are injected un-
derground; and those wells, springs,
642
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Environmental Protection Agency
§144.32
and other surface water bodies, and
drinking water wells listed in public
records or otherwise known to the ap-
plicant within a quarter mile of the fa-
cility property boundary.
(8) A brief description of the nature
of the business.
(9) For EPA-administered programs,
the applicant shall identify and submit
on a list with the permit application
the names and addresses of all owners
of record of land within one-quarter
mile of the facility boundary. This
requirement may be waived by the
Regional Administrator where the site
is located in a populous area and the
Regional Administrator determines
that the requirement would be imprac-
ticable.
(10) A plugging and abandonment
plan that meets the requirements of
§146.10 of this chapter and is acceptable
to the Director.
(f) Recordkeeping. Applicants shall
keep records of all data used to com-
plete permit applications and any sup-
plemental information submitted
under §144.31 for a period of at least 3
years from the date the application is
signed.
(g) Information Requirements for Class
I Hazardous Waste Injection Wells Per-
mits. (1) The following information is
required for each active Class I haz-
ardous waste injection well at a facil-
ity seeking a UIC permit:
(i) Dates well was operated.
(ii) Specification of all wastes which
have been injected in the well, if avail-
able.
(2) The owner or operator of any fa-
cility containing one or more active
hazardous waste injection wells must
submit all available information per-
taining to any release of hazardous
waste or constituents from any active
hazardous waste injection well at the
facility.
(3) The owner or operator of any fa-
cility containing one or more active
Class I hazardous waste injection wells
must conduct such preliminary site in-
vestigations as are necessary to deter-
mine whether a release is occurring,
has occurred, or is likely to have oc-
curred.
[48 FR 14189, Apr. 1, 1983, as amended at 49
FR 20185, May 11, 1984; 52 FR 45797, Dec. 1,
1987; 52 FE 46963, Dec. 10, 1987; 58 PR 63897,
Dec. 3, 1993]
§144.32 Signatories to permit applica-
tions and reports.
(a) Applications, All permit applica-
tions, except those submitted for Class
II wells (see paragraph (b) of this sec-
tion), shall be signed as follows:
(1) For a corporation: by a responsible
corporate officer. For the purpose of
this section, a responsible corporate of-
ficer means; (i) A president, secretary,
treasurer, or vice president of the cor-
poration in charge of a principal busi-
ness function, or any other person who
performs similar policy- or decision-
making functions for the corporation,
or (ii) the manager of one or more man-
ufacturing, production, or operating fa-
cilities employing more than 250 per-
sons or having gross annual sales or ex-
penditures exceeding $25 million (in
second-quarter I960 dollars), if author-
ity to sign documents has been as-
signed or delegated to the manager in
accordance with corporate procedures.
NOTE; EPA does not require specific assign-
ments or delegations of authority to respon-
sible corporate officers identified in
§144.32(a)(l)(i). The Agency will presume that
these responsible corporate officers have the
requisite authority to sign permit applica-
tions unless the corporation has notified the
Director to the contrary. Corporate proce-
dures governing authority to sign permit ap-
plications may provide for assignment or
delegation to applicable corporate positions
under §144.32(a)(l)(ii) rather than to specific
individuals.
(2) For a partnership or sole proprietor-
ship: by a general partner or the propri-
etor, respectively; or
(3) For a municipality, State, Federal,
or other public agency: by either a prin-
cipal executive officer or ranking elect-
ed official. For purposes of this section,
a principal executive officer of a Fed-
eral agency includes: (i) The chief exec-
utive officer of the agency, or (ii) a
senior executive officer having respon-
sibility for the overall operations of a
principal geographic unit of the agency
(e.g., Regional Administrators of EPA).
(b) Reports. All reports required by
permits, other information requested
643
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§144.33
40 CFR Ch. I (7-1-04 Edition)
by the Director, and all permit applica-
tions submitted for Class II wells under
§144.31 shall be signed by a person de-
scribed in paragraph (a) of this section,
or by a duly authorized representative
of that person. A person is a duly au-
thorized representative only if:
(1) The authorization is made in writ-
ing by a person described in paragraph
(a) of this section;
(2) The authorization specifies either
an individual or a position having- re-
sponsibility for the overall operation of
the regulated facility or activity, such
as the position of plant manager, oper-
ator of a well or a well field, super-
intendent, or position of equivalent re-
sponsibility. (A duly authorized rep-
resentative may thus be either a
named individual or any individual oc-
cupying a named position); and
(3) The written authorization is sub-
mitted to the Director.
(c) Changes to authorization. If an au-
thorization under paragraph (b) of this
section is no longer accurate because a
different individual or position has re-
sponsibility for the overall operation of
the facility, a new authorization satis-
fying the requirements of paragraph (b)
of this section must be submitted to
the Director prior to or together with
any reports, information, or applica-
tions to be signed by an authorized rep-
resentative.
(d) Certification, Any person signing a
document under paragraph (a) or (b) of
this section shall make the following
certification:
I certify under penalty of law that this
document and all attachments were prepared
under my direction or supervision in accord-
ance with a system designed to assure that
qualified personnel properly gather and
evaluate the information submitted. Based
on my inquiry of the person or persons who
manage the system, or those persons directly
responsible for gathering the information,
the information submitted is, to the best of
my knowledge and belief, true, accurate, and
complete. I am aware that there are signifi-
cant penalties for submitting false informa-
tion, including the possibility of fine and im-
prisonment for knowing violations.
(Clean Water Act (33 U.S.C. 1251 et seq.), Safe
Drinking Water Act (42 U.S.C. 300f et seq.),
Clean Air Act (42 U.S.C. 7401 et seq.),
Resource Conservation and Recovery Act (42
U.S.C. 6901 et seq.)
[48 PR 14189, Apr. 1, 1983, as amended at 48
FB 39621, Sept. 1, 1983]
§ 144.33 Area permits.
(a) The Director may issue a permit
on an area basis, rather than for each
well individually, provided that the
permit is for injection wells:
(1) Described and identified by loca-
tion in permit application(s) if they are
existing wells, except that the Director
may accept a single description of
wells with substantially the same char-
acteristics;
(2) Within the same well field, facil-
ity site, reservoir, project, or similar
unit in the same State;
(3) Operated by a single owner or op-
erator; and
(4) Used to inject other than haz-
ardous waste,
(b) Area permits shall specify:
(1) The area within which under-
ground injections are authorized, and
(2) The requirements for construc-
tion, monitoring, reporting', operation,
and abandonment, for all wells author-
ized by the permit.
(c) The area permit may authorize
the permittee to construct and operate,
convert, or plug and abandon wells
within the permit area provided:
(1) The permittee notifies the Direc-
tor at such time as the permit requires;
(2) The additional well satisfies the
criteria in paragraph (a) of this section
and meets the requirements specified
in the permit under paragraph (b) of
this section; and
(3) The cumulative effects of drilling
and operation of additional injection
wells are considered by the Director
during evaluation of the area permit
application and are acceptable to the
Director.
(d) If the Director determines that
any well constructed pursuant to para-
graph (c) of this section does not sat-
isfy any of the requirements of para-
graphs (c) (1) and (2) of this section the
Director may modify the permit under
§144.39, terminate under §144.40, or
644
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Environmental Protection Agency
§144.37
take enforcement action. If the Direc-
tor determines that cumulative effects
are unacceptable, the permit may be
modified under § 144,39.
§ 144.34 Emergency permits.
(a) Coverage, Notwithstanding any
other provision of this part or part 124,
the Director may temporarily permit a
specific underground injection if:
(1) An imminent and substantial
endangerment to the health of persons
will result unless a temporary emer-
gency permit is granted; or
(2) A substantial and irretrievable
loss of oil or gas resources will occur
unless a temporary emergency permit
is granted to a Class II well; and
(i) Timely application for a permit
could not practicably have been made;
and
(ii) The injection will not result in
the movement of fluids into under-
ground sources of drinking water; or
(3) A substantial delay in production
of oil or gas resources will occur unless
a temporary emergency permit is
granted to a new Class II well and the
temporary authorization will not re-
sult in the movement of fluids into an
underground source of drinking water,
(b) Requirements for issuance. (I) Any
temporary permit under paragraph
(a)(l) of this section shall be for no
longer term than required to prevent
the hazard.
(2) Any temporary permit under
paragraph (a)(2) of this section shall be
for no longer than 90 days, except that
if a permit application has been sub-
mitted prior to the expiration of the 90-
day period, the Director may extend
the temporary permit until final action
on the application.
(3) Any temporary permit under
paragraph (a)(3) of this section shall be
issued only after a complete permit ap-
plication has been submitted and shall
be effective until final action on the
application.
(4) Notice of any temporary permit
under this paragraph shall be published
in accordance with §124.11 within 10
days of the issuance of the permit.
(5) The temporary permit under this
section may be either oral or written.
If oral, it must be followed within 5
calendar days by a written temporary
emergency permit.
(6) The Director shall condition the
temporary permit in any manner he or
she determines is necessary to ensure
that the injection will not result in the
movement of fluids into an under-
ground source of drinking water.
[48 PR 14189, Apr. 1. 1983, as amended at 49
PR 20185, May 11, 1984]
i 144.35 Effect of a permit.
(a) Except for Class II and III wells,
compliance with a permit during its
term constitutes compliance, for pur-
poses of enforcement, with Part C of
the SDWA. However, a permit may be
modified, revoked and reissued, or ter-
minated during its term for cause as
set forth in §§144.39 and 144.40.
(b) The issuance of a permit does not
convey any property rights of any sort,
or any exclusive privilege.
(c) The issuance of a permit does not
authorize any injury to persons or
property or invasion of other private
rights, or any infringement of State or
local law or regulations.
§ 144.36 Duration of permits.
(a) Permits for Class I and Class V
wells shall be effective for a fixed term
not to exceed 10 years. UIC permits for
Class II and III wells shall be issued for
a period up to the operating life of the
facility. The Director shall review each
issued Class II or III well UIC permit at
least once every 5 years to determine
whether it should be modified, revoked
and reissued, terminated, or a minor
modification made as provided in
§§144.39, 144.40, and 144.41.
(b) Except as provided in §144,37, the
term of a permit shall not be extended
by modification beyond the maximum
duration specified in this section.
(c) The Director may issue any per-
mit for a duration that is less than the
full allowable term under this section.
§ 144.37 Continuation of expiring per-
mits.
(a) EPA permits. When EPA is the per-
mit-issuing authority, the conditions
of an expired permit continue in force
under 5 U.S.C. 558(c) until the effective
date of a new permit if:
(1) The permittee has submitted a
timely application which is a complete
application for a new permit; and
645
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§144.38
40 CFR Ch. I (7-1-04 Edition)
(2) The Regional Administrator,
through no fault of the permittee does
not issue a new permit with an effec-
tive date on or before the expiration
date of the previous permit (for exam-
ple, when issuance is impracticable due
to time or resource constraints),
(b) Effect. Permits continued under
this section remain fully effective and
enforceable.
(c) Enforcement. When the permittee
is not in compliance with the condi-
tions of the expiring or expired permit
the Regional Administrator may
choose to do any or all of the following:
(1) Initiate enforcement action based
upon the permit which has been contin-
ued;
(2) Issue a notice of intent to deny
the new permit. If the permit is denied,
the owner or operator would then be
required to cease the activities author-
ized by the continued permit or be sub-
ject to enforcement action for oper-
ating without a permit;
(3) Issue a new permit under part 124
with appropriate conditions; or
(4) Take other actions authorized by
these regulations.
(d) State continuation. An EPA issued
permit does not continue in force be-
yond its time expiration date under
Federal law if at that time a State is
the permitting authority, A State au-
thorized to administer the UIC pro-
gram may continue either EPA or
State-issued permits until the effective
date of the new permits, if State law
allows. Otherwise, the facility or activ-
ity is operating without a permit from
the time of expiration of the old permit
to the effective date of the State-issued
new permit.
§ 144,38 Transfer of permits.
(a) Transfers by modification. Except
as provided in paragraph (b) of this sec-
tion, a permit may be transferred by
the permittee to a new owner or oper-
ator only If the permit has been modi-
fied or revoked and reissued (under
§144.39(b)(2)), or a minor modification
made (under §144.41(d)), to identify the
new permittee and incorporate such
other requirements as may be nec-
essary under the Safe Drinking Water
Act.
(b) Automatic transfers. As an alter-
native to transfers under paragraph (a)
of this section, any UIC permit for a
well not injecting hazardous waste may
be automatically transferred to a new
permittee if:
(1) The current permittee notifies the
Director at least 30 days in advance of
the proposed transfer date referred to
in paragraph (b)(2) of this section;
(2) The notice includes a written
agreement between the existing and
new permittees containing a specific
date for transfer or permit responsi-
bility, coverage, and liability between
them, and the notice demonstrates
that the financial responsibility re-
quirements of §144.52(a)(7) will be met
by the new permittee; and
(3) The Director does not notify the
existing permittee and the proposed
new permittee of his or her intent to
modify or revoke and reissue the per-
mit. A modification under this para-
graph may also be a minor modifica-
tion under §144.41. If this notice is not
received, the transfer is effective on
the date specified in the agreement
mentioned in paragraph (b)(2) of this
section.
§144.39 Modification or revocation
and reisssuanco of permits.
When the Director receives any infor-
mation (for example, inspects the facil-
ity, receives information submitted by
the permittee as required in the permit
(see §144.51 of this chapter), receives a
request for modification or revocation
and reissuance under §124.5, or con-
ducts a review of the permit file) he or
she may determine whether or not one
or more of the causes listed in para-
graphs (a) and (b) of this section for
modification or revocation and
reissuance or both exist. If cause ex-
ists, the Director may modify or re-
voke and reissue the permit accord-
ingly, subject to the limitations of
paragraph (c) of this section, and may
request an updated application if nec-
essary. When a permit is modified, only
the conditions subject to modification
are reopened. If a permit is revoked
and reissued, the entire permit is re-
opened and subject to revision and the
permit is reissued for a new term. See
§124.5(c)(2) of this chapter. If cause
does not exist under this section or
§144.41 of this chapter, the Director
shall not modify or revoke and reissue
646
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Environmental Protection Agency
§ 144,39
the permit. If a permit modification
satisfies the criteria in §144.41 for
"minor modifications" the permit may
be modified without a draft permit or
public review. Otherwise, a draft per-
mit must be prepared and other proce-
dures in part 124 must be followed.
(a) Causes for modification. The fol-
lowing are causes for modification. For
Class I hazardous waste injection wells,
Class II, or Class III wells the following
may be causes for revocation and
reissuance as well as modification; and
for all other wells the following may be
cause for revocation or reisauance as
well as modification when the per-
mittee requests or agrees.
(1) Alterations. There are material and
substantial alterations or additions to
the permitted facility or activity
which occurred after permit issuance
which justify the application of permit
conditions that are different or absent
in the existing permit.
(2) Information. The Director has re-
ceived information. Permits other than
for Class II and III wells may be modi-
fied during their terms for this cause
only if the information was not avail-
able at the time of permit issuance
(other than revised regulations, guid-
ance, or test methods) and would have
justified the application of different
permit conditions at the time of
issuance. For UIC area permits
(§144.33), this cause shall include any
information indicating that cumu-
lative effects on the environment are
unacceptable.
(3) New regulations. The standards or
regulations on which the permit was
based have been changed by promulga-
tion of new or amended standards or
regulations or by judicial decision
after the permit was issued. Permits
other than for Class I hazardous waste
injection wells, Class II, or Class III
wells may be modified during their
terms for this cause only as follows:
(i) For promulgation of amended
standards or regulations, when:
(A) The permit condition requested
to be modified was based on a promul-
gated part 146 regulation; and
(B) EPA has revised, withdrawn, or
modified that portion of the regulation
on which the permit condition was
based, and
(C) A permittee requests modifica-
tion in accordance with §124.5 within
ninety (90) days after FEDERAL REG-
ISTER notice of the action on which the
request is based.
(ii) For judicial decisions, a court of
competent jurisdiction has remanded
and stayed EPA promulgated regula-
tions if the remand and stay concern
that portion of the regulations on
which the permit condition was based
and a request is filed by the permittee
in accordance with §124.5 within ninety
(90) days of judicial remand.
(4) Compliance schedules. The Director
determines good cause exists for modi-
fication of a compliance schedule, such
as an act of God, strike, flood, or mate-
rials shortage or other events over
which the permittee has little or no
control and for which there is no rea-
sonably available remedy. See also
§144.41(c) (minor modifications).
(b) Causes for modification or revoca-
tion and reissuance. The following are
causes to modify or, alternatively, re-
voke and reissue a permit:
(1) Cause exists for termination
under §144.40, and the Director deter-
mines that modification or revocation
and reissuance is appropriate.
(2) The Director has received notifi-
cation (as required in the permit, see
§144.41(d)) of a proposed transfer of the
permit. A permit also may be modified
to reflect a transfer after the effective
date of an automatic transfer
(§144.38(b)) but will not be revoked and
reissued after the effective date of the
transfer except upon the request of the
new permittee.
(3) A determination that the waste
being injected is a hazardous waste as
defined in §261.3 either because the def-
inition has been revised, or because a
previous determination has been
changed.
(c) Facility siting. Suitability of the
facility location will not be considered
at the time of permit modification or
revocation and reissuance unless new
information or standards indicate that
a threat to human health or the envi-
ronment exists which was unknown at
the time of permit issuance.
[48 FB 14189, Apr. 1, 1983, as amended at 53
FE 28147. July 26, 1988]
647
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§144.40
40 CFR Ch, I (7-1-04 Edition)
§ 144.40 Termination of permits.
(a) The Director may terminate a
permit during its term, or deny a per-
mit renewal application for the fol-
lowing causes:
(1) Noncompliance by the permittee
with any condition of the permit;
(2) The permittee's failure in the ap-
plication or during the permit issuance
process to disclose fully all relevant
facts, or the permittee's misrepresenta-
tion of any relevant facts at any time;
or
(3) A determination that the per-
mitted activity endangers human
health or the environment and can
only be regulated to acceptable levels
by permit modification or termination;
(b) The Director shall follow the
applicable procedures in part 124 in
terminating any permit under this sec-
tion.
§ 144.41 Minor modifications of per-
mits.
Upon the consent of the permittee,
the Director may modify a permit to
make the corrections or allowances for
changes in the permitted activity list-
ed in this section, without following
the procedures of part 124. Any permit
modification not processed as a minor
modification under this section must
be made for cause and with part 124
draft permit and public notice as re-
quired in §144.39. Minor modifications
may only:
(a) Correct typographical errors;
(b) Require more frequent monitoring
or reporting by the permittee;
(c) Change an interim compliance
date in a schedule of compliance, pro-
vided the new date is not more than 120
days after the date specified in the ex-
isting permit and does not interfere
with attainment of the final compli-
ance date requirement; or
(d) Allow for a change in ownership
or operational control of a facility
where the Director determines that no
other change in the permit is nec-
essary, provided that a written agree-
ment containing a specific date for
transfer of permit responsibility, cov-
erage, and liability between the cur-
rent and new permittees has been sub-
mitted to the Director.
(e) Change quantities or types of
fluids injected which are within the ca-
pacity of the facility as permitted and,
in the judgment of the Director, would
not interfere with the operation of the
facility or its ability to meet condi-
tions described in the permit and would
not change its classification.
(f) Change construction requirements
approved by the Director pursuant to
§144.52(a)(l) (establishing UIC permit
conditions), provided that any such al-
teration shall comply with the require-
ments of this part and part 146.
(g) Amend a plugging and abandon-
ment plan which has been updated
under §144.52(a)(6).
Subpart E—Permit Conditions
§ 144.51 Conditions applicable to all
permits.
The following conditions apply to all
UIC permits. All conditions applicable
to all permits shall be incorporated
into the permits either expressly or by
reference. If incorporated by reference,
a specific citation to these regulations
(or the corresponding approved State
regulations) must be given in the per-
mit.
(a) Duty to comply. The permittee
must comply with all conditions of this
permit. Any permit noncompliance
constitutes a violation of the Safe
Drinking Water Act and is grounds for
enforcement action; for permit termi-
nation, revocation and reissuance, or
modification; or for denial of a permit
renewal application; except that the
permittee need not comply with the
provisions of this permit to the extent
and for the duration such noncompli-
ance is authorized in an emergency
permit under §144.34.
(b) Duty to reapply. If the permittee
wishes to continue an activity regu-
lated by this permit after the expira-
tion date of this permit, the permittee
must apply for and obtain a new
permit.
(c) Need to halt or reduce activity not a
defense. It shall not be a defense for a
permittee in an enforcement action
that it would have been necessary to
halt or reduce the permitted activity
in order to maintain compliance with
the conditions of this permit.
(d) Duty to mitigate. The permittee
shall take all reasonable steps to mini-
mize or correct any adverse impact on
648
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Environmental Protection Agency
§144.51
the environment resulting from non-
compliance with this permit.
(e) Proper operation and maintenance.
The permittee shall at all times prop-
erly operate and maintain all facilities
and systems of treatment and control
(and related appurtenances) which are
installed or used by the permittee to
achieve compliance with the conditions
of this permit. Proper operation and
maintenance includes effective per-
formance, adequate funding, adequate
operator staffing and training, and ade-
quate laboratory and process controls,
including appropriate quality assur-
ance procedures. This provision re-
quires the operation of back-up or aux-
iliary facilities or similar systems only
when necessary to achieve compliance
with the conditions of the permit.
(f) Permit actions. This permit may be
modified, revoked and reissued, or ter-
minated for cause. The filing of a re-
quest by the permittee for a permit
modification, revocation and reissu-
ance, or termination, or a notification
of planned changes or anticipated non-
compliance, does not stay any permit
condition.
(g) Property rights. This permit does
not convey any property rights of any
sort, or any exclusive privilege.
(h) Duty to provide information. The
permittee shall furnish to the Director,
within a time specified, any informa-
tion which the Director may request to
determine whether cause exists for
modifying, revoking and reissuing, or
terminating this permit, or to deter-
mine compliance with this permit. The
permittee shall also furnish to the Di-
rector, upon request, copies of records
required to be kept by this permit.
(i) Inspection and entry. The per-
mittee shall allow the Director, or an
authorized representative, upon the
presentation of credentials and other
documents as may be required by law,
to:
(1) Enter upon the permittee's prem-
ises where a regulated facility or activ-
ity is located or conducted, or where
records must be kept under the condi-
tions of this permit;
(2) Have access to and copy, at rea-
sonable times, any records that must
be kept under the conditions of this
permit;
(3) Inspect at reasonable times any
facilities, equipment (including moni-
toring and control equipment), prac-
tices, or operations regulated or re-
quired under this permit; and
(4) Sample or monitor at reasonable
times, for the purposes of assuring per-
mit compliance or as otherwise author-
ized by the SDWA, any substances or
parameters at any location.
(j) Monitoring and records. (1) Samples
and measurements taken for the pur-
pose of monitoring shall be representa-
tive of the monitored activity.
(2) The permittee shall retain records
of all monitoring information, includ-
ing the following:
(i) Calibration and maintenance
records and all original strip chart re-
cordings for continuous monitoring in-
strumentation, copies of all reports re-
quired by this permit, and records of
all data used to complete the applica-
tion for this permit, for a period of at
least 3 years from the date of the sam-
ple, measurement, report, or applica-
tion. This period may be extended by
request of the Director at any time;
and
(it) The nature and composition of all
injected fluids until three years after
the completion of any plugging and
abandonment procedures specified
under §144.62(a)(6), or under part 148
subpart G as appropriate. The Director
may require the owner or operator to
deliver the records to the Director at
the conclusion of the retention period.
For EPA administered programs, the
owner or operator shall continue to re-
tain the records after the three year re-
tention period unless he delivers the
records to the Regional Administrator
or obtains written approval from the
Regional Administrator to discard the
records.
(3) Records of monitoring informa-
tion shall include:
(i) The date, exact place, and time of
sampling or measurements;
(ii) The individual(s) who performed
the sampling or measurements;
(ill) The date(s) analyses were per-
formed;
(iv) The individual(s) who performed
the analyses;
(v) The analytical techniques or
methods used; and
(vi) The results of such analyses.
649
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§144.51
40 CFR Ch. i (7-1-04 Edition)
(k) Signatory requirement. All applica-
tions, reports, or information sub-
mitted to the Administrator shall be
signed and certified. (See §144.32.)
(1) Reporting requirements. (1) Planned
changes. The permittee shall give no-
tice to the Director as soon as possible
of any planned physical alterations or
additions to the permitted facility.
(2) Anticipated noncompliance. The
permittee shall give advance notice to
the Director of any planned changes in
the permitted facility or activity
which may result in noncompliance
with permit requirements.
(3) Transfers, This permit is not
transferable to any person except after
notice to the Director. The Director
may require modification or revocation
and reissuance of the permit to change
the name of the permittee and incor-
porate such other requirements as may
be necessary under the Safe Drinking
Water Act. (See §144.38; in some cases,
modification or revocation and
reissuance is mandatory.)
(4) Monitoring reports. Monitoring re-
sults shall be reported at the intervals
specified elsewhere in this permit.
(5) Compliance schedules. Reports of
compliance or noncompliance with, or
any progress reports on, interim and
final requirements contained in any
compliance schedule of this permit
shall be submitted no later than 30
days following each schedule date.
(6) Twenty-four hour reporting. The
permittee shall report any noncompli-
ance which may endanger health or the
environment, including:
(i) Any monitoring or other informa-
tion which indicates that any contami-
nant may cause an endangerment to a
USDW; or
(ii) Any noncompliance with a permit
condition or malfunction of the injec-
tion system which may cause fluid mi-
gration into or between USDWs,
Any information shall be provided oral-
ly within 24 hours from the time the
permittee becomes aware of the cir-
cumstances. A written submission
shall also be provided within 5 days of
the time the permittee becomes aware
of the circumstances. The written sub-
mission shall contain a description of
the noncompliance and its cause, the
period of noncompliance, including
exact dates and times, and if the non-
compliance has not been corrected, the
anticipated time it is expected to con-
tinue: and steps taken or planned to re-
duce, eliminate, and prevent reoccur-
rence of the noncompliance.
(7) Other noncompliance. The per-
mittee shall report all instances of
noncompliance not reported under
paragraphs (1) (4), (5), and (6) of this
section, at the time monitoring reports
are submitted. The reports shall con-
tain the information listed in para-
graph (1)(6) of this section.
(8) Other information. Where the per-
mittee becomes aware that it failed to
submit any relevant facts in a permit
application, or submitted incorrect in-
formation in a permit application or in
any report to the Director, it shall
promptly submit such facts or informa-
tion.
(m) Requirements prior to commencing
injection. Except for all new wells au-
thorized by an area permit under
§144.33(c), a new injection well may not
commence injection until construction
is complete, and
(1) The permittee has submitted no-
tice of completion of construction to
the Director; and
(2)(i) The Director has inspected or
otherwise reviewed the new injection
well and finds it is in compliance with
the conditions of the permit; or
(ii) The permittee has not received
notice form the Director of his or her
intent to inspect or otherwise review
the new injection well within 13 days of
the date of the notice in paragraph
(m)(l) of this section, in which case
prior inspection or review is waived
and the permittee may commence in-
jection. The Director shall include in
his notice a reasonable time period in
which he shall inspect the well.
(n) The permittee shall notify the Di-
rector at such times as the permit re-
quires before conversion or abandon-
ment of the well or in the case of area
permits before closure of the project.
(o) A Class I, II or III permit shall in-
clude and a Class V permit may in-
clude, conditions which meet the appli-
cable requirements of §146.10 of this
chapter to insure that plugging and
abandonment of the well will not allow
the movement of fluids into or between
USDWs. Where the plan meets the re-
quirements of §146.10 of this chapter,
650
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Environmental Protection Agency
§144.52
the Director shall incorporate it into
the permit as a permit condition.
Where the Director's review of an ap-
plication indicates that the permittee's
plan is inadequate, the Director may
require the applicant to revise the
plan, prescribe conditions meeting the
requirements of this paragraph, or
deny the permit. For purposes of this
paragraph, temporary or intermittent
cessation of injection operations is not
abandonment.
(p) Plugging and abandonment report.
For EPA-administered programs, with-
in 60 days after plugging a well or at
the time of the next quarterly report
(whichever is less) the owner or oper-
ator shall submit a report to the Re-
gional Administrator. If the quarterly
report Is due less than 15 days before
completion of plugging, then the report
shall be submitted within 60 days. The
report shall be certified as accurate by
the person who performed the plugging
operation. Such report shall consist of
either:
(1) A statement that the well was
plugged in accordance with the plan
previously submitted to the Regional
Administrator; or
(2) Where actual plugging differed
from the plan previously submitted,
and updated version of the plan on the
form supplied by the regional adminis-
trator, specifying the differences.
(q) Duty to establish and maintain me-
chanical integrity, (1) The owner or op-
erator of a Class I, II or III well per-
mitted under this part shall establish
prior to commencing injection or on a
schedule determined by the Director,
and thereafter maintain mechanical in-
tegrity as defined in § 146.8 of this chap-
ter. For EPA-administered programs,
the Regional Administrator may re-
quire by written notice that the owner
or operator comply with a schedule de-
scribing when mechanical integrity
demonstrations shall be made.
(2) When the Director determines
that a Class I, II, or ni well lacks me-
chanical integrity pursuant to §146.8 of
this chapter, he shall give written no-
tice of his determination to the owner
or operator. Unless the Director re-
quires immediate cessation, the owner
or operator shall cease injection Into
the well within 48 hours of receipt of
the Director's determination. The Di-
rector may allow plugging of the well
pursuant to the requirements of § 146.10
of this chapter or require the permittee
to perform such additional construc-
tion, operation, monitoring, reporting
and corrective action as is necessary to
prevent the movement of fluid into or
between USDWs caused by the lack of
mechanical integrity. The owner or op-
erator may resume injection upon writ-
ten notification from the Director that
the owner or operator has dem-
onstrated mechanical integrity pursu-
ant to 1146.8 of this chapter.
(3) The Director may allow the owner
or operator of a well which lacks me-
chanical integrity pursuant to
§146.8(a)(l) of this chapter to continue
or resume injection, if the owner or op-
erator has made a satisfactory dem-
onstration that there is no movement
of fluid into or between USDWs.
[48 FB 14189, Apr. 1, 1983, as amended at. 49
FB 20185, May 11, 1984; 53 PR 28147, July 26,
1988; 58 FE 63898, Dec. 3, 1993]
I 144.52 Establishing permit condi-
tions.
(a) In addition to conditions required
in §144.51, the Director shall establish
conditions, as required on a case-by-
case basis under §144.36 (duration of
permits), §144.53(a) (schedules of com-
pliance), §144.54 (monitoring), and for
EPA permits only §144.53(b) (alternate
schedules of compliance), and §144.4
(considerations under Federal law).
Permits for owners or operators of haz-
ardous waste injection wells shall in-
clude conditions meeting the require-
ments of §144.14 (requirements for wells
injecting hazardous waste), §144.52
(a)(7) and (a)(9), and subpart G of part
146. Permits for other wells shall con-
tain the following requirements, when
applicable.
(1) Construction requirements as set
forth in part 146. Existing wells shall
achieve compliance with such require-
ments according to a compliance
schedule established as a permit condi-
tion. The owner or operator of a pro-
posed new injection well shall submit
plans for testing, drilling, and con-
struction as part of the permit applica-
tion. Except as authorized by an area
permit, no constuction may commence
until a permit has been issued con-
taining construction requirements (see
651
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§144.52
40 CFR Ch. i (7-1-04 Edition)
§144.11). New wells shall be in compli-
ance with, these requirements prior to
commencing injection operations.
Changes in construction plans during
construction may be approved by the
Administrator as minor modifications
(§144.41). No such changes may be phys-
ically incorporated into construction
of the well prior to approval of the
modification by the Director.
(2) Corrective action as set forth in
§§144.55 and 146.7
(3) Operation requirements as set forth
in 40 CPR part 146; the permit shall es-
tablish any maximum injection vol-
umes and/or pressures necessary to as-
sure that fractures are not initiated in
the confining zone, that injected fluids
do not migrate into any underground
source of drinking water, that forma-
tion fluids are not displaced into any
underground source of drinking water,
and to assure compliance with the part
146 operating requirements.
(4) Requirements for wells managing
hazardous waste, as set forth in §144.14.
(5) Monitoring and reporting require-
ments as set forth in 40 CFR part 146.
The permittee shall be required to
identify types of tests and methods
used to generate the monitoring data.
For EPA administered programs, moni-
toring of the nature of injected fluids
shall comply with applicable analytical
methods cited and described in table I
of 40 CFR 136.3 or in appendix III of 40
CFR part 261 or in certain cir-
cumstances by other methods that
have been approved by the Regional
Administrator.
(6) After a cessation of operations of
two years the owner or operator shall
plug and abandon the well in accord-
ance with the plan unless he:
(i) Provides notice to the Regional
Administrator;
(ii) Describes actions or procedures,
satisfactory to the Regional Adminis-
trator, that the owner or operator will
take to ensure that the well will not
endanger USDWs during the period of
temporary abandonment. These actions
and procedures shall include compli-
ance with the technical requirements
applicable to active injection wells un-
less waived by the Regional Adminis-
trator.
(7) Financial responsibility, (i) The per-
mittee, including the transferor of a
permit, is required to demonstrate and
maintain financial responsibility and
resources to close, plug, and abandon
the underground injection operation in
a manner prescribed by the Director
until:
(A) The well has been plugged and
abandoned in accordance with an ap-
proved plugging and abandonment plan
pursuant to §§144.51(o) and 146.10 of this
chapter, and submitted a plugging and
abandonment report pursuant to
§144.51(p); or
(B) The well has been converted in
compliance with the requirements of
§144.51(n); or
(C) The transferor of a permit has re-
ceived notice from the Director that
the owner or operator receiving trans-
fer of the permit, the new permittee,
has demonstrated financial responsi-
bility for the well.
(ii) The permittee shall show evi-
dence of such financial responsibility
to the Director by the submission of a
surety bond, or other adequate assur-
ance, such as a financial statement or
other materials acceptable to the Di-
rector. For EPA administered pro-
grams, the Regional Administrator
may on a periodic basis require the
holder of a lifetime permit to submit
an estimate of the resources needed to
plug and abandon the well revised to
reflect inflation of such costs, and a re-
vised demonstration of financial re-
sponsibility, if necessary. The owner or
operator of a well injecting hazardous
waste must comply with the financial
responsibility requirements of subpart
F of this part.
(8) Mechanical integrity. A permit for
any Class I, II or III well or injection
project which lacks mechanical integ-
rity shall include, and for any Class V
well may include, a condition prohib-
iting injection operations until the per-
mittee shows to the satisfaction of the
Director under §146.08 that the well haa
mechanical integrity.
(9) Additional conditions. The Director
shall impose on a case-by-case basis
such additional conditions as are nec-
essary to prevent the migration of
fluids into underground sources of
drinking water.
(b)(l) In addition to conditions re-
quired in all permits the Director shall
652
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Environmental Protection Agency
§144.53
establish conditions in permits as re-
quired on a case-by-case basis, to pro-
vide for and assure compliance with all
applicable requirements of the SDWA
and parts 144, 145, 146 and 124.
(2) For a State issued permit, an ap-
plicable requirement is a State statu-
tory or regulatory requirement which
takes effect prior to final administra-
tive disposition of the permit. For a
permit issued by EPA, an applicable re-
quirement is a statutory or regulatory
requirement (including any interim
final regulation) which takes effect
prior to the issuance of the permit.
Section 124.14 (reopening of comment
period) provides a means for reopening
EPA permit proceedings at the discre-
tion of the Director where new require-
ments become effective during the per-
mitting process and are of sufficient
magnitude to make additional pro-
ceedings desirable. For State and EPA
administered programs, an applicable
requirement is also any requirement
which takes effect prior to the modi-
fication or revocation and reissuance of
a permit, to the extent allowed in
§144.39.
(3) New or reissued permits, and to
the extent allowed under §144.39 modi-
fied or revoked and reissued permits,
shall incorporate each of the applicable
requirements referenced in § 144.52.
(c) Incorporation. All permit condi-
tions shall be incorporated either ex-
pressly or by reference. If incorporated
by reference, a specific citation to the
applicable regulations or requirements
must be given in the permit.
[48 FB 14189, Apr. 1, 1983, as amended at 49
FR 20185, May 11, 1984; 53 FR 28147, July 26,
1988; 58 FR 63898; Dec. 3, 1993; 65 FR 30913,
May 15, 2000]
§ 144.53 Schedule of compliance.
(a) General. The permit may, when
appropriate, specify a schedule of com-
pliance leading to compliance with the
SDWA and parts 144, 145,146, and 124.
(1) Time for compliance. Any schedules
of compliance shall require compliance
as soon as possible, and in no case later
than 3 years after the effective date of
the permit.
(2) Interim dates. Except as provided
in paragraph (b)(l)(ii) of this section, if
a permit establishes a schedule of com-
pliance which exceeds 1 year from the
date of permit issuance, the schedule
shall set forth interim requirements
and the dates for their achievement.
(i) The time between interim dates
shall not exceed 1 year.
(ii) If the time necessary for comple-
tion of any interim requirement is
more than 1 year and is not readily di-
visible into stages for completion, the
permit shall specify interim dates for
the submission of reports of progress
toward completion of the interim re-
quirements and indicate a projected
completion date.
(3) Reporting. The permit shall be
written to require that if paragraph
(a)(l) of this section is applicable,
progress reports be submitted no later
than 30 days following each interim
date and the final date of compliance.
(b) Alternative schedules of compliance.
A permit applicant or permittee may
cease conducting regulated activities
(by plugging and abandonment) rather
than continue to operate and meet per-
mit requirements as follows:
(1) If the permittee decides to cease
conducting' regulated activities at a
given time within the term of a permit
which has already been issued:
(i) The permit may be modified to
contain a new or additional schedule
leading to timely cessation of activi-
ties; or
(ii) The permittee shall cease con-
ducting permitted activities before
noncompliance with any interim or
final compliance schedule requirement
already specified in the permit.
(2) If the decision to cease conducting
regulated activities is made before
issuance of a permit whose term will
include the termination date, the per-
mit shall contain a schedule leading to
termination which will ensure timely
compliance with applicable require-
ments.
(3) If the permittee is undecided
whether to cease conducting regulated
activities, the Director may issue or
modify a permit to contain two sched-
ules as follows:
(i) Both schedules shall contain an
identical interim deadline requiring a
final decision on whether to cease con-
ducting regulated activities no later
than a date which ensures sufficient
time to comply with applicable re-
quirements in a timely manner if the
653
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§144.54
40 CFR Ch. i (7-1-04 Edition)
decision is to continue conducting reg-
ulated activities;
(ii) One schedule shall lead to timely
compliance with applicable require-
ments;
(Hi) The second schedule shall lead to
cessation of regulated activities by a
date which will ensure timely compli-
ance with applicable requirements;
(iv) Bach permit containing two
schedules shall include a requirement
that after the permittee has made a
final decision under paragraph (b)(3)(i)
of this section it shall follow the sched-
ule leading to compliance if the deci-
sion is to continue conducting regu-
lated activities, and follow the sched-
ule leading to termination if the deci-
sion is to cease conducting- regulated
activities.
(4) The applicant's or permittee's de-
cision to cease conducting regulated
activities shall be evidenced by a firm
public commitment satisfactory to the
Director, such as a resolution of the
board of directors of a corporation,
§ 144.54 Requirements for recording
and reporting of monitoring results.
All permits shall specify:
(a) Requirements concerning the
proper use, maintenance, and installa-
tion, when appropriate, of monitoring
equipment or methods (including bio-
logical monitoring methods when ap-
propriate);
(b) Kequired monitoring including
type, intervals, and frequency suffi-
cient to yield data which are represent-
ative of the monitored activity includ-
ing when appropriate, continuous mon-
itoring;
(c) Applicable reporting requirements
based upon the impact of the regulated
activity and as specified in part 146.
Reporting shall be no less frequent
than specified in the above regulations.
§ 144.55 Corrective action.
(a) Coverage. Applicants for Class I,
II, (other than existing), or III injec-
tion well permits shall identify the lo-
cation of all known wells within the in-
jection well's area of review which pen-
etrate the injection zone, or in the case
of Class II wells operating over the
fracture pressure of the injection for-
mation, all known wells within the
area of review penetrating formations
affected by the increase in pressure.
For such wells which are improperly
sealed, completed, or abandoned, the
applicant shall also submit a plan con-
sisting of such steps or modifications
as are necessary to prevent movement
of fluid into underground sources of
drinking water ("corrective action").
Where the plan is adequate, the Direc-
tor shall incorporate it into the permit
as a condition. Where the Director's re-
view of an application indicates that
the permittee's plan is inadequate
(based on the factors in § 146.07), the Di-
rector shall require the applicant to re-
vise the plan, prescribe a plan for cor-
rective action as a condition of the per-
mit under paragraph (b) of this section,
or deny the application. The Director
may disregard the provisions of § 146.06
(Area of Review) and §146.07 (Correc-
tive Action) when reviewing an
application to permit an existing Class
II well.
(b) Requirements—(1) Existing injection
wells. Any permit issued for an existing
injection well (other than Class II) re-
quiring corrective action shall include
a compliance schedule requiring any
corrective action accepted or pre-
scribed under paragraph (a) of this sec-
tion to be completed as soon as
possible.
(2) New injection wells. No owner or
operator of a new injection well may
begin injection until all required cor-
rective action has been taken.
(3) Injection pressure limitation. The
Director may require as a permit con-
dition that injection pressure be so
limited that pressure in the injection
zone does not exceed hydrostatic pres-
sure at the site of any improperly com-
pleted or abandoned well within the
area of review. This pressure limitation
shall satisfy the corrective action re-
quirement. Alternatively, such injec-
tion pressure limitation can be part of
a compliance, schedule and last until
all other required corrective action has
been taken.
(4) Class III wells only. When setting
corrective action requirements the Di-
rector shall consider the overall effect
of the project on the hydraulic gra-
dient in potentially affected USDWs,
and the corresponding changes in
654
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Environmental Protection Agency
§144.62
potentiometric surface(s) and flow di-
rection(s) rather than, the discrete ef-
fect of each well. If a decision is made
that corrective action is not necessary
based on the determinations above, the
monitoring program required in
§146.33(b) shall be designed to verify
the validity of such determinations.
Subpart F—Financial Responsi-
bility: Class I Hazardous Waste
Injection Wells
SOURCE: 49 FR 20186, May 11, 1984, unless
otherwise noted.
§ 144.60 Applicability.
(a) The requirements of §§144.62,
144.63, and 144.70 apply to owners and
operators of all existing and new Class
I Hazardous waste injection wells, ex-
cept as provided otherwise in this sec-
tion.
9144.61 Definitions of terms as used in
this subpart,
(a) Plugging and abandonment plan
means the plan for plugging and aban-
donment prepared in accordance with
the requirements of §§144.28 and 144.51.
(b) Current plugging cost estimate
means the most recent of the estimates
prepared in accordance with §144.62 (a),
(b) and (c).
(c) Parent corporation means a cor-
poration which directly owns at least
50 percent of the voting stock of the
corporation which is the injection well
owner or operator; the latter corpora-
tion is deemed a subsidiary of the par-
ent corporation.
(d) The following terms are used in
the specifications for the financial test
for plugging and abandonment. The
definitions are intended to represent
the common meanings of the terms as
they are generally used by the business
community.
Assets means all existing and all
probable future economic benefits ob-
tained or controlled by a particular en-
tity.
Current assets means cash or other as-
sets or resources commonly identified
as those which are reasonably expected
to be realized in cash or sold or con-
sumed during the normal operating
cycle of the business.
Current liabilities means obligations
whose liquidation is reasonably ex-
pected to require the use of existing re-
sources properly classifiable as current
assets or the creation of other current
liabilities,
Independently audited refers to an
audit performed by an independent cer-
tified public accountant in accordance
with generally accepted auditing
standards.
Liabilities means probable future sac-
rifices of economic benefits arising
from present obligations to transfer as-
sets or provide services to other enti-
ties in the future as a result of past
transactions or events.
Net working capital means current as-
sets minus current liabilities.
Net worth means total assets minus
total liabilities and is equivalent to
owner's equity.
Tangible net worth means the tangible
assets that remain after deducting li-
abilities; such assets would not include
intangibles such as goodwill and rights
to patents or royalties.
§ 144.62 Coat estimate for plugging and
abandonment.
(a) The owner or operator must pre-
pare a written estimate, in current dol-
lars, of the cost of plugging the injec-
tion well in accordance with the plug-
ging and abandonment plan as specified
in §§144.28 and 144.51. The plugging and
abandonment cost estimate must equal
the cost of plugging and abandonment
at the point in the facility's operating
life when the extent and manner of its
operation would making plugging and
abandonment the most expensive, as
indicated by its plugging and abandon-
ment plan.
(b) The owner or operator must ad-
just the plugging and abandonment
cost estimate for inflation within 30
days after each anniversary of the date
on which the first plugging and aban-
donment cost estimate was prepared.
The adjustment must be made as speci-
fied in paragraphs (b) (1) and (2) of this
section, using an inflation factor de-
rived from the annual Oil and Gas
Field Equipment Cost Index. The infla-
tion factor is the result of dividing the
latest published annual Index by the
Index for the previous year.
655
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§144.63
40 CFR Ch. I (7-1-04 Edition)
(1) The first adjustment Is made by
multiplying the plugging and abandon-
ment cost estimate by the inflation
factor. The result is the adjusted plug-
ging and abandonment cost estimate,
(2) Subsequent adjustments are made
by multiplying the latest adjusted
plugging and abandonment cost esti-
mate by the latest inflation factor,
(c) The owner or operator must revise
the plugging and abandonment cost es-
timate whenever a change in the plug-
ging and abandonment plan increases
the cost of plugging and abandonment.
The revised plugging and abandonment
cost estimate must be adjusted for in-
flation as specified in §144.62{b).
(d) The owner or operator must keep
the following at the facility during the
operating life of the facility: the latest
plugging and abandonment cost esti-
mate prepared in accordance with
§144.62 (a) and (c) and, when this
estimate has been adjusted in accord-
ance with § 144.62(b), the latest adjusted
plugging and abandonment cost esti-
mate.
1144.63 Financial assurance for plug-
ging and abandonment.
An owner or operator of each facility
must establish financial assurance for
the plugging and abandonment of each
existing and new Class I hazardous
waste injection well. He must choose
from the options as specified in para-
graphs (a) through (f) of this section.
(a) Plugging and abandonment trust
fund. (1) An owner or operator may sat-
isfy the requirements of this section by
establishing a plugging and abandon-
ment trust fund which conforms to the
requirements of this paragraph and
submitting an originally signed dupli-
cate of the trust agreement to the Re-
gional Administrator. An owner or op-
erator of a Class I well injecting haz-
ardous waste must submit the origi-
nally signed duplicate of the trust
agreement to the Regional Adminis-
trator with the permit application or
for approval to operate under rule. The
trustee must be an entity which has
the authority to act as a trustee and
whose trust operations are regulated
and examined by a Federal or State
agency,
(2) The wording of the trust agree-
ment must be identical to the wording
specified in §144.70(a)(l), and the trust
agreement must be accompanied by a
formal certification of acknowledg-
ment (for example, see § 144.70(a)(2)).
Schedule A of the trust agreement
must be updated within 60 days after a
change in the amount of the current
plugging and abandonment cost esti-
mate covered by the agreement.
(3) Payments into the trust fund
must be made annually by the owner or
operator over the term of the initial
permit or over the remaining operating
life of the injection well as estimated
in the plugging and abandonment plan,
whichever period is shorter; this period
is hereafter referred to as the "pay-in
period." The payments into the plug-
ging and abandonment trust fund must
be made as follows:
(i) For a new well, the first payment
must be made before the initial injec-
tion of hazardous waste. A receipt from
the trustee for this payment must be
submitted by the owner or operator to
the Regional Administrator before this
initial injection of hazardous waste.
The first payment must be at least
equal to the current plugging and
abandonment cost estimate, except as
provided in §144.70(g), divided by the
number of years in the pay-in period.
Subsequent payments must be made no
later than 30 days after each anniver-
sary date of the first payment. The
amount of each subsequent payment
must be determined by this formula:
Next payment =
PE-CV
where PE IB the current plugging and aban-
donment cost estimate, CV is the current
value of the trust fund, and Y is the number
of years remaining in the pay-in period.
(ii) If an owner or operator estab-
lishes a trust fund as specified in
§ 144.63(a) of this chapter, and the value
of that trust fund is less than the cur-
rent plugging and abandonment cost
estimate when a permit is awarded for
the injection well, the amount of the
current plugging and abandonment
cost estimate still to be paid into the
trust fund must be paid in over the
pay-in period as defined in paragraph
(a)(3) of this section. Payments must
continue to be made no later than 30
days after each anniversary date of the
656
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Environmental Protection Agency
§ 144,63
first payment made pursuant to part
144 of this chapter. The amount of each
payment must be determined by this
formula:
Next payment =
PE-CV
where PE is the current plugging and aban-
donment cost estimate, CV is the current
value of the trust fund, and Y is the number
of years remaining in the pay-in period.
(4) The owner or operator may accel-
erate payments into the trust fund or
he may deposit the full amount of the
current plugging and abandonment
cost estimate at the time the fund is
established. However, he must main-
tain the value of the fund at no less
than the value that the fund would
have if annual payments were made as
specified in paragraph (a)(3) of this sec-
tion.
(5) If the owner or operator estab-
lishes a plugging and abandonment
trust fund after having used one or
more alternate mechanisms specified
in this section or in §144.63 of this
chapter, his first payment must be in
at least the amount that the fund
would contain if the trust fund were es-
tablished initially and annual pay-
ments made according to specifications
of this paragraph.
(6) After the pay-in period is com-
pleted, whenever the current plugging
and abandonment cost estimate
changes, the owner or operator must
compare the new estimate with the
trustee's most recent annual valuation
of the trust fund. If the value of the
fund is less than the amount of the new
estimate, the owner or operator, within
80 days after the change in the cost es-
timate, must either deposit an amount
into the fund so that its value after
this deposit at least equals the amount
of the current plugging and abandon-
ment cost estimate, or obtain other fi-
nancial assurance as specified in this
section to cover the difference.
(7) If the value of the trust fund is
greater than the total amount of the
current plugging and abandonment
cost estimate, the owner or operator
may submit a written request to the
Regional Administrator for release of
the amount in excess of the current
plugging and abandonment cost esti-
mate.
(8) If an owner or operator sub-
stitutes other financial assurance as
specified in this section for all or part
of the trust fund, he may submit a
written request to the Regional Admin-
istrator for release of the amount in
excess of the current plugging and
abandonment cost estimate covered by
the trust fund.
(9) Within 60 days after receiving- a
request from the owner or operator for
release of funds as specified in para-
graph (a) (7) or (8) of this section, the
Regional Administrator will instruct
the trustee to release to the owner or
operator such funds as the Regional
Administrator specifies in writing.
(10) After beginning final plugging
and abandonment, an owner or oper-
ator or any other person authorized to
perform plugging and abandonment
may request reimbursement for plug-
ging and abandonment expenditures by
submitting itemized bills to the Re-
gional Administrator. Within 60 days
after receiving bills for plugging and
abandonment activities, the Regional
Administrator will determine whether
the plugging and abandonment expend-
itures are in accordance with the plug-
ging and abandonment plan or other-
wise justified, and if so, he will in-
struct the trustee to make reimburse-
ment in such amounts as the Regional
Administrator specifies in writing. If
the Regional Administrator has reason
to believe that the cost of plugging and
abandonment will be significantly
greater than the value of the trust
fund, he may withhold reimbursement
of such amounts as he deems prudent
until he determines, in accordance
with §144.63(1), that the owner or oper-
ator is no longer required to maintain
financial assurance for plugging and
abandonment.
(11) The Regional Administrator will
agree to termination of the trust when:
(i) An owner or operator substitutes
alternate financial assurance as speci-
fied in this section; or
(ii) The Regional Administrator re-
leases the owner or operator from the
requirements of this section in accord-
ance with §144.63(1).
(b) Surety bond guaranteeing payment
into a plugging and abandonment trust
fund. (1) An owner or operator must
satisfy the requirements of this section
657
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§144.63
40 CFR Ch. I (7-1-04 Edition)
by obtaining a surety bond which con-
forms to the requirements of this para-
graph and submitting the bond to the
Regional Administrator with the appli-
cation for a permit or for approval to
operate under rule. The bond must be
effective before the initial injection of
hazardous waste. The surety company
issuing the trust must, at a minimum,
be among those listed as acceptable
sureties on Federal bonds in Circular
570 of the U.S. Department of the
Treasury.
(2) The wording of the surety bond
must be identical to the wording in
§144.70(b).
(3) The owner or operator who uses a
surety bond to satisfy the require-
ments of this section must also estab-
lish a standby trust fund. Under the
terms of the bond, all payments made
thereunder will be deposited by the
surety directly into the standby trust
fund in accordance with instructions
from the Regional Administrator. This
standby trust fund must meet the re-
quirements specified in §144.63(a), ex-
cept that:
(i) An originally signed duplicate of
the trust agreement must be submitted
to the Regional Administrator with the
surety bond; and
(ii) Until the standby trust fund is
funded pursuant to the requirements of
this section, the following are not re-
quired by these requirements;
(A) Payments into the trust fund as
specified in §144.63(a);
(B) Updating of Schedule A of the
trust agreement [see § 144.70(a)] to show
current plugging and abandonment
cost estimates;
(C) Annual valuations as required by
the trust agreement; and
(D) Notices of nonpayment as re-
quired by the trust agreement.
(4) The bond must guarantee that the
owner or operator will:
(i) Fund the standby trust fund in an
amount equal to the penal sum of the
bond before beginning of plugging and
abandonment of the injection well; or
(ii) Fund the standby trust fund in an
amount equal to the penal sum within
15 days after an order to begin plugging
and abandonment is issued by the Re-
gional Administrator or a U.S. district
court or other court of competent ju-
risdiction; or
(iii) Provide alternate financial as-
surance as specified in this section, and
obtain the Regional Administrator's
written approval of the assurance pro-
vided, within 90 days after receipt by
both the owner or operator and the Re-
gional Administrator of a notice of
cancellation of the bond from the sur-
ety.
(5) Under the terms of the bond, the
surety will become liable on the bond
obligation when the owner or operator
fails to perform as guaranteed by the
bond.
(6) The penal sum of the bond must
be in amount at least equal to the cur-
rent plugging and abandonment cost
estimate, except as provided in
§144.63(g).
(7) Whenever the current plugging
and abandonment cost estimate in-
creases to an amount greater than the
penal sum, the owner or operator,
within 60 days after the increase, must
either cause the penal sum to be in-
creased to an amount at least equal to
the current plugging and abandonment
cost estimate and submit evidence of
such increase to the Regional Adminis-
trator, or obtain other financial assur-
ance as specified in this section to
cover the increase. Whenever the cur-
rent plugging and abandonment cost
estimate decreases, the penal sum may
be reduced to the amount of the cur-
rent plugging and abandonment cost
estimate following written approval by
the Regional Administrator.
(8) Under the terms of the bond, the
surety may cancel the bond by sending
notice of cancellation by certified mail
to the owner or operator and to the Re-
gional Administrator. Cancellation
may not occur, however, during 120
days beginning on the date of the re-
ceipt of the notice of cancellation by
both owner or operator and the Re-
gional Administrator as evidenced by
the returned receipts.
(9) The owner or operator may cancel
the bond if the Regional Administrator
has given prior written consent based
on his receipt of evidence of alternate
financial assurance as specified in this
section.
(c) Surety bond guaranteeing perform-
ance of plugging and abandonment. (1)
An owner or operator may satisfy the
658
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Environmental Protection Agency
§144.63
requirements of this section by obtain-
ing a surety bond which conforms to
the requirements of this paragraph and
submitting the bond to the Regional
Administrator, An owner or operator of
a new facility must submit the bond to
the Regional Administrator with the
permit application or for approval to
operate under rule. The bond must be
effective before injection of hazardous
waste is started. The surety company
issuing the bond must, at a minimum,
be among those listed as acceptable
sureties on Federal bonds in Circular
570 of the U.S. Department of the
Treasury.
(2) The wording of the surety bond
must be identical to the wording speci-
fied in §144.70(c).
(3) The owner or operator who uses a
surety bond to satisfy the require-
ments of this section must also estab-
lish a standby trust fund. Under the
terms of the bond, all payments made
thereunder will be deposited by the
surety directly into the standby trust
fund in accordance with instructions
from the Regional Administrator. The
standby trust must meet the require-
ments specified in §144.63(a), except
that:
(i) An original signed duplicate of the
trust agreement must be submitted to
the Regional Administrator with the
surety bond; and
(ii) Unless the standby trust fund is
funded pursuant to the requirements of
this section, the following are not re-
quired by these regulations:
(A) Payments into the trust fund as
specified in §144.63(a);
(B) Updating of Schedule A of the
trust agreement [see § 144.70(a)] to show
current plugging" and abandonment
cost estimates;
(C) Annual valuations as required by
the trust agreement; and
(D) Notices of nonpayment as re-
quired by the trust agreement.
(4) The bond must guarantee that the
owner or operator will:
(i) Perform plugging and abandon-
ment in accordance with the plugging
and abandonment plan and other re-
quirements of the permit for the injec-
tion well whenever required to do so; or
(ii) Provide alternate financial assur-
ance as specified in this section, and
obtain the Regional Administrator's
written approval of the assurance pro-
vided, within 90 days after receipt by
both the owner or operator and the Re-
gional Administrator of a notice of
cancellation of the bond from the sur-
ety.
(5) Under the terms of the bond, the
surety will become liable on the bond
obligation when the owner or operator
fails to perform as guaranteed by the
bond. Following a determination that
the owner or operator has failed to per-
form plugging and abandonment in ac-
cordance with the plugging and aban-
donment plan and other permit re-
quirements when required to do so,
under terms of the bond the surety will
perform plugging and abandonment as
guaranteed by the bond or will deposit
the amount of the penal sum into the
standby trust fund.
(6) The penal sum of the bond must
be in an amount at least equal to the
current plugging and abandonment
cost estimate.
(7) Whenever the current plugging
and abandonment cost estimate in-
creases to an amount greater than the
penal sum, the owner or operator,
within 60 days after the increase, must
either cause the penal sum to be in-
creased to an amount at least equal to
the current plugging and abandonment
cost estimate and submit evidence of
such increase to the Regional Adminis-
trator, or obtain other financial assur-
ance as specified in this section. When-
ever the plugging and abandonment
cost estimate decreases, the penal sum
may be reduced to the amount of the
current plugging and abandonment
cost estimate following written ap-
proval by the Regional Administrator.
(8) Under the terms of the bond, the
surety may cancel the bond by sending
notice of cancellation by certified mail
to the owner or operator and to the Re-
gional Administrator. Cancellation
may not occur, however, during the 120
days beginning on the date of receipt of
the notice of cancellation by both the
owner or operator and the Regional Ad-
ministrator, as evidenced by the return
receipts.
(9) The owner or operator may cancel
the bond if the Regional Administrator
has given prior written consent. The
Regional Administrator will provide
such written consent when:
659
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§144.63
40 CFR Ch. I (7-1-04 Edition)
(i) An owner or operator substitute
alternate financial assurance as speci-
fied in this section; or
(ii) The Regional Administrator re-
leases the owner or operator from the
requirements of this section in accord-
ance with § 144.63(1),
(10) The surety will not be liable for
deficiencies in the performance of plug-
ging and abandonment by the owner or
operator after the Regional Adminis-
trator releases the owner or operator
from the requirements of this section
in accordance with §144.63(1).
(d) Plugging and abandonment letter of
credit. (1) An owner or operator may
satisfy the requirements of this section
by obtaining an irrevocable standby
letter of credit which conforms to the
requirements of this paragraph and
submitting the letter to the Regional
Administrator. An owner or operator of
an injection well must submit the
letter of credit to the Regional Admin-
istrator during submission of the per-
mit application or for approval to oper-
ate under rule. The letter of credit
must be effective before initial injec-
tion of hazardous waste. The issuing
institution must be an entity which
has the authority to issue letters of
credit and whose letter-of-credit oper-
ations are regulated and examined by a
Federal or State agency.
(2) The wording of the letter of credit
must be identical to the wording speci-
fied in §144.70(d).
(3) An owner or operator who uses a
letter of credit to satisfy the require-
ments of this section must also estab-
lish a standby trust fund. Under the
terms of the letter of credit, all
amounts paid pursuant to a draft by
the Regional Administrator will be de-
posited by the issuing institution di-
rectly into the standby trust fund in
accordance with instructions from the
Regional Administrator. This standby
trust fund must meet the requirements
of the trust fund specified in §144.63(a),
except that:
(i) An originally signed duplicate of
the trust agreement must be submitted
to the Regional Administrator with the
letter of credit; and
(ii) Unless the standby trust fund is
funded pursuant to the requirements of
this section, the following are not re-
quired by these regulations:
(A) Payments into the trust fund as
specified in § 144.63(a);
(B) Updating of Schedule A of the
trust agreement (see §144.70(a)) to show
current plugging and abandonment
cost estimates;
(C) Annual valuations as required by
the trust agreement; and
(D) Notices of nonpayment as re-
quired by the trust agreement.
(4) The letter of credit must be ac-
companied by a letter from the owner
or operator referring to the letter of
credit by number, issuing institution,
and date, and providing the following
information: the EPA Identification
Number, name, and address of the facil-
ity, and the amount of funds assured
for plugging and abandonment of the
well by the letter of credit.
(5) The letter of credit must be irrev-
ocable and issued for a period of at
least 1 year. The letter of credit must
provide that the expiration date will be
automatically extended for a period of
at least 1 year unless, at least 120 days
before the current expiration date, the
issuing institution notifies both the
owner or operator and the Regional Ad-
ministrator by certified mail of a deci-
sion not to extend the expiration date.
Under the terms of the letter of credit,
the 120 days will begin on the date
when both the owner or operator and
the Regional Administrator have re-
ceived the notice, as evidenced by the
return receipts.
(6) The letter of credit must be issued
in an amount at least equal to the cur-
rent plugging and abandonment cost
estimate, except as provided in
§144.63(g).
(7) Whenever the current plugging
and abandonment cost estimate in-
creases to an amount greater than the
amount of the credit, the owner or op-
erator, within 60 days after the in-
crease, must either cause the amount
of the credit to be increased so that it
at least equals the current plugging
and abandonment cost estimate and
submit evidence of such increase to the
Regional Administrator, or obtain
other financial assurance as specified
in this section to cover the increase.
Whenever the current plugging and
abandonment cost estimate decreases,
the amount of the credit may be re-
duced to the amount of the current
660
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Environmental Protection Agency
§144.63
plugging and abandonment cost esti-
mate following written approval by the
Regional Administrator.
(8) Following a determination that
the owner or operator has failed to per-
form final plugging and abandonment
in accordance with the plugging and
abandonment plan and other permit re-
quirements when required to do so, the
Regional Administrator may draw on
the letter of credit.
(9) If the owner or operator does not
establish alternate financial assurance
as specified in this section and obtain
written approval of such alternate as-
surance from the Regional Adminis-
trator within 90 days after receipt by
both the owner or operator and the Re-
gional Administrator of a notice from
the issuing institution that it has de-
cided not to extend the letter of credit
beyond the current expiration date, the
Regional Administrator will draw on
the letter of credit. The Regional Ad-
ministrator may delay the drawing if
the issuing institution grants an exten-
sion of the term of the credit. During
the last 30 days of any such extension
the Regional Administrator will draw
on the letter of credit if the owner or
operator has failed to provide alternate
financial assurance as specified in this
section and obtain written approval of
such assurance from the Regional Ad-
ministrator.
(10) The Regional Administrator will
return the letter of credit to the
issuing institution for termination
when:
(i) An owner or operator substitutes
alternate financial assurance as speci-
fied in this section; or
(ii) The Regional Administrator re-
leases the owner or operator from the
requirements of this section in accord-
ance with §144.63(1).
(e) Plugging and abandonment insur-
ance. (1) An owner or operator may sat-
isfy the requirements of this section by
obtaining plugging and abandonment
insurance which conforms to the re-
quirements of this paragraph and sub-
mitting a certificate of such insurance
to the Regional Administrator. An
owner or operator of a new injection
well must submit the certificate of in-
surance to the Regional Administrator
with the permit application or for ap-
proval operate under rule. The insur-
ance must be effective before injection
starts. At a minimum, the insurer
must be licensed to transact the busi-
ness of insurance, or eligible to provide
insurance as an excess or surplus lines
insurer, in one or more States,
(2) The wording of the certificate of
insurance must be identical to the
wording specified in §144.70(e).
(3) The plugging and abandonment
insurance policy must be issued for a
face amount at least equal to the cur-
rent plugging and abandonment esti-
mate, except as provided in §144.63(g).
The term "face amount" means the
total amount the insurer is obligated
to pay under the policy. Actual pay-
ments by the insurer will not change
the face amount, although the insurers
future liability will be lowered by the
amount of the payments.
(4) The plugging and abandonment
insurance policy must guarantee that
funds will be available whenever final
plugging and abandonment occurs. The
policy must also guarantee that once
plugging and abandonment begins, the
issurer will be responsible for paying
out funds, up to an amount equal to
the face amount of the policy, upon the
direction of the Regional Adminis-
trator, to such party or parties as the
Regional Administrator specifies.
(5) After beginning plugging and
abandonment, an owner or operator or
any other person authorized to perform
plugging and abandonment may re-
quest reimbursement for plugging and
abandonment expenditures by submit-
ting itemized bills to the Regional Ad-
ministrator. Within 60 days after re-
ceiving bills for plugging and abandon-
ment activities, the Regional Adminis-
trator will determine whether the plug-
ging and abandonment expenditures
are in accordance with the plugging
and abandonment plan or otherwise
justified, and if so, he will instruct the
insurer to make reimbursement in such
amounts as the Regional Adminis-
trator specifies in writing. If the Re-
gional Administrator has reason to be-
lieve that the cost of plugging and
abandonment will be significantly
greater than the face amount of the
policy, he may withhold reimburse-
ment of such amounts as he deems pru-
dent until he determines, in accordance
661
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§144.63
40 CFR Ch, I {7-1-04 Edition)
with §144.63(1), that the owner or oper-
ator is no longer required to maintain
financial assurance for plugging and
abandonment of the injection well.
(6) The owner or operator must main-
tain the policy in full force and effect
until the Regional Administrator con-
sents to termination of the policy by
the owner or operator as specified in
paragraph (e)(10) of this section. Fail-
ure to pay the premium, without sub-
stitution of alternate financial assur-
ance as specified in this section, will
constitute a significant violation of
these regulations, warranting such
remedy as the Regional Administrator
deems necessary. Such violation will
be deemed to begin upon receipt by the
Regional Administrator of a notice of
future cancellation, termination, or
failure to renew due to nonpayment of
the premium, rather than upon the
date of expiration.
(7) Each policy must contain provi-
sions allowing assignment to a suc-
cessor owner or operator. Such assign-
ment may be conditional upon consent
of the insurer, provided such consent is
not unreasonably refused.
(8) The policy must provide that the
insurer may not cancel, terminate, or
fail to renew the policy except for fail-
ure to pay the premium. The auto-
matic renewal of the policy must, at a
minimum, provide the insured with the
option of renewal at the face amount of
the expiring policy. If there is a failure
to pay the premium, the insurer may
elect to cancel, terminate, or fail to
renew the policy by sending notice by
certified mail to the owner or operator
and the Regional Administrator. Can-
cellation, termination, or failure to
renew may not occur, however, during
120 days beginning with the date of re-
ceipt of the notice by both the Re-
gional Administrator and the owner or
operator, as evidenced by the return of
receipts. Cancellation, termination, or
failure to renew may not occur and the
policy will remain in full force and ef-
fect in the event that on or before the
date of expiration:
(i) The Regional Administrator
deems the injection well abandoned; or
(ii) The permit is terminated or re-
voked or a new permit is denied; or
(iii) Plugging and abandonment is or-
dered by the Regional Administrator or
a U.S. district court or other court of
competent jurisdiction; or
(iv) The owner or operator is named
as debtor in a voluntary or involuntary
proceeding under title 11 (Bankruptcy),
U.S. Code; or
(v) The premium due is paid.
(9) Whenever the current plugging
and abandonment cost estimate in-
creases to an amount greater than the
face amount of the policy, the owner or
operator, within 60 days after the in-
crease, must either cause the face
amount to be increased to an amount
at least equal to the current plugging
and abandonment estimate and submit
evidence of such increase to the Re-
gional Administrator, or obtain other
financial assurance as specified in this
section to cover the increase. Whenever
the current plugging and abandonment
cost estimate decreases, the face
amount may be reduced to the amount
of the current plugging and abandon-
ment cost estimate following written
approval by the Regional Adminis-
trator.
(10) The Regional Administrator will
give written consent to the owner or
operator that he may terminate the in-
surance policy when:
(i) An owner or operator substitutes
alternate financial assurance as speci-
fied in this section; or
(ii) The Regional Administrator re-
leases the owner or operator from the
requirements of this section in accord-
ance with §144.63(i).
(f) Financial test and corporate guar-
antee for plugging and abandonment. (1)
An owner or operator may satisfy the
requirements of this section by dem-
onstrating that he passes a financial
test as specified in this paragraph. To
pass this test the owner or operator
must meet the criteria of either para-
graph (fXIXi) or (f)(l)(ii) of this sec-
tion:
(i) The owner or operator must have:
(A) Two of the following three ratios:
A ratio of total liabilities to net worth
less than 2.0; a ratio of the sum of net
income plus depreciation, depletion,
and amortization to total liabilities
greater than 0.1; and a ratio of current
assets to current liabilities greater
than 1.5; and
(B) Net working capital and tangible
net worth each at least six times the
662
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Environmental Protection Agency
§144.63
sum of the current plugging and aban-
donment cost estimate; and
(C) Tangible net worth of at least $10
million; and
(D) Assets in the United States
amounting to at least 90 percent of his
total assets or at least six times the
sum of the. .current plugging and aban-
donment cost estimate,
(ii) The owner or operator must have:
(A) A current rating for his most re-
cent bond issuance of AAA, AA. A or
BBB as issued by Standard and Poor's
or Aaa, Aa, A, or Baa as issued by
Moody's; and
(B) Tangible net worth at least six
times the sum of the current plugging
and abandonment cost estimate; and
(0) Tangible net worth of at least $10
million; and
(D) Assets located in the United
States amounting to at least 90 percent
of his total assets or at least six times
the sum of the current plugging and
abandonment cost estimates.
(.21 The phrase "current plugging and
abandonment cost estimate" as used in
paragraph (f)(11 of this section refers to
the cost estimate required to be shown
in paragraphs 1 through 4 of the letter
from the owner's or operator's chief fi-
nancial officer §144.70(f).
(3) To demonstrate that he meets
this test, the owner or operator must
submit the following items to the Re-
gional Administrator:
(i) A letter signed by the owner's or
operator's chief financial officer and
worded as specified in §144.70(f): and
(ii) A copy of the independent cer-
tified public accountant's report on ex-
amination of the owner's or operator's
financial statements for the latest
completed fiscal year; and
(ill) A special report from the owner's
or operator's independent certified pub-
lic accountant to the owner or operator
stating that:
(A) He has compared the data which
the letter from the chief financial offi-
cer specifies as having been derived
from the independently audited, year-
end financial statements for the latest
fiscal year with the amounts in such fi-
nancial statements; and
(B) In connection with that proce-
dure, no matters came to his attention
which caused him to believe that the
specified data should be adjusted.
(4) An owner or operator of a new in-
jection well must submit the items
specified in paragraph (f)(3) of this sec-
tion to the Regional Administrator
within 90 days after the close of each
succeeding fiscal year. This informa-
tion must consist of all three items
specified in paragraph (f)(3) of this sec-
tion.
(5) After the initial submission of
items specified in paragraph (f)(3) of
this section, the owner or operator
must send updated information to the
Regional Administrator within 90 days
after the close of each succeeding fiscal
year. This information must consist of
all three items specified in paragraph
(f)(3) of this section.
(6) If the owner or operator no longer
meets the requirements of paragraph
(f)(l) of this section, he must send no-
tice to the Regional Administrator of
intent to establish alternate financial
assurance as specified in this section.
The notice must he sent by certified
mail within 90 days after the end of the
fiscal year for which the year-end fi-
nancial data show that the owner or
operator no longer meets the require-
ments. The owner or operator must
provide the alternate financial assur-
ance within 120 days after the end of
such fiscal year.
(7) The Regional Administrator may.
based on a reasonable belief that the
owner or operator may no longer meet
the requirements of paragraph (f)(l) of
this section, require reports of finan-
cial condition at any time from the
owner or operator in addition to those
specified in paragraph (f)(31 of this sec-
tion. If the Regional Administrator
finds, on the basis of such reports or
other information, that the owner or
operator no longer meets the require-
ments of paragraph (fid) of this sec-
tion, the owner or operator must pro-
vide alternate financial assurance as
specified in this section within 30 days
after notification of such a finding.
(8) The Regional Administrator may
disallow use of this test on the basis of
Qualifications in the opinion expressed
by the independent certified public ac-
countant in his report on examination
of the owner's or operator's financial
statements [see paragraph (fX3)(ii) of
this section]. An adverse opinion or
disclaimer of opinion will be cause for
663
203-160 D-22
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§144,63
40 CFR Ch. I (7-1-04 Edition)
disallowance. The Regional Adminis-
trator will evaluate other qualifica-
tions on an individual basis. The owner
or operator must provide alternate fi-
nancial assurance as specified in this
section within 30 days after notifica-
tion of the disallowance.
(9) The owner or operator is no longer
required to submit the items specified
in paragraph (f)(3) of this section when:
(i) An owner or operator substitutes
alternate financial assurance as speci-
fied in this section; or
(ii) The Regional Administrator re-
leases the owner or operator from the
requirements of this section in accord-
ance with §144.63(1).
(10) An owner or operator may meet
the requirements of this section by ob-
taining a written guarantee, hereafter
referred to as "corporate guarantee."
The guarantee must be the parent cor-
poration of the owner or operator. The
guarantee must meet the requirements
for owners or operators in paragraphs
(f)(l) through (f)(8) of this section and
must comply with the terms of the cor-
porate guarantee. The wording of the
corporate guarantee must be identical
to the wording specified in §144.70(h).
The corporate guarantee must accom-
pany the items sent to the Regional
Administrator as specified In para-
graph (f)(3) of this section. The terms
of the corporate guarantee must pro-
vide that:
(i) If the owner or operator fails to
perform plugging and abandonment of
the injection well covered by the cor-
porate guarantee in accordance with
the plugging and abandonment plan
and other permit requirements when-
ever required to do so, the guarantee
will do so or establish a trust fund as
specified in §144.63(a) in the name of
the owner or operator.
(ii) The corporate guarantee will re-
main in force unless the guarantor
sends notice of cancellation by cer-
tified mail to the owner or operator
and the Regional Administrator, as
evidenced by the return receipts. Can-
cellation may not occur, however, dur-
ing the 120 days beginning on the date
of receipt of the notice of cancellation
by both the owner or operator and the
Regional Administrator, as evidenced
by the return receipts.
(ill) If the owner or operator fails to
provide alternate financial assurance
as specified in this section and obtain
the written approval of such alternate
assurance from the Regional Adminis-
trator within 90 days after receipt by
both the owner or operator and the Re-
gional Administrator of a notice of
cancellation of the corporate guar-
antee from the guarantor, the guar-
antor will provide such alternative fi-
nancial assurance in the name of the
owner or operator.
(g) Use of multiple financial mecha-
nisms. An owner or operator may sat-
isfy the requirements of this section by
establishing more than one financial
mechanism per injection well. These
mechanisms are limited to trust funds,
surety bonds, guaranteeing payment
into a trust fund, letters of credit, and
insurance. The mechanisms must be as
specified in paragraphs (a), (b), (d), and
(e), respectively, of this section, except
that it is the combination of mecha-
nisms, rather than the single mecha-
nism, which must provide financial as-
surance for an amount at least equal to
the adjusted plugging and abandon-
ment cost. If an owner or operator uses
a trust fund in combination with a sur-
ety bond or letter of credit, he may use
that trust fund as the standby trust
fund for the other mechanisms, A sin-
gle standby trust may be established
for two or more mechanisms. The Re-
gional Administrator may invoke any
or all of the mechanisms to provide for
plugging and abandonment of the injec-
tion well.
(h) Use of a financial mechanism for
multiple facilities. An owner or operator
may use a financial assurance mecha-
nism specified in this section to meet
the requirements of this section for
more than one injection well. Evidence
of financial assurance submitted to the
Regional Administrator must include a
list showing, for each injection well,
the EPA Identification Number, name,
address, and the amount of funds for
plugging and abandonment assured by
the mechanism. If the injection wells
covered by the mechanism are in more
than one Region, identical evidence of
financial assurance must be submitted
to and maintained with the Regional
Administrators of all such Regions.
The amount of funds available through
664
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Environmental Protection Agency
§144.6S
the mechanism must be no less than
the sum of funds that would be avail-
able if a separate mechanism had been
established and maintained for each in-
jection well. In directing funds avail-
able through the mechanism for plug-
ging and abandonment of any of the in-
jection wells covered by the mecha-
nism, the Eegional Administrator may
direct only the amount of funds des-
ignated for that injection well, unless
the owner or operator agrees to use ad-
ditional funds available under the
mechanism.
-------
§144.66
40 CFR Ch. 1 (7-1-04 Edition)
through the State and Federal mecha-
nisms must at least equal the amounts
required by this subpart.
§ 144.66 State assumption of responsi-
bility.
(a) If a State either assumes legal re-
sponsibility for an owner's or opera-
tor's compliance with the plugging and
abandonment requirements of these
regulations or assures that funds will
be available from State sources to
cover these requirements, the owner or
operator will be in compliance with the
requirements of this subpart if the Re-
gional Administrator determines that
the State's assumption of responsi-
bility is at least equivalent to the
mechanisms specified in this subpart.
The Regional Administrator will evalu-
ate the equivalency of State guaran-
tees mainly in terms of (1) certainty of
the availability of funds for the re-
quired plugging and abandonment cov-
erage and (2) the amount of funds that
will be made available. The Regional
Administrator may also consider other
factors. The owner or operator must
submit to the Regional Administrator
a letter from the State describing the
nature of the State's assumption of re-
sponsibility together with a letter from
the owner or operator requesting' that
the State's asumption of responsibility
be considered acceptable for meeting
the requirements of this subpart. The
letter from the State must include, or
have attached to it, the following in-
formation: the facility's EPA Identi-
fication Number, name and address,
and the amounts of funds for plugging
and abandonment coverage that are
guaranteed by the State. The Regional
Administrator will notify the owner or
operator of his determination regard-
ing the acceptability of the State's
guarantee in lieu of mechanisms speci-
fied in this subpart. The Regional Ad-
ministrator may require the owner or
operator to submit additional informa-
tion as is deemed necessary to make
this determination. Pending this deter-
mination, the owner or operator will be
deemed to be in compliance with
§144.63.
(b) If a State's assumption of respon-
sibility is found acceptable as specified
in paragraph (a) of this section except
for the amount of funds available, the
owner or operator may satisfy the re-
quirements of this subpart by use of
both the State's assurance and addi-
tional financial mechanisms as speci-
fied in this subpart. The amount of
funds available through the State and
Federal mechanisms must at least
equal the amount required by this sub-
part.
§ 144.70 Wording of the instruments,
(a)(l) A trust agreement for a trust
fund, as specified in §144.63(a) of this
chapter, must be worded as follows, ex-
cept that instructions in brackets are
to be replaced with the relevant infor-
mation and the brackets deleted:
TRUST AGREEMENT
TRUST AGREEMENT, the "Agreement,"
entered into as of [date] by and between
[name of the owner or operator], a [name of
State] [insert "corporation," "partnership,"
"association," or "proprietorship"], the
"Grantor," and [name of corporate trustee],
[insert "incorporated in the State of "
or "a national bank"], the Trustee."
Whereas, the United States Environmental
Protection Agency, "EPA," an agency of the
United States Government, has established
certain regulations applicable to the Grant-
or, requiring that an owner or operator of an
injection well stall provide assurance that
funds will be available when needed for plug-
ging and abandonment of the injection well,
Whereas, the Grantor has elected to estab-
lish a trust to provide all or part of such fi-
nancial assurance for the facility(ies) identi-
fied herein,
Whereas, the Grantor, acting through its
duly authorized officers, has selected the
Trustee to be the trustee under this agree-
ment, and the Trustee is willing" to act as
trustee,
Now, therefore, the Grantor and the Trust-
ee agree as follows:
Section 1. Definitions. As used in this Agree-
ment:
(a) The term "Grantor" means the owner or
operator who enters into this Agreement and
any successors or assigns of the Grantor.
(b) The term "Trustee" means the Trustee
who enters into this Agreement and any suc-
cessor Trustee.
(c) Facility or activity means any "under-
ground injection well" or any other facility
or activity that is subject to regulation
under the Underground Injection Control
Program.
Section 2. Identification of Facilities and Cost
Estimates. This Agreement pertains to the fa-
cilities and cost estimates identified on at-
tached Schedule A [on Schedule A, for each
facility list the EPA Identification Number,
666
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Environmental Protection Agency
§144.70
name, address, and the current plugging and
abandonment cost estimate, or portions
thereof, for which financial assurance is
demonstrated by this Agreement],
Section 3, Establishment of Fund, The Grant-
or and the Trustee hereby establish a trust
fund, the "Fund," for the benefit of EPA. The
Grantor and the Trustee intend that no third
party have access to the Fund except as
herein provided. The Fund is established ini-
tially as consisting of the property, which is
acceptable to the Trustee, described in
Schedule B attached hereto. Such property
and any other property subsequently trans-
ferred to the Trustee is referred to as the
Fund, together with all earnings and profits
thereon, less any payments or distributions
made by the Trustee pursuant to this Agree-
ment. The Fund shall be held by the Trustee.
IN TRUST, as hereinafter provided. The
Trustee shall not be responsible nor shall it
undertake any responsibility for the amount
or adequacy of, nor any duty to collect from
the Grantor, any payments necessary to dis-
charge any liabilities of the Grantor estab-
lished by EPA.
Section 4. Payment for Plugging and Aban-
donment, The Trustee shall make payments
from the Fund as the EPA Regional Admin-
istrator shall direct, in writing-, to provide
for the payment of the costs of plugging and
abandonment of the injection wells covered
by this Agreement. The Trustee shall reim-
burse the Grantor or other persons as speci-
fied by the EPA Regional Administrator
from the Fund for plugging and abandon-
ment expenditures in such amounts as the
EPA Regional Administrator shall direct in
writing, In addition, the Trustee shall refund
to the Grantor such amounts as the EPA Re-
gional Administrator specifies in writing,
Upon refund, such funds shall no longer con-
stitute part of the Fund as defined herein.
Section 5, Payments Comprising the Fund.
Payments made to the Trustee for the Fund
shall consist of cash or securities acceptable
to the Trustee.
Section 6, Trustee Management. The Trustee
shall invest and reinvest the principal and
income of the Fund and keep the Fund in-
vested as a single fund, without distinction
between principal and income, in accordance
with general investment policies and guide-
lines which the Grantor may communicate
in writing to the Trustee from time to time.
subject, however, to the provisions of this
Section. In investing, reinvesting1, exchang-
ing, selling, and managing the Fund, the
Trustee shall discharge his duties with re-
spect to the trust fund solely in the interest
of the beneficiary and with the care, skill,
prudence, and diligence under the cir-
cumstanoes ther. prevailing which persons of
prudence, acting in a like capacity and fa-
miliar with such matters, would use in the
conduct of an enterprise of a like character
and with like aims: except that:
(i) Securities or other obligations of the
Grantor, or a.ny other owner or operator of
the facilities, or any of their affiliates as de-
fined in the Investment Company Act of 1940,
as amended. 15 U.S.C. 80a-2.(a), shall not be
acquired or held, unless they are securities
or other obligations of the Federal or a State
government;
(ii) The Trustee is authorized to invest the
Fund in time or demand deposits of the
Trustee, to the extent insured by an agency
of the Federal or State government; and
{iiiS The Trustee is authorized to hold cash
awaiting investment or distribution
uninvested for a reasonable time and with-
out liability for the payment of interest-
thereon.
Section 7. Commingling and Investment. The
Trustee is expressly authorized in its discre-
tion:
(a) To transfer from time to time any or
all of the assets of the Fund to any common,
commingled, or collective trust fund created
by the Trustee in which the Fund is eligible
to participate, subject to all of the provi-
sions thereof, to be commingled with the as-
sets of other trusts participating therein:
and
(b) To purchase shares in any investment
company registered under the Investment
Company Act of 1940, 15 U.S.C, SOa^l et seg.,
including one which may he created, man-
aged, underwritten, or to which investment
advice is rendered or the shares of which are
sold by the Trustee. The Trustee may vote
shares in Its discretion.
Section 8. Express Powers of Trustee. Without
in any way limiting the powers and discre-
tions conferred upon the Trustee by the
other provisions of this Agreement or by
law. the Trustee is expressly authorized and
empowered:
(a) To sell, exchange, convey, transfer, or
otherwise dispose of any property held by it,
by public or private sale. No person dealing
with the Trustee shall be bound to see to the
application of the purchase money or to in-
quire into the validity or expediency of any
such sale or other disposition:
(b) To make, execute, acknowledge, and de-
liver any and all documents of transfer and
conveyance and any and all other instru-
ments that may be necessary or appropriate
to carry out the powers herein granted:
(c) To register any securities held in the
Fund in its own name or in the name of a
nominee and to hold any security in bearer
form or in book entry, or to combine certifi-
cates representing1 such securities with cer-
tificates of the same issue held by the Trust-
ee in other fiduciary capacities, or to deposit
or arrange for the deposit of such securities
in a qualified central depository even
though, when so deposited, such securities
may be merged and held in bulk in the na,rne
of the nominee of such depositary with other
667
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§144.70
40 CFR Ch. I (7-1-04 Edition)
securities deposited therein by another per-
son, or to deposit or arrange for the deposit
of any securities issued by the United States
Government, or any agency or instrumen-
tality thereof, with a Federal Reserve bank,
but the books and records of the Trustee
shall at all times show that all such securi-
ties are part of the Fund;
(d) To deposit any cash in the Fund in in-
terest-bearing accounts maintained or sav-
ing's certificates issued by the Trustee, in its
separate corporate capacity, or in any other
banking institution affiliated with the
Trustee, to the extent insured by an agency
of the Federal or State government; and
(e) To compromise or otherwise adjust all
claims in favor of or against, the Fund.
Section 9. Taxes and Expenses, All taxes of
any kind that may be assessed or levied
against or in respect of the Fund and all bro-
kerage commissions incurred by the Fund
shall be paid from the Fund. All other ex-
penses incurred by the Trustee in connection
with, the administration of this Trust, in-
cluding fees for legal services rendered to the
Trustee, the compensation of the Trustee to
the extent not paid directly by the Grantor,
and all other proper charges and disburse-
ments of the Trustee shall be paid from the
Fund.
Section 10. Annual Valuation. The Trustee
shall annually, at least 30 days prior to the
anniversary date of establishment of the
Fund, furnish to the Grantor and to the ap-
propriate EPA Regional Administrator a
statement confirming the value of the Trust.
Any securities in the Fund shall be valued at
market value as of no more than 60 days
prior to the anniversary date of establish-
ment of the Fund. The failure of the Grantor
to object in writing to the Trustee within 90
days after the statement has been furnished
to the Grantor and the EPA Regional Admin-
istrator shall constitute a conclusively bind-
ing assent by the Grantor, barring the
Grantor from asserting any claim or liability
against the Trustee with respect to matters
disclosed in the statement.
Section 11. Advice of Counsel. The Trustee
may from time to time consult with counsel,
who may be counsel to the Grantor, with re-
spect to any question arising as to the con-
struction of this Agreement of any action to
be taken hereunder. The Trustee shall be
fully protected, to the extent permitted by
law, in acting upon the advice of counsel.
Section 12. Trustee Compensation. The Trust-
ee shall be entitled to reasonable compensa-
tion for its services as agreed upon in writ-
ing from time to time with the Grantor.
Section 13. Successor Trustee. The Trustee
may resign or the Grantor may replace the
Trustee, but such resignation or replacement
shall not be effective until the Grantor has
appointed a successor trustee and this suc-
cessor accepts the appointment. The suc-
cessor trustee shall have the same powers
and duties as those conferred upon the
Trustee hereunder. Upon the successor trust-
ee's acceptance of the appointment, the
Trustee shall assign, transfer, and pay over
to the successor trustee the funds and prop-
erties then constituting the Fund. If for any
reason the Grantor cannot or does not act in
the event of the resignation of the Trustee,
the Trustee may apply to a court of com-
petent jurisdiction for the appointment of a
successor trustee or for instructions. The
successor trustee shall specify the date on
which it assumes administration of the trust
in a writing sent to the Grantor, the EPA
Regional Administrator, and the present
Trustee by certified mail 10 days before such
change becomes effective. Any expenses in-
curred by the Trustee as a result of any of
the acts contemplated by this Section shall
be paid as provided in Section 9.
Section 14. Instructions to the Trustee, All or-
ders, requests, and instructions by the
Grantor to the Trustee shall be in writing,
signed by such persons as are designated in
the attached Exhibit A or such other des-
ignees as the Grantor may designate by
amendment to Exhibit A. The Trustee shall
be fully protected in acting without inquiry
in accordance with the Grantor's orders, re-
quests, and instructions. All orders, re-
quests, and instructions by the EPA Re-
gional Administrator to the Trustee shall be
in writing, signed by the EPA Regional Ad-
ministrators of the Regions in which the fa-
cilities are located, or their designees, and
the Trustee shall act and shall be fully pro-
tected in acting in accordance with such or-
ders, requests, and instructions. The Trustee
shall have the right to assume, in the ab-
sence of written notice to the contrary, that
no event constituting' a change or a termi-
nation of the authority of any person to act
on behalf of the Grantor or EPA hereunder
has occurred. The Trustee shall have no duty
to act in the absence of such orders, re-
quests, and instructions from the Grantor
and/or EPA, except as provided for herein.
Section IS. Notice of Nonpayment. The Trust-
ee shall notify the Grantor and the appro-
priate EPA Regional Administrator, by cer-
tified mail within 10 days following the expi-
ration of the 30-day period after the anniver-
sary of the establishment of the Trust, if no
payment is received from the Grantor during
that period. After the pay-in period is com-
pleted, the Trustee shall not be required to
send a notice of nonpayment.
Section 16. Amendment of Agreement. This
Agreement may be amended by an instru-
ment in writing executed by the Grantor, the
Trustee, and the appropriate EPA Regional
Administrator, or by the Trustee and the ap-
propriate EPA Regional Administrator if the
Grantor ceases to exist.
Section 17. Irrevocability and Termination.
Subject to the right of the parties to amend
this Agreement as provided in Section 16,
668
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Environmental Protection Agency
§144.70
this Trust shall be irrevocable and shall con -
tinue until terminated at the written agree-
ment of the Grantor, the Trustee, and the
EPA Regional Administrator, or by the
Trustee and the EPA Regional Adminis-
trator if the Grantor ceases to exist. Upon
termination of the Trust, all remaining trust
property, less final trust administration ex-
penses, shall be delivered to the Grantor,
Section 18. Immunity and Indemnification.
The Trustee shall not incur personal liabil-
ity of any nature in connection with any act-
or omission, made in good faith, in the ad-
ministration of this Trust, or in carrying out
any directions by the Grantor or the EPA
Regional Administrator issued in accordance
with this Agreement, The Trustee shall be
indemnified and saved harmless by the
Grantor or from the Trust Fund, or both,
from and against any personal liability to
which the Trustee may be subjected by rea-
son of any act or conduct in its official ca-
pacity, including all expenses reasonably in-
curred in its defense in the event the Grant-
or fails to provide such defense.
Section 19. Choice of Law. This Agreement
shall be administered, construed, and en-
forced according to the laws of the State of
[insert name of State].
Section 20. Interpretation. As used in this
Agreement, words in the singular include the
plural and words in the plural include the
singular. The descriptive headings for each
Section of this Agreement shall not affect
the interpretation or the legal efficacy of
this Agreement.
In Witness Whereof the parties have caused
this Agreement to be executed by their re-
spective officers duly authorized and their
corporate seals to he hereunto affixed and at-
tested as of the date first above written. The
parties below certify that the wording: of this
Agreement is identical to the wording speci-
fied in 40 CPB 144.70(a)(l) as such regulations
were constituted on the date first above
written.
[Signature of Grantor!
By [Title]
Attest:
[TITLE]
[SEAL]
[Signature of Trustee]
By
Attest:
[TITLE]
[SEAL]
(2) The following Is an example of the
certification of acknowledgment which
must accompany the trust agreement
for a trust fund as specified in
§144.63(a). State requirements may dif-
fer on the proper content of this ac-
knowledgment.
State of
County of
On this (date], before me personally came
[owner or operator] to me known, who, being
by me duly sworn, did depose and say that
she/he resides at [address], that she/he is
[title] of [corporation], the corporation de-
scribed in and which executed the above in-
strument: that she/he knows the seal of said
corporation; that the seal affixed to such in-
strument is such corporate seal; that it was
so affixed by order to the Board of Directors
of said corporation, and that she/he signed
her/his name thereto by like order.
[Signature of Notary Public]
(b) A surety bond guaranteeing pay-
ment into a trust fund, as specified in
§144,63 of this chapter, must be worded
as follows, except that instructions in
brackets are to be replaced with the
relevant information and the brackets
deleted:
FINANCIAL GUARANTEE BOND
Dated bond executed:
Effective date:
Principal: llegal name and business address
of owner or operator].
Type of organization: [insert "individual,"
"joint venture," "partnership," or "corpora-
tion"].
State of incorporation:
Surety(ies): [narne(s) and business ad-
dress(es;].
EPA Identification Number, name, address.
and plugging: and abandonment amount(s)
for each facility guaranteed by this bond [in-
dicate plugging and abandonment amounts
separately]:
Total penal sum of bond: $
Surety's bond number:
Know All Persons By These Presents, That
we, the Principal and Surity(ies) hereto are
firmly bound to the U.S. Environmental Pro-
tection Agency (hereinafter called EPA), in
the above penal sum for the payment of
which we bind ourselves, our heirs, execu-
tors, administrators, successors, and assigns
jointly and severally; provided that, where
the Surety(les) are corporations acting as co-
surties, we, the Sureties, hind ourselves in
such sum "jointly and severally" only for the
purpose of allowing a joint action or actions
against any or all of us. and for all other pur-
poses each Surety binds itself, jointly and
severally with the Principal, for the pay-
ment of such sum only as is set forth oppo-
site the name of such Surety, but if no limit
of liability is indicated, the limit of liability
shall be the full amount of the penal sum.
669
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§144.70
40 CFR Ch. 1 (7-1-04 Edition)
Whereas said Principal is required, under
the Underground Injection Control Regula-
tions (UIC), to have a permit or comply with
requirements to operate under rule in order
to own or operate each injection well identi-
fied above, and
Whereas said Principal is required to pro-
vide financial assurance for plugging and
abandonment as a condition of the permit or
provisions to operate under rule, and
Whereas said Principal shall establish a
standby trust fund as is required when a sur-
ety bond is used to provide such financial as-
surance;
Now, therefore, the conditions of the obli-
gation are such that if the Principal shall
faithfully, before the beginning of plugging
and abandonment of each injection well
identified above, fund the standby trust fund
in the amount(s) identified above for the in-
jection well,
Or if the Principal shall fund the standby
trust fund in such amount(s) within 15 days
after an order to begin plugging and aban-
donment Is issued by an EPA Regional Ad-
ministrator or a U.S. district court or other
court of competent jurisdiction,
Or, if the Principal shall provide alternate
financial assurance, as specified in subpart P
of 40 CPE part 144, as applicable, and obtain
the EPA Regional Administrator's written
approval of such assurance, within 90 days
after the date of notice of cancellation is re-
ceived by both the Principal and the EPA
Regional Administrator(s) from the Sur-
ety(ies), then this obligation shall be null
and void, otherwise it is to remain in full
force and effect.
The Surety(ies) shall become liable on this
bond obligation only when the Principal has
failed to fulfill the conditions described
above. Upon notification by an EPA Re-
gional Administrator that the Principal has
failed to perform as guaranteed by this bond,
the Surety(ies) shall place funds in the
amount guaranteed for the injection well(s)
into the standby trust funds as directed by
the EPA Regional Administrator.
The liability of the Surety(ies) shall not be
discharged by any payment or succession of
payments hereunder, unless and until such
payment or payments shall amount in the
aggregate to the penal sum of the bond, but
in no event shall the obligation of the Sur-
ety(ies) hereunder exceed the amount of said
penal sum.
The Surety(ies) may cancel tie bond by
sending notice of cancellation by certified
mail to the Principal and to the EPA Re-
gional Administrator(s) for the Region(s) in
which the injection well(s) is (are) located,
provided, however, that that cancellation
shall not occur during the 120 days beginning
on the date of receipt of the notice of can-
cellation by both the Principal and the EPA
Regional Administrator(s), as evidenced by
the return receipts.
The Principal may terminate this bond by
sending written notice to the Surety(ies),
provided, however, that no such notice shall
become effective until the Surety(ies) re-
ceive(s) written authorization for termi-
nation of the bond by the EPA Regional Ad-
ministrator(s) of the Region(s) in which the
bonded facility(ies) is (are) located.
[The following paragraph is an optional
rider that may be included but is not re-
quired.]
Principal and Surety(ies) hereby agree to
adjust the penal sum of the bond yearly so
that it guarantees a new plugging and aban-
donment amount, provided that the penal
sum does not increase by more than 20
percent in any one year, and no decrease in
the penal sum takes place without the writ-
ten permission of the EPA Regional Admin-
istrator(s).
In Witness Whereof, the Principal and Snr-
ety(ies) have executed this Financial Guar-
antee Bond and have affixed their seals on
the date set forth above.
The persons whose signatures appear below
hereby certify that they are authorized to
execute this surety bond on behalf of the
Principal and Surety(ies) and that the word-
ing of this surety bond is identical to the
wording specified in 40 CPR 144.70(b) as such
regulations were constituted on the date this
bond was executed.
PRINCIPAL
[Signature(s)]
[Name(s)]
[Title(s)]
[Corporate seal]
CORPORATE SURETY(IES)
[Name and address]
State of incorporation: .
Liability limit: $ .
[Signature(s)]
[Name(s) and title(s)]
[Corporate seal]
[For every co-surety, provide signature(s),
corporate seal, and other information in the
same manner as for Surety above.]
Bond premium: $ ,
(c) A surety bond guaranteeing per-
formance of plugging and abandon-
ment, as specified in § 144.63(c), must be
worded as follows, except that the in-
structions in brackets are to be re-
placed with the relevant information
and the brackets deleted:
PERFORMANCE BOND
Date bond executed: .
Effective date: .
Principal: [legal name and business address
of owner or operator].
670
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Environmental Protection Agency
Type of organization: [insert "individual."
"joint venture," "partnership," or "corf
tion"].
joint venture," "partnership
on"].
State of incorporation:
corpora-
Surety(ies):
dress(es)]
[name(s) and business ad-
EPA Identification Number, name, address.
and plug'ging1 and abandonment amounts(s)
for each injection well guaranteed by this
bond [indicate plug'ging and abandonment
amounts for each well]:
Total penal sum of bond: $_
Surety's bond number: _
Know All Persons By These Presents. That
We. the Principal and Suretydes'i hereto are
firmly bound to the U.S. Environmental Pro-
tection Agency [hereinafter called EPA], in
the above penal sum for the payment of
which we bind ourselves, our heirs, execu-
tors, administrators, successors, and assigns
jointly and severally; provided that, where
the Surety(ies) are corporations acting as co-
sureties, we, the Sureties, bind ourselves in
such sum "jointly and severally" only for the
purpose of allowing a joint action or actions
against any or all of us, and for all other pur-
poses each Surety binds itself, jointly and
severally with the Principal, for the pay-
ment of such sum only as is set forth oppo-
site the name of such Surety, but if no limit
of liability is indicated, the limit of liability
shall be the full amount of the penal sum.
Whereas said Principal is required, under
the Undergourid Injection Control Regula-
tions, as amended, to have a permit or com-
ply with provisions to operate under rule for
each injection well identified a.bove, and
Whereas said Principal is required to pro-
vide financial assurance for plugging and
abandonment as a condition of the permit or
approval to operate under rule, and
Whereas said Principal shall establish a
standby trust fund as is required when a
surety bond is used to provide such financial
assurance:
Now. Therefore, the conditions of this obli-
gation are such that if the Principal shall
faithfully perform plugging and abandon-
ment, whenever required to do so, of each in-
jection well for which this bond guarantees
plugging and abandonment, in accordance
with the plugging and abandonment plan and
other retirements of the permit or provi-
sions for operating tinder rule and other re-
quirements of the permit or provisions for
operating under rule as may be amended,
pursuant to all applicable laws, statutes,
rules and regulations, as such laws, statutes.
rules, and regulations may be amended,
Or. if the Principal shall provide alternate
financial assurance as specified in subpart P
of 40 CFB part 144. and obtain the EPA Re-
gional Administrator's written approval of
such, assurance, within 90 days after the date
of notice of cancellation is received by both
§144.70
the Principal and the EPA Regional Admin-
istrator(s) from the Surety(ies), then this ob-
ligation shall be null and void, otherwise it
is to remain in full force and effect.
The Surety(ies) shall become liable on this
bond obligation only when the Principal has
failed to fulfill the conditions described
above.
Upon notification by an EPA Regional Ad-
ministrator that the Principal has been
found in violation of the plugging and aban-
donment requirements of 40 CFR part 144. for
an injection well which this bond guarantees
performances of plugging and abandonment,
the Surety(ies) shall either perform plugging
and abandonment in accordance with the
plugging and abandonment plan and other
permit requirements or previsions for oper-
ating under rule and other requirements or
place the amount for plugging and abandon-
ment into a standby trust fund as directed
by the EPA Regional Administrator.
Upon notification by an EPA Regional Ad-
ministrator that the Principal has failed to
provide alternate financial assurance as
specified in subpart P of 40 GPR part 144, and
obtain written approval of such assurance
from the EPA Regional Administrators;
during the 90 days following receipt by both
the Principal and the EPA Regional Admin-
istrator(s) of a notice of cancellation of the
bond, the Stirety(ies) shall place funds in the
amount guaranteed for the injection well(s)
into the standby trust fund as directed by
the EPA Regional Administrator.
The surety(ies) hereby waive(s) notifica-
tion of amendments to plugging and aban-
donment plans, permits, applicable laws,
statutes, rules, and regulations and agrees
that no such amendment shall in any way al-
leviate its (their) obligation on this bond.
The liability of the Surety(ies) shall not be
discharged by any payment or succession of
payments hereunder. unless and until such
payment or payments shall amount in the
aggregate to the penal sum of the bond, but
in no event shall the obligation of the Sur-
ety(ies) hereunder exceed the amount of said
penal sum.
The Surety(ies) may cancel the bond by
sending notice by certified mail to the owner
or operator and to the EPA Eegional Admin-
istrator(s) for the Region(s) in which the in-
jection well(s) is (are) located, provided.
however, that cancellation shall not occur
during the 120 days beginning on the date of
receipt of the notice of cancellation by both
the Principal and the EPA Regional Admin-
istrator(s), as evidenced by the return re-
ceipts.
The principal may terminate this bond by
sending written notice to the Surety(ies),
provided, however, that no such notice shall
671
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§144.70
40 CFR Ch. I (7-1-04 Edition)
become effective until the Surety(ies) re-
celve(s) written authorization for termi-
nation of the bond by the EPA Regional Ad-
ministrator(s) of the EPA Region(s) in which
the bonded injection well(s) is (are) located.
[The following paragraph is an optional
rider that may be included but is not re-
quired.]
Principal and Surety(ies) hereby agree to
adjust the penal sum of the bond yearly so
that it guarantees a new plugging and aban-
donment amount, provided that the penal
sum does not increase by more than 20
percent in any one year, and no decrease in
the penal sum takes place without the
written permission of the EPA Regional Ad-
ministrator(s).
In Witness Whereof, The Principal and Sur-
ety(ies) have executed this Performance
Bond and have affixed their seals on the date
set- forth above.
The persons whose signatures appear below
hereby certify that they are authorized to
execute this surety bond on behalf of the
Principal and Surety(ies) and that the word-
ing on this surety bond is identical to the
wording specified in 40 CPR 144.70(c) as such
regulation was constituted on the date this
bond was executed.
Principal.
[Signature(s)]
[Name(s)]
[Title(s)]
[Corporate seal]
[Corporate Surety(ies)]
[Name and address]
State of incorporation:
Liability limit: $ .
[Signature(s)]
[Name(s) and title(s)]
Corporate seal:
[For every co-surety, provide signature(s),
corporate seal, and other information in the
same manner as for Surety above.]
Bond premium: $ .
(d) A letter of credit, as specified in
|144.63(d) of this chapter, must be
worded as follows, except that Instruc-
tions in brackets are to be replaced
with the relevant information and the
brackets deleted:
IRREVOCABLE STANDBY LETTER OP CREDIT
Regional Adminlstrator(s)
Region(s)
U.S. Environmental Protection Agency.
Dear Sir or Madam:
We hereby establish our Irrevocable Stand-
by Letter of Credit No. in your favor,
at the request and for the account of [own-
er's or operator's name and address] up to
the aggregate amount of [In words] U.S. dol-
lars $ , available upon presentation [in-
sert, if more than one Regional Adminis-
trator is a beneficiary, "by any one of you"]
of
(1) Your sight draft, bearing reference to
this letter of credit No, , and
(2) Your signed statement reading as fol-
lows: "I certify that the amount of the draft
is payable pursuant to regulations issued
under authority of the Safe Drinking Water
Act."
This letter of credit is effective as of [date]
and shall expire on [date at least 1 year
later], but such expiration date shall be
automatically extended for a period of [at
least 1 year] on [date] and on each successive
expiration date, unless, at least 120 days be-
fore the current expiration date, we notify
both you and [owner's or operator's name] by
certified mail that we have decided not to
extend this letter of credit beyond the cur-
rent expiration date. In the event you are so
notified, any unused portion of the credit
shall be available upon presentation of your
sight draft for 120 days after the date of re-
ceipt by both you and [owner's or operator's
name], as shown on the signed return
receipts.
Whenever this letter of credit is drawn on
under and in compliance with the terms of
this credit, we shall duly honor such draft
upon presentation to us, and we shall deposit
the amount of the draft directly into the
standby trust fund of [owner's or operator's
name] in accordance with your instructions.
We certify that the wording of this letter
of credit is identical to the wording specified
in 40 CPR 144.7Q(d) as such regulations were
constituted on the date shown immediately
below.
[Signature(s) and title(s) of official(s) of
issuing institution]
[Date]
This credit is subject to [insert "the most
recent edition of the Uniform Customs and
Practice for Documentary Credits, published
and copyrighted by the International Cham-
ber of Commerce," or "the Uniform Commer-
cial Code"],
(e) A certificate of insurance, as spec-
ified in §144.63(e) of this chapter, must
be worded as follows, except that in-
structions in brackets are to be re-
placed with the relevant information
and the brackets deleted:
Certificate of Insurance for Plugging and
Abandonment
Name and Address of Insurer (herein called
the "insurer"):
Name and Address of Insurer (herein called
the "insurer"):
Injection Wells covered: [list for each well:
The EPA Identification Number, name, ad-
dress, and the amount of insurance for plug-
ging and abandonment (these amounts for all
672
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Environmental Protection Agency
§ 144.70
injection wells covered must total the face
amount shown below).]
Pace Amount: _
Policy Number: __
Effective Date:
The insurer hereby certifies that it has
issued to the Insured the policy of insurance
identified above to provide financial assur-
ance for plugging and abandonment for the
injection wells identified above. The Insurer
further warrants that such policy conforms
in all respects with the requirements of 40
CPE, 144.63(e), as applicable and as such regu-
lations were constituted on the date shown
immediately below. It Is agreed that any
provision of the policy inconsistent with
such regulations is hereby amended to elimi-
nate such inconsistency.
Whenever requested by the EPA Regional
Admlnistrator(s) of the U.S. Environmental
Protection Agency, the Insurer agrees to fur-
nish to the EPA Regional Administrators) a
duplicate original of the policy listed above,
including all endorsements thereon.
I hereby certify that the wording' of this
certificate is identical to the wording speci-
fied in 40 CFR 144.70(6) as such regulations
were constituted on the date shown imme-
diately below.
[Authorized signature of Insurer]
[Name of person signing]
[Title of person signing]
[Signature of witness or notary:]
[Date] ~ " ~~ "
(f) A letter from the chief financial
officer, as specified in §144.63(f) of this
chapter, must be worded as follows, ex-
cept that instructions in brackets are
to be replaced with the relevant infor-
mation and the brackets deleted:
LETTER FROM CHIEF FINANCIAL OFFICEH
[Address to Regional Administrator of
every Region in which Injection wells for
which financial responsibility is to be dem-
onstrated through the financial test are
located.]
I am the chief financial officer of [name
and address of firm.] This letter is in support
of this firm's use of the financial test to
demonstrate financial assurance, as specified
in subpart P of 40 CFE part 144.
[Fill out the following four paragraphs re-
garding' injection wells and associated cost
estimates. If your firm has no injection wells
that belong in a particular paragraph, write
"None" in the space indicated. For each injec-
tion well, include its EPA Identification
Number, name, address, and current plug-
ging and abandonment cost estimate.]
1. This firm is the owner or operator of the
following injection wells for which financial
assurance for plugging and abandonment is
demonstrated through the financial test
specified in subpart F of 40 CFR part 144. The
current plugging and abandonment cost esti-
mate covered by the test is shown for each
injection well:
2. This firm guarantees, through the cor-
porate guarantee specified in subpart F of 40
CFR part 144, the plugging and abandonment
of the following1 injection wells owned or op-
erated by subsidaries of this firm. The cur-
rent cost estimate for plugging and abandon-
ment so guaranteed is shown for each injec-
tion well:
3. In States where EPA is not admin-
istering the financial requirements of sub-
part P of 40 CPR part 144, this firm, as owner
or operator or guarantor, is demonstrating
financial assurance for the plugging and
abandoment of the following' injection wells
through the use of a test equivalent or sub-
stantially equivalent to the financial test
specified in subpart F of 40 CFR part 144. The
current plugging and abandonment cost esti-
mate covered by such a test is shown for
each injection well: .
4. This firm is the owner or operator of the
following injection wells for which financial
assurance for plugging and abandonment is
not demonstrated either to EPA or a State
through the financial test or any other fi-
nancial assurance mechanism specified in
subpart P of 40 CFR part 144 or equivalent or
substantially equivalent State mechanisms.
The current plugging and abandonment cost
estimate not covered by such financial assur-
ance is shown for each injection well:
This firm [insert "is required" or "is not re-
quired"] to file a Form 10K with the Securi-
ties and Exchange Commission (SEC) for the
latest fiscal year.
The fiscal year of this firm ends on
[month, day]. The figures for the following
items marked with an asterisk are derived
from this firm's independently audited, year-
end financial statements for the latest com-
pleted fiscal year, ended [date],
[Fill in Alternative I if the criteria of para-
graph (f)(lXi) of §144.63 of this chapter are
used. Fill in Alternative II if the criteria of
paragraph CfXIKii) of §144.63 of this chapter
are used.]
ALTERNATIVE I
1. (a) Current plugging and abandonment cost $
(b) Sum of the company's financial re-
sponsiDilities under 40 CFR Parts 264
and 265, Subpart H, currently met using
the financial test or corporate guarantee
(c) Total of Sines a and b
'2. Total liabilities [if any portion o! the plug-
ging and abandonment cosi is included in
iotal liabilities, you may deduct the amount
of that portion from this line and add that
amoun! to lines 3 and 41
'3. Tangible net worth
"4. Net worth
*5. Current assets
*6, Current liabilities
*7, Net working capital [line 5 minus line 6]
673
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§ 144.70
40 CFR Ch. I (7-1-04 Edition)
ALTERNATIVE I — Continued
'8. The sum of net income plus depreciation,
depletion and amortization .............................
*9. Total assets in U.S. {required only if less
than 90% of firm's assets are located in
U.S.) [[[
Yes
10, Is line 3 at least S10 million? ..................
11 . Is line 3 at least 6 times line
Kc)? [[[
12. Is line 7 at least 6 times line
"13. Are at least 90% of firm's as-
sets located in the U.S.? If not,
complete line 14
14. is line 9 at least 6 times line
He)?
15. Is line 2 divided by line 4 less
than 2,0?
16. Is line 8 divided by line 2
greater than 0.1?
17. Is line 5 divided by line 6
greater than 1.S?
ALTERNATIVE II
1. (a) Current plugging and abandonment cost
(b) Sum of the company's financial re-
sponsibilities under 40 CFR Parts 264
and 265, Subpart H, currently met using
the financial test or corporate guarantee
(c) Total of lines a and b
2. Current bond rating of most recent issuance
of this firm and name of rating service
3. Date of issuance of bond
4. Date of maturity of bond
*5. Tangible net worth [if any portion of the
plugging and abandonment cost estimate is
included in 'total liabilities1' on your firm's fi-
nancial statements, you may add the amount
of that portion to this line] ,....
*6, Total assets in U.S. (required only if less
than 90% of firm's assets are located in
U.S.)
Yes
7. Is line S at least $10 million? ....
8. Is line 5 at least 6 times line
"9. Are at least 90% of the firm's
assets located in the U.S.? If
not, complete line 10 ..................
10, Is line 6 at least 6 times line
I hereby certify that the wording of this
letter is identical to the wording specified in
40 CFR 144.70(f) as such regulations were con-
stituted on the date shown immediately
below.
[Signature]
[Name]
[Title]
[Date]
(g) A corporate guarantee as specified
in §144.63(e) must tie worded as follows
except that instructions in brackets
are to be replaced with the relevant in-
formation and the bracketed material
deleted:
GUARANTEE FOE PLUGGING AND ABANDONMENT
Guarantee made this day of ,
19 , by [name of guaranteeing entity], a
business corporation organized under the
laws of the State of , herein referred
to as guarantor, to the United States Envi-
ronmental Protection Agency (EPA), obli-
gee, on behalf of our subsidiary [owner or op-
erator] of [business address].
Recitals
1. Guarantor meets or exceeds the financial
test criteria and agrees to comply with the
reporting requirements for guarantors as
specified in 40 CFR 144.63(e).
2, [Owner or operator] owns or operates the
following Class I hazardous waste injection
well covered by this guarantee: [List for each
facility: EPA Identification Number, name,
and address. Indicate for each whether guar-
antee is for closure, post-closure care, or
both.]
3. "Plugging and abandonment plan" as
used below refers to the plans maintained as
required by 40 CFR part 144 for the plugging
and abandonment of injection wells as iden-
tified above.
4, For value received from [owner or oper-
ator], guarantor guarantees to EPA that in
the event that [owner or operator] fails to
perform ["plugging and abandonment"] of the
above facility(ies) in accordance with the
plugging and abandonment plan and other
requirements when required to do so, the
guarantor will do so or fund a trust fund as
specified in 40 CFR 144.63 in the name of
[owner or operator] in the amount of the ad-
justed plugging and abandonment cost esti-
mates prepared as specified in 40 CFR 144.62,
5. Guarantor agrees that, if at the end of
any fiscal year before termination of this
guarantee, the guarantor fails to meet the fi-
nancial test criteria, guarantor will send
within 90 days, by certified mail, notice to
the EPA Regional Administrator(s) for the
Reglon(s) in which the facility(ies) is (are)
located and to [owner or operator] that he
intends to provide alternate financial assur-
ance as specified in 40 CFE 144.63 in the name
of [owner or operator]. Within 30 days after
sending such notice, the guarantor will es-
tablish such financial assurance if [owner or
operator] has not done so.
6. The guarantor agrees to notify the Re-
gional Administrator, by certified mail, of a
voluntary or involuntary case under Title 11,
U.S. Code, naming guarantor as debtor, with-
in 10 days after its commencement.
7, Guarantor agrees that within 30 days
after being notified by an EPA Regional Ad-
ministrator of a determination that guar-
antor no longer meets the financial test cri-
teria or that he is disallowed from con-
tinuing as a guarantor of plugging and
-------
Environmental Protection Agency
§144,80
144,63, in the name of [owner or operator] if
[owner or operator] has not done so.
8. Guarantor agrees to remain bound under
tills guarantee notwithstanding any or all of
the following: amendment or modification of
the plugging and abandonment plan, the ex-
tension or reduction of the time of perform-
ance of plugging and abandonment or any
other modification or alteration of an obli-
gation of [owner or operator] pursuant to 40
CFR part 144.
9. Guarantor agrees to remain bound under
this guarantee for so long as [owner or oper-
ator] must comply with tie applicable finan-
cial assurance requirements of 40 CFR part
144 for the above-listed facilities, except that
guarantor may cancel this guarantee by
sending notice by certified mail, to the EPA
Regional Administrators) for the Reglon(s)
in which the facillty(ies) is (are) located and
to [owner or operator], such cancellation to
become effective no earlier than 120 days
after actual receipt of such notice by both
EPA and [owner or operator] as evidenced by
the return receipts.
10. Guarantor agrees that if [owner or oper-
ator] fails to provide alternate financial as-
surance and obtain written approval of such
assurance from the EPA Regional Admlnis-
trator(s) within 90 days after a notice of can-
cellation by the guarantor is recei\'ed by
both the EPA Regional Adrninistrator(s) and
[owner or operator], guarantor will provide
alternate financial assurance as specified in
40 CFR 144.63 in the name of [owner or oper-
ator],
1.1. Guarantor expressly waives notice of
acceptance of this guarantee by the EPA or
by [owner or operator]. Guarantor also ex-
pressly waives notice of amendments or
modifications of the plugging and abandon-
ment plan.
I hereby certify that the wording of this
guarantee is identical to the wording speci-
fied in 40 CPR 144.70if),
Effective date:
[Name of guarantor]
[Authorized signature for guarantor]
[Type name of person signing]
[Title of person sig'ningj
Signature of witness or notary:
[48 PR 14189. Apr, 1, 1983, as amended at 59
FR 29959, June 10, 1994]
Subpart G—Requirements for
Owners and Operators of
Class V Injection Wells
SOURCK: 64 FR 6856G. Dec. 7, 1999, unless
otherwise noted.
§ 144,79 General.
This subpart tells you what require-
ments apply if you own or operate a
Class V injection well. You may also be
required to follow additional require-
ments listed in the rest of this part.
Where they may apply, these other re-
quirements are referenced rather than
repeated. The requirements described
in this subpart and elsewhere in this
part are to protect underground
sources of drinking water and are part
of the Underground Injection Control
(UIC) Program established under the
Safe Drinking Water Act. This subpart
Is written in a special format to make
it easier to understand the regulatory
requirements. Like other EPA regula-
tions, it establishes enforceable legal
requirements.
DEFINITION OF CLASS V INJECTION
WELLS
§144,80 What is a Class V injection
well?
As described in §144.6, injection wells
are classified as follows:
(a) Class I. (1) Wells used by genera-
tors of hazardous waste or owners or
operators of hazardous waste manage-
ment facilities to inject hazardous
waste beneath the lowermost forma-
tion containing, within one-quarter
mile of the well bore, an underground
source of drinking water.
(2) Other industrial and municipal
disposal wells which inject fluids be-
neath the lowermost formation con-
taining-, within one quarter mile of the
well bore, an underground source of
drinking- water;
(3) Kadioactive waste disposal wells
which inject fluids below the lower-
most formation containing an under-
ground source of drinking water within
one quarter mile of the well bore.
(b) Class II. Wells which inject fluids:
(1) Which are brought to the surface
in connection with natural gas storage
operations, or conventional oil or nat-
ural gas production and may be com-
mingled with waste waters from gas
plants which are an integral part of
production operations, unless those wa-
ters are classified as a hazardous waste
at the time of injection.
(2) For enhanced recovery of oil or
natural gas; and
(3) For storage of hydrocarbons
which are liquid at standard tempera-
ture and pressure.
675
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§144.81
40 CFR Ch. I (7-1-04 Edition)
(c) Class IH, Wells which inject fluids
for extraction of minerals including:
(1) Mining of sulfur by the Frasch
process;
(2) In situ production of uranium or
other metals; this category includes
only in situ production from ore bodies
which have not been conventionally
mined. Solution mining of conven-
tional mines such as stopes leaching is
included in Class V.
(3) Solution mining of salts or pot-
ash,
(d) Class IV, (1) Wells used by genera-
tors of hazardous waste or of radio-
active waste, by owners and operators
of hazardous waste management facili-
ties, or by owners or operators of radio-
active waste disposal sites to dispose of
hazardous waste or radioactive waste
into a formation which within one
quarter (Vt) mile of the well contains
an underground source of drinking
water.
(2) Wells used by generators of haz-
ardous waste or of radioactive waste,
by owners and operators of hazardous
waste management facilities, or by
owners or operators of radioactive
waste disposal sites to dispose of haz-
ardous waste or radioactive waste
above a formation which within one
quarter (V*) mile of the well contains
an underground source of drinking
water.
(3) Wells used by generators of haz-
ardous waste or owners or operators of
hazardous waste management facilities
to dispose of hazardous waste, which
cannot be classified under paragraph
(a)(l) or (d)(l) and (2) of this section
(e.g., wells used to dispose of hazardous
waste into or above a formation which
contains an aquifer which has been ex-
empted pursuant to 40 CPB 146.04).
(e) Class V. Injection wells not in-
cluded in Class I, II, III or IV. Typi-
cally, Class V wells are shallow wells
used to place a variety of fluids di-
rectly below the land surface. However,
if the fluids you place in the ground
qualify as a hazardous waste under the
Resource Conservation and Eecovery
Act (BOBA), your well is either a Class
I or Class IV well, not a Class V well.
Examples of Class V wells are described
in §144.81.
§ 144.81 Does this suhpart apply to me?
This subpart applies to you if you
own or operate a Class V well, for ex-
ample:
(1) Air conditioning return flow wells
used to return to the supply aquifer the
water used for heating or cooling in a
heat pump;
(2) Large capacity cesspools includ-
ing multiple dwelling, community or
regional cesspools, or other devices
that receive sanitary wastes, con-
taining human excreta, which have an
open bottom and sometimes perforated
sides. The TJIC requirements do not
apply to single family residential cess-
pools nor to non-residential cesspools
which receive solely sanitary waste
and have the capacity to serve fewer
than 20 persons a day.
(S) Cooling water return flow wells
used to inject water previously used for
cooling;
(4) Drainage wells used to drain sur-
face fluids, primarily storm runoff,
into a subsurface formation;
(5) Dry wells used for the injection of
wastes into a subsurface formation;
(6) Recharge wells used to replenish
the water in an aquifer;
(7) Salt water intrusion barrier wells
used to inject water into a fresh aqui-
fer to prevent the intrusion of salt
water into the fresh water;
(8) Sand backfill and other backfill
wells used to inject a mixture of water
and sand, mill tailings or other solids
into mined out portions of subsurface
mines whether what is injected is a ra-
dioactive waste or not.
(9) Septic system wells used to inject
the waste or effluent from a multiple
dwelling, business establishment, com-
munity or regional business establish-
ment septic tank. The TJIC require-
ments do not apply to single family
residential septic system wells, nor to
non-residential septic system wells
which are used solely for the disposal
of sanitary waste and have the capac-
ity to serve fewer than 20 persons a
day.
(10) Subsidence control wells (not
used for the purpose of oil or natural
gas production) used to inject fluids
into a non-oil or gas producing zone to
reduce or eliminate subsidence associ-
ated with the overdraft of fresh water;
676
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Environmental Protection Agency
§144.82
(11) Injection wells associated with
the recovery of geothermal energy for
heating, aquaculture and production of
electric power;
(12) Wells used for solution mining of
conventional mines such as stopes
leaching;
(13) Wells used to inject spent brine
into the same formation from which it
was withdrawn after extraction of
halogens or their salts;
(14) Injection wells used in experi-
mental technologies.
(15) Injection wells used for in situ
recovery of lignite, coal, tar sands, and
oil shale,
(16) Motor vehicle waste disposal
wells that receive or have received
fluids from vehicular repair or mainte-
nance activities, such as an auto body
repair shop, automotive repair shop,
new and used car dealership, specialty
repair shop (e.g., transmission and
muffler repair shop), or any facility
that does any vehicular repair work.
Fluids disposed in these wells may con-
tain organic and inorganic chemicals
in concentrations that exceed the max-
imum contaminant levels (MCLs) es-
tablished by the primary drinking
water regulations (see 40 CFR part 141).
These fluids also may include waste pe-
troleum products and may contain con-
taminants, such as heavy metals and
volatile organic compounds, which
pose risks to human health.
[64 FR 68566, Dec. 7. 1999, as amended at 67
PR 39593, June 7, 2002]
REQUIREMENTS FOR ALL CLASS V
INJECTION WELLS
§ 144.82 What must I do to protect un-
derground sources of drinking
water?
If you own or operate any type of
Class V well, the regulations below re-
quire that you cannot allow movement
of fluid into USDWs that might cause
endangerment, you must comply with
other Federal UIC requirements in 40
CFR parts 144 through 147, and you
must comply with any other measures
required by your State or EPA Re-
gional Office UIC Program to protect
USDWs, and you must properly close
your well when you are through using
it. You also must submit basic infor-
mation about your well, as described in
§144.83.
(a) Prohibition of fluid movement. (1)
As described in §144.12(a), your injec-
tion activity cannot allow the move-
ment of fluid containing any contami-
nant into USDWs, if the presence of
that contaminant may cause a viola-
tion of the primary drinking water
standards under 40 CFR part 141, other
health based standards, or may other-
wise adversely affect the health of per-
sons. This prohibition applies to your
well construction, operation, mainte-
nance, conversion, plugging, closure, or
any other injection activity.
(2) If the Director of the UIC Pro-
gram in your State or EPA Region
learns that your injection activity may
endanger USDWs, he or she may re-
quire you to close your well, require
you to get a permit, or require other
actions listed in §144.12(c), (d), or fe).
(b) Closure requirements. You must
close the well in a manner that com-
plies with the above prohibition of
fluid movement. Also, you must dis-
pose or otherwise manage any soil,
gravel, sludge, liquids, or other mate-
rials removed from or adjacent to your
well in accordance with all applicable
Federal, State, and local regulations
and requirements.
(c) Other requirements in Parts 144
through 147. Beyond this subpart, you
are subject to other UIC Program re-
quirements in 40 CFR parts 144 through
147. While most of the relevant require-
ments are repeated or referenced in
this subpart for convenience, you need
to read these other parts to understand
the entire UIC Program.
(d) Other State or EPA requirements. 40
CPR parts 144 through 147 define min-
imum Federal UIC requirements. EPA
Regional Offices administering the UIC
Program have the flexibility to estab-
lish additional or more stringent re-
quirements based on the authorities in
parts 144 through 147, if believed to be
necessary to protect USDWs. States
can have their own authorities to es-
tablish additional or more stringent re-
quirements if needed to protect
USDWs. You must comply with these
additional requirements, if any exist in
your area. Contact the UIC Program
Director in your State or EPA Region
to learn more.
677
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§ 144.83
40 CFR Ch. I (7-1-04 Edition)
§ 144.83 Do I need to notify anyone
about my Class V injection well?
Yes, you need to provide basic "in-
ventory information" about your well
to the TJIO Director, if you haven't al-
ready. You also need to provide any ad-
ditional information that your UIC
Program Director requests in accord-
ance with the provisions of the UIC
regulations.
(a) Inventory requirements. Unless you
know you have already satisfied the in-
ventory requirements in §144.26 that
were in effect prior to the issuance of
this Subpart G, you must give your
UIC Program Director certain informa-
tion about yourself and your injection
operation.
NOTE: This information is requested on na-
tional form "Inventory of Injection Wells,"
OMB No. 2040-0042.
(1) The requirements differ depending
on your well status and location, as de-
scribed in the following table:
If your well is ...
(i) New (prior to construction of your welt}
(ii) Existing (construction underway or
completed).
And you're in one of these locations
("Primacy" States, where the State runs
the Class V UIC Program): Alabama, Ar-
kansas, Commonwealth of Northern
Mariana islands, Connecticut, Delaware,
Florida, Georgia, Guam, Idaho, Illinois,
Kansas, Louisiana, Maine, Maryland,
Massachusetts, Mississippi, Missouri,
Nebraska, Nevada, New Hampshire,
New Jersey, New Mexico, North Caro-
lina, North Dakota, Ohio, Oklahoma, Or-
egon, Puerto Rico, Rhode Island, South
Carolina, Texas, Utah, Vermont, Wash-
ington, West Virginia, Wisconsin, or Wy-
oming
. , . then you must contact your State
UIC Program to determine what you
must submit and by when,-
, , . then you must contact your State
UIC Program to determine what you
must submit and by when..
Or you're in one of these locations f* Di-
rect Implementation" or D! Programs,
where EPA runs the Class V UIC Pro-
gram); Alaska, American Samoa, Ari-
zona, California, Colorado, Hawaii, Indi-
ana, Iowa, Kentucky, Michigan, Min-
nesota, Montana, New York, Pennsyl-
vania, South Dakota, Tennessee, Vir-
ginia, Virgin Islands, Washington, DC, or
any Indian Country
. . , then you must submit the Inventory
information described in (a)(2) of this
section prior to constructing your well.
. . , then you must cease injection and
submit the inventory information. You
may resume injection 90 days after
you submit the information unless the
UIC Program Director notifies you that
injection may not resume or may re-
sume sooner.
(2) If your well is in a Primacy State
or a DI Program State, here is the in-
formation you must submit:
(i) No matter what type of Class V
well you own or operate, you must sub-
mit at least the following information
for each Class V well: facility name and
location; name and address of legal
contact; ownership of facility; nature
and type of injection well(s); and oper-
ating status of injection well(s).
(ii) Additional information. If you are
in a Direct Implementation State and
you own or operate a well listed below
you must also provide the information
listed in paragraph (a) (2) (iii) as fol-
lows:
(A) Sand or other backfill wells (40
OFE 144,81(8) and 146.5(e)(8) of this
chapter);
(B) Geothermal energy recovery wells
(40 CPR 144.81(11) and 146.5 (e)(12) of
this chapter);
(0) Brine return flow wells (40 CFR
144.81(13) and 146.5 (e)(14) of this chap-
ter);
(D) Wells used in experimental tech-
nology (40 CFR 144.81(14) and 146.5
(e)(15) of this chapter);
(E) Municipal and industrial disposal
wells other than Class I; and
(F) Any other Class V wells at the
discretion of the Regional Adminis-
trator.
(iii) You must provide a list of all
wells owned or operated along with the
following information for each well. (A
single description of wells at a single
facility with substantially the same
characteristics is acceptable).
(A) Location of each well or project
given by Township, Range, Section,
and Quarter-Section, or by latitude and
longitude to the nearest second, ac-
cording to the conventional practice in
your State;
(B) Date of completion of each well;
678
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Environmental Protection Agency
§144.84
(0) Identification and depth of the
underground formation(s) into which
each well is injecting:
(D) Total depth of each well;
(K) Construction narrative and sche-
matic (both plan view and cross-sec-
tional drawings);
(F) Nature of the injected fluids;
(G) Average and maximum injection
pressure at the wellhead;
(H) Average and maximum injection
rate; and
(I) Date of the last inspection.
(3) Regardless of whether your well is
in a Primacy State or DI Program you
are responsible for knowing about, un-
derstanding, and complying with these
inventory requirements.
(b) Information In response to requests.
If you are in one of the DI Programs
listed in the table above, the UIC Pro-
gram Director may require you to sub-
mit other information believed nec-
essary to protect underground sources
of drinking water.
(1) Such information requirements
may include, but are not limited to:
(i) Perform ground water monitoring
and periodically submit your moni-
toring results;
(ii) Analyze the fluids you inject and
periodically submit the results of your
analyses;
(ill) Describe the geologic layers
through which and into which you are
injecting; and
(iv) Conduct other analyses and sub-
mit other information, if needed to
protect underground sources of drink-
ing water.
(2) If the Director requires this other
information, he or she will request it
from you in writing, along with a brief
statement on why the information is
required. This written notification also
will tell you when to submit the infor-
mation.
(3) You are prohibited from using
your injection well if you fail to com-
ply with the written request within the
time frame specified. You can start in-
jecting again only if you receive a per-
mit.
§ 144.84 Do I need to get a permit?
No, unless you fall within an excep-
tion described below:
(a) General authorisation by rule. With
certain exceptions listed in paragraph
(b) of this section, your Class V injec-
tion activity is "authorized by rule,"
meaning you have to comply with all
the requirements of this subpart and
the rest of the UIC Program but you
don't have to get an individual permit.
Well authorization expires once you
have properly closed your well, as de-
scribed in §144.82(b).
(b) Circumstances in Which Permits or
other Actions are Required. If you fit
into one of the categories listed below,
your Class V well is no longer author-
ized by rule. This means that you have
to either get a permit or close your in-
jection well. You can find out by con-
tacting the DIC Program Director in
your State or EPA Region if this is the
case. Subpart D of this Part tells you
how to apply for a permit and describes
other aspects of the permitting proc-
ess. Subpart E of this Part outlines
some of the requirements that apply to
you if you get a permit.
(1) You fail to comply with the prohi-
bition of fluid movement standard in
§144.12(a) and described in §144.82(a) (in
which case, you have to get a permit,
close your well, and/or comply with
other conditions determined by the
UIC Program Director in your State or
EPA Region);
(2) You own or operate a Class V
large-capacity cesspool (in which case,
you must close your well as specified in
the additional requirements below) or a
Class V motor vehicle waste disposal
well in a ground water protection area
or sensitive ground water area (in
which case, you must either close your
well or get a permit as specified in the
additional requirements in this sub-
section). New motor vehicle waste dis-
posal wells and new cesspools are pro-
hibited as of April 5, 2000;
(3) You are specifically required by
the UIC Program Director in your
State or EPA Region to get a permit
(in which case, rule authorization ex-
pires upon the effective date of the per-
mit issued, or you are prohibited from
injecting into your well upon:
(i) Failure to submit a permit appli-
cation in a timely manner as specified
in a notice from the Director; or
(ii) Upon the effective date of permit
denial);
(4) You have failed to submit inven-
tory information to your UIC Program
679
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§144.85
40 CFR Ch. I (7-1-04 Edition)
Director, as described in §144.83(a) (in
which case, you are prohibited from in-
jecting into your well until you comply
with the inventory requirements); or
(5) If you are in a DI State and you
received a request from your UIC Pro-
gram Director for additional informa-
tion under § 144.83(b), and have failed to
comply with the request in a timely
manner (in which case, you are prohib-
ited from injecting into your well until
you get a permit).
ADDITIONAL REQUIREMENTS FOB CLASS
V LARGE-CAPACITY CESSPOOLS AND
MOTOR VEHICLE WASTE DISPOSAL
WELLS
§ 144.85 Do these additional require-
ments apply to me?
(a) Large-Capacity Cesspools. The ad-
ditional requirements apply to all new
and existing large-capacity cesspools
regardless of their location. If you are
using a septic system for these type of
wastes you are not subject to the addi-
tional requirements in this subpart.
(b) Motor Vehicle Waste Disposal Wells
Existing on April 5, 2000. If you have a
Class V motor vehicle waste disposal
well these requirements apply to you if
your well is located in a ground water
protection area or other sensitive
ground water area that is identified by
your State or EPA Region. If your
State or EPA Region fails to identify
ground water protection areas and/or
other sensitive ground water areas
these requirements apply to all Class V
motor vehicle wells in the State.
(c) New Motor Vehicle Waste Disposal
Wells. The additional requirements
apply to all new motor vehicle waste
disposal wells as of April 5, 2000.
§144.86 What are the definitions I
need to know?
(a) State Drinking Water Source Assess-
ment and Protection Program. This is a
new approach to protecting drinking
water sources, specified in the 1996
Amendments to the Safe Drinking
Water Act at Section 1453. States must
prepare and submit for EPA approval a
program that sets out how States will
conduct local assessments, including:
delineating the boundaries of areas
providing source waters for public
water systems; identifying significant
potential sources of contaminants in
such areas; and determining the sus-
ceptibility of public water systems in
the delineated areas to the inventoried
sources of contamination.
(b) Complete Local Source Water Assess-
ment for Ground Water Protection Areas.
When BPA has approved a State's
Drinking Water Source Assessment and
Protection Program, States will begin
to conduct local assessments for each
public water system in their State. For
the purposes of this rule, local assess-
ments for community water systems
and non-transient non-community sys-
tems are complete when four require-
ments are met: First, a State must de-
lineate the boundaries of the assess-
ment area for community and non-
transient non-community water sys-
tems. Second, the State must identify
significant potential sources of con-
tamination in these delineated areas.
Third, the State must "determine the
susceptibility of community and non-
transient non-community water sys-
tems in the delineated area to such
contaminants." Lastly, each State will
develop its own plan for making the
completed assessments available to the
public.
(c) Ground Water Protection Area. A
ground water protection area is a geo-
graphic area near and/or surrounding
community and non-transient non-
community water systems that use
ground water as a source of drinking
water. These areas receive priority for
the protection of drinking water sup-
plies and States are required to delin-
eate and assess these areas under sec-
tion 1453 of the Safe Drinking Water
Act. The additional requirements in
§144.88 apply to you if your Class V
motor vehicle waste disposal well is in
a ground water protection area for ei-
ther a community water system or a
non-transient non-community water
system, in many States, these areas
will be the same as Wellhead Protec-
tion Areas that have been or will be de-
lineated as defined In section 1428 of
the SDWA.
(d) Community Water System. A com-
munity water system is a public water
system that serves at least 15 service
connections used by year-round resi-
dents or regularly serves at least 25
year-round residents.
680
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Environmental Protection Agency
§144.87
(e) Non-transient Non-community Water
System. A public water system that is
not a community water system and
that regularly serves at least 25 of the
same people over six months a year.
These may include systems that pro-
vide water to schools, day care centers,
government/military installations,
manufacturers, hospitals or nursing
homes, office buildings, and other fa-
cilities.
(f) Delineation. Once a State's Drink-
ing Water Source Assessment and Pro-
tection Program is approved, the
States will begin delineating their
local assessment areas. Delineation is
the first step in the assessment process
in which the boundaries of ground
water protection areas are identified.
(g) Other Sensitive Ground Water
Areas. States may also identify other
areas in the State in addition to
ground water protection areas that are
critical to protecting underground
sources of drinking water from con-
tamination. These other sensitive
ground water areas may include areas
such as areas overlying sole-source
aquifers; highly productive aquifers
supplying private wells; continuous
and highly productive aquifers at
points distant from public water supply
\vells: areas where water supply
aquifers are recharged; karst aquifers
that discharge to surface reservoirs
serving as public water supplies; vul-
nerable or sensitive hydrogeologlc set-
tings, such as glacial outwash deposits,
eolian sands, and fractured volcanic
rock; and areas of special concern se-
lected based on a combination of fac-
tors, such as hydrogeologic sensitivity,
depth to ground water, significance as
a drinking water source, and prevailing
land-use practices.
§ 144,87 How does the identification of
ground water protection areas and
other sensitive ground water areas
affect me?
(a) You are subject to these new re-
quirements if you own or operate an
existing motor vehicle well and you are
located in a ground water protection
area or an other sensitive ground water
area. If your State or EPA Region fails
to identify these areas within the spec-
ified time frames these requirements
apply to all existing motor vehicle
waste disposal wells within your State.
(b) Ground Water Protection Areas. (1)
For the purpose of this subpart, States
are required to complete all local
source water assessments for ground
water protection areas by January 1,
2004. Once a local assessment, for a
ground water protection area is com-
plete every existing motor vehicle
waste disposal well owner in that
ground water protection area has one
year to close the well or receive a per-
mit. If a State fails to complete all
local assessments for ground water pro-
tection areas by January 1, 2004, the
following may occur:
(i) The new requirements in this sub-
part will apply to all existing motor
vehicle waste disposal wells in the
State and owners and operators of
motor vehicle waste disposal wells lo-
cated outside of completed assessments
for ground water protection areas must
close their well or receive a permit by
January 1, 2005.
(ii) EPA may grant a State an exten-
sion for up to one year from the Janu-
ary 1, 2004 deadline if the State is mak-
ing reasonable progress in completing
the source water assessments for
ground water protection areas. States
must apply for the extension by June 1,
2003. If a State fails to complete the as-
sessments for the remaining ground
water protection areas by the extended
date the rale requirements will apply
to all motor vehicle waste disposal
wells in the State and owners and oper-
ators of motor vehicle waste disposal
wells located outside of ground water
protection areas with completed as-
sessments must close their well or re-
ceive a permit by January 1, 2006.
(2) The UIC Program Director may
extend the compliance deadline for spe-
cific motor vehicle waste disposal wells
for up to one year if the most efficient
compliance option for the well is con-
nection to a sanitary sewer or installa-
tion of new treatment technology.
(c) Other Sensitive Ground Water
Areas. States may also delineate other
sensitive ground water areas by Janu-
ary 1. 2004. Existing motor vehicle
waste disposal well owners and opera-
tors within other sensitive ground
water areas have until January 1, 2007
to receive a permit or close the well. If
681
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§144.87
40 CFR Ch. I (7-1-04 Edition)
a State or EPA Region fails to identify
these additional sensitive ground water
areas by January 1, 2004, the new re-
quirements of this rule will apply to all
motor vehicle waste disposal wells in
the State effective January 1, 2007 un-
less they are subject to a different
compliance date pursuant to paragraph
(b) of this section. Again, EPA may ex-
tend the January 1, 2004 deadline for up
to one year for States to delineate
other sensitive ground water areas if
the State is making reasonable
progress in identifying the sensitive
areas. States must apply for this exten-
sion by June 1, 2003. If a State has been
granted an extension, existing motor
vehicle waste disposal well owners and
operators within the sensitive ground
water areas have until January 1, 2008
to close the well or receive a permit.
unless they are subject to a different
compliance date pursuant to paragraph
(b) of this section. If a State has been
granted an extension and fails to delin-
eate sensitive areas by the extended
date, the rule requirements will apply
to all motor vehicle waste disposal
wells in the State and owners and oper-
ators have until January 1, 2008 to
close the well or receive a permit, un-
less they are subject to a different
compliance date pursuant to paragraph
(b) of this section.
(d) How to Find Out if Your Well is in
a Ground Water Protection Area or Sen-
sitive Ground Water Area. States are re-
quired to make their local source water
assessments widely available to the
public through a variety of methods
after the assessments are complete.
You can find out if your Class V well is
in a ground water protection area by
contacting the State agency respon-
sible for the State Drinking Water
Source Assessment and Protection Pro-
gram in your area. You may call the
Safe Drinking Water Hotline at 1-800-
426-4791 to find out who to call in your
State for this information. The State
office responsible for implementing- the
Drinking Water Source Assessment and
Protection Program makes the final
and official determination of bound-
aries for ground water protection
areas. Because States that choose to
delineate other sensitive ground water
areas are also required to make the in-
formation on these areas accessible to
the public, they may do so in a manner
similar to the process used by the
States in publicizing the EPA approved
Drinking Water Source Assessment and
Protection Program. You can find out
if your Class V well is in an other sen-
sitive ground water area by contacting
the State or Federal agency respon-
sible for the Underground Injection
Control Program. You may call the
Safe Drinking Water Hotline at 1-800-
426-4791 to find oat who to call for in-
formation.
(e) Changes in the Status of the EPA
Approved State Drinking Water Source
Assessment and Protection Program.
After January 1. 2004 your State may
assess a ground water protection area
for ground water supplying a new com-
munity water system or a new non-
transient non-community water sys-
tem that includes your Class V injec-
tion well. Also, your State may offi-
cially re-delineate the boundaries of a
previously delineated ground water
protection area to include additional
areas that includes your motor vehicle
waste disposal well. This would make
the additional regulations apply to you
if your motor vehicle waste disposal
well is in such an area. The additional
regulations start applying to you one
year after the State completes the
local assessment for the ground water
protection area for the new drinking
water system or the new re-delineated
area. The UIC Program Director re-
sponsible for your area may extend this
deadline for up to one year if the most
efficient compliance option for the well
is connection to a sanitary sewer or in-
stallation of new treatment tech-
nology.
(f) What Happens if My State Doesn't
Designate Other Sensitive Ground Water
Areas? If your State or EPA Region
elects not to delineate the additional
sensitive ground water areas, the addi-
tional regulations apply to you regard-
less of the location of your well by Jan-
uary 1, 2007, or January 2008 if an ex-
tension has been granted as explained
in paragraph (c) of this section, except
for wells in ground water protection
areas which are subject to different
compliance deadlines explained in
paragraph (b) of this section.
(g) [Reserved]
682
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Environmental Protection Agency
§144.88
(h) Application of Requirements Outside
of Ground Water Protection Areas and
Sensitive Ground Water Areas. EPA ex-
pects and strongly encourages States
to use existing authorities in the UIC
program to take whatever measures
are needed to ensure Class V wells are
not endangering USDWs in any other
areas outside of delineated ground
water protection areas and sensitive
ground water areas. Such measures
could include, if believed to be nec-
essary by a UIO Program Director, ap-
plying the additional requirements
below to other areas and/or other types
of Class V wells. Therefore, the Direc-
tor may apply the additional require-
ments to you, even if you are not lo-
cated in the areas listed in paragraph
(a) of this section.
§144.88 What are the additional re-
quirements?
The additional requirements are
specified in the following tables:
(a) TABLE 1—ADDITIONAL REQUIREMENTS FOR LARGE-CAPACITY CESSPOOLS STATEWIDE
|See § 144.85 to determine if these additional requirements appfy to you]
Weil Status
Requirement
If your cesspool is, . .
Then you, . .
(1) Existing (operational or under con-
struction by April 5, 2000).
Deadline
By.. .
(i) Must close the well
(2) New or converted (construction not
started before April 5, 2000).
[ (ii) Must notify the UIC Program Director
{both Primacy States and Direct Im-
plementation States) of your intent to
close the well-
Note: This information is requested on
national form "Preclosure Notification
for Closure of Injection Wells,".
[ April 5, 2005,
At least 30 days prior to closure.
Are prohibited .
.,.,....,,..,... • Aprii 5, 2000,
(b) TABLE 2—ADDITIONAL REQUIREMENTS FOR MOTOR VEHICLE WASTE DISPOSAL WELLS
[See § 144.85 to determine if these additional requirements apply to you]
Weil status
If your motor vehicle waste disposal weii
is
Requirement
Deadline
By...
(1) Existing (operational or under con- ; (!) If your well is in a ground water pro- Within 1 year of the completion of your
struction by Aprii 5- 2000).
tection area, you must close the well
or obtain a permit.
(ii) If your well is m an other sensitive
ground water area, you must close the
well or obtain a permit
(iii) If you plan to seek a waiver from the
ban and apply for a permit* you musl
meet MCLs at the point of injection
wtiile your permit application is under
reyiew, it you choose to keep oper-
ating your well.
local source water assessment; your
UlC Program Director may extend the
closure deadline, but not the permit
application deadline, for up to one
year if the most efficient compliance
option is connection to a sanitary
sewer or instal!ation of new treatment
technology.
By January 1, 2GG7; your UiC Program
Director may extend the closure dead-
line, but not the permit application
deadline, for up to one year if the
most efficient compliance option is
connection 1o a sanitary sewer or in-
stallation of new treatment technology.
The date you submit your permit appli-
cation.
683
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§144.89
40 CFR Ch. I (7-1-04 Edition)
(b) TABLE 2—ADDITIONAL REQUIREMENTS FOR MOTOR VEHICLE WASTE DISPOSAL WELLS—
Continued
[See § 144.85 to determine if these additional requirements apply to you]
If your motor vehicle waste disposal we
(iv) If you receive a permit, you musl ' The date(s) specified in your permit.
comply with alf permit conditions, if
you choose to keep operating your
well, including requirements to meet
MCLs and other health based stand-
ards at the point of injection, follow
best management practices, and mon- j
itor your injeetate and sludge quality.
v) If your well is in a State which has
not completed ail their local assess-
ments by January 1, 2004 or by the
extended date if your State has ob-
tained an extension as described in
144.87, and you are outside an area
with a completed assessment you
must close the well or obtain a permit.
(2) New or converted (construction not Are prohibited ,
started before April 5, 2000).
(vi) If your well is in a State that has not
delineated other sensitive ground
water areas by January 1, 2004 and
you are outside of an area with a
completed assessment you must close
the welt or obtain a permit regardless
of your location.
(vii) If you plan to close your well, you
must notify the UIC Program Director
of your intent to close the well (this in-
cludes closing your well prior to con-
version).
Note: This information is requested on
national form ''Preclosure Notification
for Closure of Injection Weils"..
Ja
anuary 1, 2005 unless your State ob-
tains an extension as described in
144.8? (b) in which case your dead-
line is January 1, 2006; your UIC Pro-
gram Director may extend the closure
deadline, but not the permit applica-
tion deadline, for up to one year if the
most efficient compliance option is
connection to a sanitary sewer or in-
stallation of new treatment technology.
January 1, 2007 unless your State ob-
tains an extension as described in
144.87(c) in which case your deadline
is January 2008.
At least 30 days prior to closure.
April 5, 2000.
[64 PR 68566, Dec. 7. 1999; 64 FB, 70316, Dec. 16, 1999]
§ 144.89 How do I close my Class V in-
jection well?
The following' describes the require-
ments for closing your Class V injec-
tion well.
(a.) Closure. (1) Prior to closing- a
Class V large-capacity cesspool or
motor vehicle waste disposal well, you
muse plug or otherwise close the well
in a manner that complies with the
prohibition of fluid movement standard
in §144.12 and summarized in §144.82(a).
If the UIC Program Director in your
State or EPA Region has any addi-
tional or more specific closure stand-
ards, you have to meet those standards
too. You also must dispose or other-
wise manage any soil, gravel, sludg-e,
liquids, or other materials removed
from or adjacent to your well in ac-
cordance with all applicable Federal,
State, and local regulations and re-
quirements, as in §144.82(0).
(2) Closure does not mean that you
need to cease operations at your facil-
ity, only that you need to close your
well. A number of alternatives are
available for disposing of waste fluids.
Examples of alternatives that may be
available to motor vehicle stations in-
clude: recycling1 and reusing waste-
water as much as possible; collecting
and recycling petroleum-based fluids.
684
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Environmental Protection Agency
§145.1
coolants, and battery acids drained
from vehicles: washing parts In a self-
contained, recirculating solvent sink,
with spent solvents being recovered
and replaced by the supplier: using
absorbents to clean up minor leaks and
spills, and placing the used materials
in approved waste containers and dis-
posing of them properly; using a wet
vacuum or mop to pick up accumulated
rain or snow melt, and if allowed, con-
necting floor drains to a municipal
sewer system or holding tank, and if
allowed, disposing of the holding tank
contents through a publicly owned
treatment works. You should check
with the publicly owned treatment
works you might use to see if they
would accept your wastes. Alternatives
that may be available to owners and
operators of a large-capacity cesspool
include: conversion to a septic system;
connection to sewer; and installation
of an on-site treatment unit.
(b) Conversions. In limited cases, the
UTC Director may authorize the con-
version (reclassification) of a motor ve-
hicle waste disposal well to another
type of Class V well. Motor vehicle
wells may only be converted if: all
motor vehicle fluids are segregated by
physical barriers and are not allowed
to enter the well; and, injection of
motor vehicle waste is unlikely based
on a facility's compliance history and
records showing proper waste disposal.
The use of a semi-permanent plug as
the means to segregate waste is not
sufficient to convert a motor vehicle
waste disposal well to another type of
Class V well.
[64 FR 68566, Deo. 7, 1999; 65 PR 5024, Feb. 2,
2000]
PART 145—STATE UIC PROGRAM
REQUIREMENTS
Subparf A—General Program
Requirements
Sec.
145.1 Purpose and scope.
145.2 Definitions.
Subpart B—Requirements for State
Programs
145.11 Requirements for permitting.
145.12 Requirements for compliance evalua-
tion programs.
145.13 Requirements for enforcement au-
thority.
145.14 Sharing of information.
Subpart C—State Program Submissions
145.21 General requirements for program ap-
provals.
145.22 Elements of a program submission.
145.23 Program description.
145.24 Attorney General's statement.
145.25 Memorandum of Agreement with the
Regional Administrator.
Subpart D—Program Approval, Revision
and Withdrawal
145.31 Approval process.
145.32 Procedures for revision of State pro-
grams,
145.33 Criteria for withdrawal of State pro-
grams.
145.34 Procedures for withdrawal of State
programs.
Subpart E—Indian Tribes
145.52 Requirements for Tribal eligibility.
145.56 Request by an Indian Tribe for a de-
termination of eligibility.
145.58 Procedure for processing' an Indian
Tribe's application.
AUTHORITY: 42 U.S.C. 300f et seg,
SOURCE: 48 FR 14202, Apr. 1, 1983, unless
otherwise noted.
Subpart A—General Program
Requirements
§ 145,1 Purpose and scope.
(a) This part specifies the procedures
EPA will follow in approving, revising,
and withdrawing State programs under
section 1422 (underground injection
control—UIC) of SDWA, and includes
the elements which must be part of
submissions to EPA for program ap-
proval and the substantive provisions
which must be present in State pro-
g-rams for them to be approved.
(b) State submissions for program ap-
proval must be made in accordance
with the procedures set out in subpart
C. This includes developing and sub-
mitting to EPA a program description
(§145.23), an Attorney General's State-
ment (§145.24), and a Memorandum of
Agreement with the Regional Adminis-
trator (§145.25).
(c) The substantive provisions which
must be included in State programs to
obtain approval include requirements
685
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§145.2
40 CFR Ch. I (7-1-04 Edition)
for permitting, compliance evaluation,
enforcement, public participation, and
sharing of information. The require-
ments are found in subpart B. Many of
the requirements for State programs
are made applicable to States by cross-
referencing other EPA regulations. In
particular, many of the provisions of
parts 144 and 124 are made applicable to
States by the references contained in
§145.11.
(d) Upon submission of a complete
program, EPA will conduct a public
hearing, if interest is shown, and deter-
mine whether to approve or disapprove
the program taking into consideration
the requirements of this part, the Safe
Drinking Water Act and any comments
received.
(e) Upon approval of a State program.
the Administrator shall suspend tile
issuance of Federal permits for those
activities subject to the approved State
program.
(f) Any State program approved by
the Administrator shall at all times be
conducted in accordance with the re-
quirements of this part.
(g) Nothing in this part precludes a
State from:
(1) Adopting or enforcing require-
ments which av<3 more stringent or
more extensive than those required
under this part;
(2) Operating a program with a great-
er scope of coverage than that required
under this part. Where an approved
State program has a greater scope of
coverage than required by Federal law
the additional coverage is not part of
the federally approved program,
(h) Section 1451 of the SDWA author-
izes the Administrator to delegate pri-
mary enforcement responsibility for
the Underground Injection Control
Progra.m to eligible Indian Tribes. An
Indian Tribe must establish its eligi-
bility to be treated as a State before it
is eligible to apply for Underground In-
jection Control grants and primary en-
forcement responsibility. All require-
ments of parts 124, 144, 145, and 146 that
apply to States with UIC primary en-
forcement responsibility also apply to
Indian Tribes except where specifically
noted,
[48 PR 14202, Apr. 1. 1983, as amended at 53
PR 37412, Sept. 26. 1988: 59 PK 64345, Deo. 14.
1994]
§ 145.2 Definitions.
The definitions of part 144 apply to
all subparts of this part,
Subpart B—Requirements for State
Programs
§ 145.11 Requirements for permitting.
(a) All State programs under this
part must have legal authority to im-
plement each of the following provi-
sions and must be administered in con-
formance with each; except that States
are not precluded from omitting or
modifying any provisions to impose
more stringent requirements,
(1) Section 144.5(b)—(Confidential in-
formation):
(2) Section 144.6—(Classification of
injection wells);
(3) Section 144,7—(Identification of
underground sources of drinking water
and exempted aquifers);
(4) Section 144.8—(Noncompliance re-
porting);
(5) Section 144.11—(Prohibition of un-
authorized injection);
(6s Section 144.12—(Prohibition of
movement of fluids into underground
sources of drinking water);
(7) Section 144.13—(Elimination of
Class IV wells);
(8) Section 144.14—(Requirements for
wells managing hazardous waste);
(9) Sections 144.21-144.26—(Authoriza-
tion by rule);
(10) Section 144.31—(Application for a
permit);
(11) Section 144.32—(Signatories):
(12) Section 144.33—(Area Permits);
(13) Section 144.34—(Emergency per-
mits);
(14) Section 144.35—(Effect of permit);
(15) Section 144.36—(Duration);
(16) Section 144.38—(Permit transfer);
(17) Section 144.39—(Permit modifica-
tion):
(18) Section 144.40—(Permit termi-
nation);
(19) Section 144.51—(Applicable per-
mit conditions);
(20) Section 144.52—(Establishing per-
mit conditions);
(21) Section 144.53(a)—(Schedule of
compliance):
(22) Section 144,54—(Monitoring re-
quirements);
(23) Section 144.55—(Corrective Ac-
tion);
686
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Environmental Protection Agency
§145.12
(24) Section 124.3(a)—(Application for
a permit);
(25) Section 124.5 (a), (c), (d), and (f)—
(Modification of permits);
(26) Section 124.6 (a), (c), (d), and (e)—
(Draft Permit);
(27) Section 124.8—(Pact sheets);
(28) Section 124.10 (a)(l)(ii), (a)(l)(iii),
(a)(l)(v), (b), (c), (d), and (e)—(Public
notice);
(29) Section 124.11—(Public comments
and requests for hearings);
(30) Section 124,12(a)—(Public hear-
ings); and
(31) Section 124.17 (a) and (c)—(Re-
sponse to comments).
(32) Section 144.88—(What are the ad-
ditional requirements?);
(b)(l) States need not implement pro-
visions identical to the provisions list-
ed in paragraphs (a)(l) through (a)(32)
of this section. Implemented provisions
must, however, establish requirements
at least as stringent as the cor-
responding listed provisions. While
States may impose more stringent re-
quirements, they may not make one re-
quirement more lenient as a tradeoff
for making another requirement more
stringent; for example, by requiring
that public hearings be held prior to
issuing any permit while reducing the
amount of advance notice of such a
hearing.
(2) State programs may, if they have
adequate legal authority, implement
any of the provisions of parts 144 and
124. See, for example §144.37(d) (con-
tinuation of permits) and §124.4 (con-
solidation of permit processing).
[48 FR 14202, Apr. 1, 1983. as amended at 64
FR 78572, Dec. 7. 1999]
§145.12 Beqtiirements for compliance
evaluation programs.
(a) State programs shall have proce-
dures for receipt, evaluation, retention
and investigation for possible enforce-
ment of all notices and reports re-
quired of permittees and other regu-
lated persons (and for investigation for
possible enforcement of failure to sub-
mit these notices and reports).
(b) State programs shall have inspec-
tion and surveillance procedures to de-
termine, independent of information
supplied by regulated persons, compli-
ance or noncompliance with applicable
program requirements. The State shall
maintain:
(1) A program which is capable of
making comprehensive surveys of all
facilities and activities subject to the
State Director's authority to identify
persons subject to regulation who have
failed to comply with permit applica-
tion or other program requirements.
Any compilation, index, or inventory
of such facilities and activities shall be
made available to the Regional Admin-
istrator upon request;
(2) A program for periodic inspections
of the facilities and activities subject
to regulation. These inspections shall
be conducted in a manner designed to:
(i) Determine compliance or non-
compliance with issued permit condi-
tions and other program requirements;
(ii) Verifjr the accuracy of informa-
tion submitted by permittees and other
regulated persons in reporting forms
and other forms supplying monitoring
data; and
(iii) Verify the adequacy of sampling,
monitoring, and other methods used by
permittees and other regulated persons
to develop that information;
(3) A program for investigating infor-
mation obtained regarding violations
of applicable program and permit re-
quirements; and
(4) Procedures for receiving and en-
suring proper consideration of informa-
tion submitted by the public about vio-
lations. Public effort in reporting vio-
lations shall be encouraged and the
State Director shall make available in-
formation on reporting procedures.
(c) The State Director and State offi-
cers engaged in compliance evaluation
shall have authority to enter any site
or premises subject to regulation or in
which records relevant to program op-
eration are kept in order to copy any
records, inspect, monitor or otherwise
investigate compliance with permit
conditions and other program require-
ments. States whose law requires a
search warrant before entry conform
with this requirement.
(d) Investigatory inspections shall be
conducted, samples shall be taken and
other information shall be gathered in
a manner [e.g., using proper "chain of
custody" procedures] that will produce
evidence admissible in an enforcement
proceeding or in court.
687
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§145.13
40 CFR Ch. I (7-1-04 Edition)
§ 145.13 Requirements for enforcement
authority.
(a) Any State agency administering a
program shall have available the fol-
lowing remedies for violations of State
program requirements:
(1) To restrain immediately and ef-
fectively any person by order or by suit
in State court from engaging in any
unauthorized activity which is endan-
gering or causing damage to public
health or environment;
NOTE: This paragraph requires that States
have a mechanism (e.g., an administrative
cease and desist order or the ability to seek
a temporary restraining order) to stop any
unauthorized activity endangering public
health or the environment.
(2) To sue in courts of competent ju-
risdiction to enjoin any threatened or
continuing violation of any program
requirement, including permit condi-
tions, without the necessity of a prior
revocation of the permit;
(3) To assess or sue to recover in
court civil penalties and to seek crimi-
nal remedies, including fines, as fol-
lows:
(i) For all wells except Class II wells,
civil penalties shall be recoverable for
any program violation In at least the
amount of $2,500 per day. For Class II
wells, civil penalties shall be recover-
able for any program violation in at
least the amount of $1,000 per day,
(ii) Criminal fines shall be recover-
able in at least the amount of $5,000 per
day against any person who willfully
violates any program requirement, or
for Class II wells, pipeline (production)
severance shall be imposable against
any person who willfully violates any
program requirement.
NOTE: In many States the State Director
will be represented in State courts by the
State Attorney General or other appropriate
legal officer. Although the State Director
need not appear in court actions he or she
should have power to request that any of the
above actions be brought.
(b)Cl) The maximum civil penalty or
criminal fine (as provided in paragraph
(a)(3) of this section) shall "be assess-
able for each instance of violation and,
if the violation is continuous, shall be
assessable up to the maximum amount
for each day of violation.
(2) The burden of proof and degree of
knowledge or intent required under
State law for establishing violations
under paragraph (a)<3) of this section,
shall be no greater than the burden of
proof or degree of knowledge or intent
EPA must provide when it brings an
action under the Safe Drinking Water
Act.
NOTE: For example, this requirement is not
met if State law includes mental state as an
element of proof for civil violations.
(c) A civil penalty assessed, sought,
or agreed upon by the State Director
under paragraph (a)(3) of this section
shall be appropriate to the violation.
NOTE: To the extent that State judgments
or settlements provide penalties in amounts
which EPA believes to be substantially inad-
equate in comparison to the amounts which
EPA would require under similar facts, EPA,
when authorized by the applicable statute,
may commence separate actions for pen-
alties.
In addition to the requirements of this
paragraph, the State may have other en-
forcement remedies. The following enforce-
ment options, while not mandatory, are
highly recommended:
Procedures for assessment by the State of
the costs of investigations, inspections, or
monitoring surveys which lead to the estab-
lishment of violations:
Procedures which enable the State to as-
sess or to sue any persons responsible for un-
authorized activities for any expenses in-
curred by the State in removing, correcting,
or terminating any adverse effects upon
human health and the environment resulting
from the unauthorized activity, or both; and
Procedures for the administrative assess-
ment of penalties by the Director.
(d) Any State administering a pro-
gram shall provide for public participa-
tion in the State enforcement process
by providing either:
(1) Authority which allows interven-
tion as of right in any civil or adminis-
trative action to obtain remedies speci-
fied in paragraph (a) (1), (2) or (3) of
this section by any citizen having an
interest which is or may be adversely
affected; or
(2) Assurance that the State agency
or enforcement authority will:
(i) Investigate and provide written
responses to all citizen complaints sub-
mitted pursuant to the procedures
specified in §145.12(b)(4);
(ii) Not oppose intervention by any
citizen when permissive intervention
may be authorized by statute, rule, or
regulation; and
688
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Environmental Protection Agency
§145.21
(ill) Publish notice of and provide at
least 30 days for public comment on
any proposed settlement of a State en-
forcement action.
(e) To the extent that an Indian
Tribe does not assert or is precluded
from asserting criminal enforcement
authority the Administrator will as-
sume primary enforcement responsi-
bility for criminal violations. The
Memorandum of Agreement in §145.25
shall reflect a system where the Tribal
agency will refer such violations to the
Administrator in an appropriate and
timely manner.
(Clean Water Act (33 U.S.C. 1251 et seq.), Safe
Drinking- Water Act (42 U.S.C. 300f et seq,),
Clean Air Act (42 U.S.C. 7401 et seq.). Re-
source Conservation and Recovery Act (42
U.S.C. 6901 et seq,))
[48 FR 14202, Apr. 1, 1983. as amended at 48
PR 39621, Sept, 1, 1983: 53 FR 37412, Sept. 26,
1988]
§145.14 Sharing of information.
(a) Any information obtained or used
in the administration of a State pro-
gram shall be available to EPA upon
request without restriction. If the in-
formation has been submitted to the
State under a claim of confidentiality,
the State must submit that claim to
EPA when providing information under
this section. Any information obtained
from a State and subject to a claim of
confidentiality will be treated in ac-
cordance with the regulations in 40
CFR part 2. If EPA obtains from a
State information that is not claimed
to be confidential, EPA may make that
information available to the public
without further notice.
(b) EPA shall furnish to States with
approved programs the information in
its files not submitted under a claim of
confidentiality which the State needs
to implement its approved program.
EPA shall furnish to States with ap-
proved programs information sub-
mitted to EPA under a claim of con-
fidentiality, which the State needs to
implement its approved program, sub-
ject to the conditions in 40 CPB part 2.
Subpart C—State Program
Submissions
§ 145.21 General requirements for pro-
gram approvals.
(a) States shall submit to the Admin-
istrator a proposed State UIC program
complying with §145.22 of this part
within 270 days of the date of promul-
gation of the TJIC regulations on June
24, 1980. The administrator may, for
good cause, extend the date for submis-
sion of a proposed State UIC program
for up to an additional 270 days.
(b) States shall submit to the Admin-
istrator 6 months after the date of pro-
mulgation of the UIC regulations a re-
port describing the State's progress in
developing a UIC program. If the Ad-
ministrator extends the time for sub-
mission of a UIC program an additional
270 days, pursuant to §145.21(a), the
State shall submit a second report six
months after the first report is due.
The Administrator may prescribe the
manner and form of the report.
(c) The requirements of §145.21 (a)
and (b) shall not apply to Indian
Tribes.
(d) EPA will establish a UIC program
in any State which does not comply
with paragraph (a) of this section. EPA
will continue to operate a UIC program
in such a State until the State receives
approval of a UIC program in accord-
ance with the requirements of this
part.
NOTE: States wliieh are authorized to ad-
minister the NPDBS permit program under
section 402 of CWA are encouraged to rely on
existing statutory authority, to the extent
possible, in developing- a State UIC program.
Section 402(b)UXD) of CWA requires that
NPDES States have the authority "to issue
permits which control the disposal of pollut-
ants into wells." In many instances, there-
fore, NPDES States will have existing statu-
tory authority to regulate well disposal
which satisfies the requirements of the UIC
program. Note, however, that CWA excludes
certain types of well injections from the def-
inition of "pollutant." If the State's statu-
tory authority contains a similar exclusion
it may need to be modified to qualify for UIC
program approval.
(e) If a State can demonstrate to
EPA's satisfaction that there are no
underground injections within the
State for one or more classes of injec-
tion wells (other than Class IV wells)
689
-------
§145.22
40 CFR Ch. I (7-1-04 Edition)
subject to SDWA and that such injec-
tions cannot legally occur in the State
until the State has developed an ap-
proved program for those classes of in-
jections, the State need not submit a
program to regulate those injections
and a partial program may be ap-
proved. The demonstration of legal pro-
hibition shall be made by either explic-
itly banning new injections of the class
not covered by the State program or
providing a certification from the
State Attorney General that such new
injections cannot legally occur until
the State has developed an approved
program for that class. The State shall
submit a program to regulate both
those classes of injections for which a
demonstration is not made and class IV
wells.
(f) When a State UIC program is fully
approved by EPA to regulate all classes
of Injections, the State assumes pri-
mary enforcement authority under sec-
tion 1422(b)(3) of SDWA. EPA retains
primary enforcement responsibility
whenever the State program is dis-
approved in whole or in part. States
which have partially approved pro-
grams have authority to enforce any
violation of the approved portion of
their program. EPA retains authority
to enforce violations of State under-
ground injection control programs, ex-
cept that, when a State has a fully ap-
proved program, EPA will not take en-
forcement actions without providing
prior notice to the State and otherwise
complying with section 1423 of SDWA.
(g) A State can assume primary en-
forcement responsibility for the UIC
program, notwithstanding §145.21(3),
when the State program is unable to
regulate activities on Indian lands
within the State. EPA will administer
the program on Indian lands if the
State does not seek this authority.
[48 PR 14202. Apr. 1, 1983. as amended at 53
FR 37412, Sept. 26, 1988]
§145.22 Elements of a program sub-
mission.
(a) Any State that seeks to admin-
ister a program under this part shall
submit to the Administrator at least
three copies of a program submission.
The submission shall contain the fol-
lowing:
(1) A letter from the Governor of the
State requesting program approval;
(2) A complete program description,
as required by §145,23, describing how
the State intends to carry out its re-
sponsibilities under this part;
(3) An Attorney General's statement
as required by § 145.24;
(4) A Memorandum of Agreement
with the Regional Administrator as re-
quired by §145.25;
(5) Copies of all applicable State stat-
utes and regulations, including those
governing State administrative proce-
dures;
(6) The showing required by §145.31(b)
of the State's public participation ac-
tivities prior to program submission.
(b) Within 30 days of receipt by EPA
of a State program submission, EPA
will notify the State whether its sub-
mission is complete. If EPA finds that
a State's submission is complete, the
statutory review period (i.e., the period
of time allotted for formal EPA review
of a proposed State program under the
Safe Drinking Water Act) shall be
deemed to have begun on the date of
receipt of the State's submission. If
EPA finds that a State's submission is
incomplete, the statutory review pe-
riod shall not begin until all the nec-
essary information is received by EPA.
(c) If the State's submission is mate-
rially changed during'.the statutory re-
view period, the statutory review pe-
riod shall begin again upon receipt of
the revised submission.
(d) The State and EPA may extend
the statutory review period by agree-
ment.
§ 145.23 Program description.
Any State that seeks to administer a
program under this part shall submit a
description of the program it proposes
to administer in lieu of the Federal
program under State law or under an
interstate compact. The program de-
scription shall include:
(a) A description in narrative form of
the scope, structure, coverage and
processes of the State program.
(b) A description (including organiza-
tion charts) of the organization and
structure of the State agency or agen-
cies which will have responsibility for
administering- the program, including
the information listed below. If more
690
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Environmental Protection Agency
§ 145.23
than one agency is responsible for ad-
ministration of a program, each agency
must have statewide jurisdiction over a
class of activities. The responsibilities
of each agency must be delineated,
their procedures for coordination set
forth, and an agency may be designated
as a "lead agency" to facilitate commu-
nications between EPA and the State
agencies having program responsi-
bility. When the State proposes to ad-
minister a program of greater scope of
coverage than is required by Federal
law, the information provided under
this paragraph shall indicate the re-
sources dedicated to administering the
Federally required portion of the pro-
gram.
(1) A description of the State agency
staff who will carry out the State pro-
gram, including the number, occupa-
tions, and general duties of the em-
ployees. The State need not submit
complete job descriptions for every em-
ployee carrying out the State program,
(2) An itemization of the estimated
costs of establishing and administering
the program for the first two years
after approval, including cost of the
personnel listed in paragraph (b)(l) of
this section, cost of administrative
support, and cost of technical support.
(3) An itemization of the sources and
amounts of funding, including an esti-
mate of Federal grant money, available
to the State Director for the first two
years after approval to meet the costs
listed in paragraph (b)(2) of this sec-
tion, identifying any restrictions or
limitations upon this funding.
(c) A description of applicable State
procedures, including permitting pro-
cedures and any State administrative
or judicial review procedures.
(d) Copies of the permit forni(s), ap-
plication form(s), reporting form(s),
and manifest format the State intends
to employ in its program. Forms used
by States need not be identical to the
forms used by EPA but should require
the same basic information. The State
need not provide copies of uniform na-
tional forms it intends to use but
should note its intention to use such
forms.
NOTE: States are encouraged to use uni-
form national forms established by the Ad-
ministrator. If uniform national forms are
used, they may be modified to include the
State Agency's name, address, logo, and
other similar information, as appropriate, in
place of EPA's.
(e) A complete description of the
State's compliance tracking and en-
forcement program.
(f) A State UIC program description
shall also include:
(1) A schedule for issuing permits
within five years after program ap-
proval to all injection wells within the
State which are required to have per-
mits under this part and part 144;
(2) The priorities (according to cri-
teria set forth in 40 CFR 146.09) for
issuing permits, including the number
of permits in each class of injection
well which will be Issued each year
during the first five years of program
operation;
(3) A description of how the Director
will implement the mechanical integ-
rity testing requirements of 40 CFR
146.08, including the frequency of test-
ing that will be required and the num-
ber of tests that will be reviewed by
the Director each year;
(4) A description of the procedure
whereby the Director will notify own-
ers and operators of injection wells of
the requirement that they apply for
and obtain a permit. The notification
required by this paragraph shall re-
quire applications to be filed as soon as
possible, but not later than four years
after program approval for all injection
wells requiring a permit;
(5) A description of any rule under
which the Director proposes to author-
ize injections, including the text of the
rule;
(6) For any existing enhanced recov-
ery and hydrocarbon storage wells
which the Director proposes to author-
ize by rule, a description of the proce-
dure for reviewing the wells for compli-
ance with applicable monitoring, re-
porting, construction, and financial re-
sponsibility requirements of §§144.51
and 144.52, and 40 CFR part 146;
(7) A description of and schedule for
the State's program to establish and
maintain a current inventory of Injec-
tion wells which must be permitted
under State law;
(8) Where the Director had designated
underground sources of drinking water
691
-------
§145.24
40 CFR Ch. I (7-1-04 Edition)
in accordance with §144.7(a), a.descrip-
tion and identification of all such des-
ignated sources in the State;
(9) A description of aquifers, or parts
thereof, which the Director has identi-
fied under §144.7(b) as exempted
aquifers, and a summary of supporting
data;
(10) A description of and schedule for
the State's program to ban Class IV
wells prohibited under §144.13; and
(11) A description of and schedule for
the State's program to establish an in-
ventory of Class V wells and to assess
the need for a program to regulate
Class V wells.
(12) For Class V programs only, A de-
scription of and a schedule for the
State's plan to identify and delineate
other sensitive ground water areas.
States should consider geologic and
hydrogeologlc settings, ground water
flow and occurrence, topographic and
geographic features, depth to ground
water, significance as a drinking water
source, prevailing land use practices
and any other existing information re-
lating to the susceptibility of ground
water to contamination from Class V
injection wells when developing their
plan. Within the schedule for the plan,
States must commit to: completing all
delineations of other sensitive ground
water areas by no later than Jan. 1,
2004; making these delineation avail-
able to the public; implementing the
Class V regulations, effective April 5,
2000, in these delineated areas by no
later than January 1, 2007. Alternately,
if a State chooses not to identify other
sensitive ground water areas, the re-
quirements for motor vehicle waste
disposal wells would apply statewide by
January 1. 2007,
[48 PR 14202, Apr. 1, 1983, as amended at 64
PR 68572. Dec. 7, 1999]
§ 145.24 Attorney General's statement.
(a) Any State that seeks to admin-
ister a program under this part shall
submit a statement from the State At-
torney General (or the attorney for
those State or interstate agencies
which have independent legal counsel)
that the laws of the State, or an inter-
state compact, provide adequate au-
thority to carry out the program de-
scribed under §145.23 and to meet the
requirements of this part. This state-
ment shall include citations to the spe-
cific statutes, administrative regula-
tions, and, where appropriate, judicial
decisions which demonstrate adequate
authority. State statutes and regula-
tions cited by the State Attorney Gen-
eral or independent legal counsel shall
be in the form of lawfully adopted
State statutes and regulations at the
time the statement is signed and shall
be fully effective by the time the pro-
gram is approved. To qualify as "inde-
pendent legal counsel" the attorney
signing the statement required by this
section must have full authority to
independently represent the State
agency in court on all matters per-
taining to the State program,
NOTE: EPA will supply States with an
Attorney General's statement format on
request.
(b) When a State seeks authority
over activities on Indian lands, the
statement shall contain an appropriate
analysis of the State's authority.
§ 14S.25 Memorandum of Agreement
with the Regional Administrator,
(a) Any State that seeks to admin-
ister a program under this part shall
submit a Memorandum of Agreement.
The Memorandum of Agreement shall
be executed by the State Director and
the Regional Administrator and shall
become effective when approved by the
Administrator. In addition to meeting
the requirements of paragraph (b) of
this section, the Memorandum of
Agreement may include other terms,
conditions, or agreements consistent
with this part and relevant to the ad-
ministration and enforcement of the
State's regulatory program. The Ad-
ministrator shall not approve any
Memorandum of Agreement which con-
tains provisions which restrict BPA's
statutory oversight responsibility.
(b) The Memorandum of Agreement
shall include the following:
(1) Provisions for the prompt transfer
from EPA to the State of pending per-
mit applications and any other infor-
mation relevant to program operation
not already in the possession of the
State Director (e.g., support files for
permit issuance, compliance reports,
692
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Environmental Protection Agency
§145.31
etc.). When existing permits are trans-
ferred from EPA to State for adminis-
tration, the Memorandum of Agree-
ment shall contain provisions speci-
fying a procedure for transferring the
administration of these permits. If a
State lacks the authority to directly
administer permits issued by the Fed-
eral government, a procedure may be
established to transfer responsibility
for these permits,
NOTE: For example, EPA and the State and,
the permittee could agree that the State
would Issue a permit(s) identical to the out-
standing Federal permit which would simul-
taneously be terminated.
(2) Provisions specifying classes and
categories of permit applications, draft
permits, and proposed permits that the
State will send to the Regional Admin-
istrator for review, comment and,
where applicable, objection.
(3) Provisions specifying the fre-
quency and content of reports, docu-
ments and other information which the
State is required to submit to EPA.
The State shall allow EPA to routinely
review State records, reports, and files
relevant to the administration and en-
forcement of the approved program.
State reports may be combined with
grant reports where appropriate.
(4) Provisions on the State's compli-
ance monitoring and enforcement pro-
gram, including:
(i) Provisions for coordination of
compliance monitoring activities by
the State and by EPA. These may
specify the basis on which the Regional
Administrator will select facilities or
activities within the State for EPA In-
spection. The Regional Administrator
will normally notify the State at least
7 days before any such inspection; and
(ii) Procedures to assure coordination
of enforcement activities.
(5) When appropriate, provisions for
joint processing of permits by the
State and EPA, for facilities or activi-
ties which require permits from both
EPA and the State under different pro-
grams. See §124.4.
(6) Provisions for modification of the
Memorandum of Agreement in accord-
ance with this part.
(o) The Memorandum of Agreement,
the annual program and grant and the
State/EPA Agreement should be con-
sistent. If the State/EPA Agreement
indicates that a change is needed in the
Memorandum of Agreement, the
Memorandum of Agreement may be
amended through the procedures set
forth in this part. The State/EPA
Agreement may not override the
Memorandum of Agreement.
NOTE: Detailed program priorities and spe-
cific arrangements for EPA support of the
State program will change and are therefore
more appropriately negotiated in the con-
text of annual agreements rather than in the
MOA. However, it may still be appropriate to
specify in the MOA the basis for such de-
tailed agreements, e.g., a provision in the
MOA specifying that EPA will select facili-
ties in the State for inspection annually as
part of the State/EPA agreement.
Subpart p—Program Approval,
Revision ana Withdrawal
§ 145.31 Approval process.
(a) Prior to submitting an applica-
tion to the Administrator for approval
of a State UIC program, the State shall
issue public notice of its intent to
adopt a UIC program and to seek pro-
gram approval from EPA. This public
notice shall:
(1) Be circulated in a manner cal-
culated to attract the attention of in-
terested persons. Circulation of the
public notice shall include publication
in enough of the largest newspapers in
the State to attract Statewide atten-
tion and mailing to persons on appro-
priate State mailing lists and to any
other persons whom the agency has
reason to believe are Interested;
(2) Indicate when and where the
State's proposed program submission
may be reviewed by the public;
(3) Indicate the cost of obtaining a
copy of the submission;
(4) Provide for a comment period of
not less than 30 days during which in-
terested persons may comment on the
proposed UIC program;
(5) Schedule a public hearing on the
State program for no less than 30 days
after notice of the hearing is published;
(6) Briefly outline the fundamental
aspects of the State UIC program; and
(7) Identify a person that an inter-
ested member of the public may con-
tact for further information.
(b) After complying with the require-
ments of paragraph (a) of this section
any State may submit a proposed UIC
693
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§145.32
40 CFR Ch. I (7-1-04 Edition)
program under section 1422 of SDWA
and §145,22 of this part to EPA for ap-
proval. Such a submission shall include
a showing of compliance with para-
graph (a) of this section; copies of all
written comments received by the
State; a transcript, recording or sum-
mary of any public hearing which was
held by the State: and a responsiveness
summary which identifies the public
participation activities conducted, de-
scribes the matters presented to the
public, summarizes significant com-
ments received, and responds to these
comments. A copy of the responsive-
ness summary shall be sent to those
who testified at the hearing, and others
upon request.
(c) After determining that a State's
submission for UIC program approval is
complete the Administrator shall issue
public notice of the submission in the
FEDERAL REGISTER and in accordance
with paragraph fa){l) of this section.
Such notice shall:
(1) Indicate that a public hearing will
be held by EPA no earlier than 30 days
after notice of the hearing. The notice
may require persons wishing to present
testimony to file a request with the
Regional Administrator, who may can-
cel the public hearing if sufficient pub-
lic interest in a hearing is not ex-
pressed;
(2) Afford the public 30 days after the
notice to comment on the State's sub-
mission; and
(3) Note the availability of the State
submission for inspection and copying
by the public.
(d) The Administrator shall approve
State programs which conform to the
applicable requirements of this part,
(e) Within 90 days of the receipt of a
complete submission (as provided in
§145.22) or material amendment there-
to, the Administrator shall by rule ei-
ther fully approve, disapprove, or ap-
prove in part the State's UIC program
taking into account any comments
submitted. The Administrator shall
give notice of this rule in the FEDERAL
REGISTER and in accordance with para-
graph (a)(l) of this section. If the Ad-
ministrator determines not to approve
the State program or to approve it
only in part, the notice shall include a
concise statement of the reasons for
this determination. A responsiveness
summary shall be prepared by the Re-
gional Office which identifies the pub-
lic participation activities conducted,
describes the matters presented to the
public, summarizes significant com-
ments received, and explains the Agen-
cy's response to these comments. The
responsiveness summary shall be sent
to those who testified at the public
hearing, and to others upon request,
§ 145.32 Procedures for revision of
State programs.
(a) Either EPA or the approved State
may initiate program revision. Pro-
gram revision may be necessary when
the controlling Federal or State statu-
tory or regulatory authority is modi-
fied or supplemented. The state shall
keep EPA fully informed of any pro-
posed modifications to its basic statu-
tory or regulatory authority, its forms.
procedures, or priorities.
(b) Revision of a State program shall
be accomplished as follows:
(1) The State shall submit a modified
program description. Attorney Gen-
eral's statement, Memorandum of
Agreement, or such other documents as
EPA determines to be necessary under
the circumstances.
(2) Whenever EPA determines that
the proposed program revision is sub-
stantial, EPA shall issue public notice
and provide an opportunity to com-
ment for a period of at least 30 days.
The public notice shall be mailed to in-
terested persons and shall be published
in the FEDERAL REGISTER and in
enough of the largest newspapers in the
State to provide Statewide coverage.
The public notice shall summarize the
proposed revisions and provide for the
opportunity to request a public hear-
ing. Such a hearing" will be held is
there if significant public interest
based on requests received.
(3) The Administrator shall approve
or disapprove program revisions based
on the requirements of this part and of
the Safe Drinking Water Act.
(4) A program revision shall become
effective upon the approval of the Ad-
ministrator. Notice of approval of any
substantial revision shall be published
in the FEDERAL REGISTER. Notice of ap-
proval of non-substantial program revi-
sions may be given by a letter from the
694
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Environmental Protection Agency
§145.34
Administrator to the State Governor
or his designee.
(c) States with approved programs
shall notify BPA whenever they pro-
pose to transfer all or part of any pro-
gram from the approved State agency
to any other State agency, and shall
identify any new division of respon-
sibilities among" the agencies involved.
The new agency is not authorized to
administer the program until approval
by the Administrator under paragraph
(b) of this section. Organizational
charts required under §145,23(b) shall
be revised and resubmitted.
(d) Whenever the Administrator has
reason to believe that circumstances
have changed with respect to a State
program, he may request, and the
State shall provide, a supplemental At-
torney General's statement, program
description, or such other documents
or information as are necessary.
(e) The State shall submit the infor-
mation required under paragraph (b)(l)
of this section within 270 days of any
amendment to this part or 40 CFB part
144. 146, or 124 which revises or adds
any requirement respecting an ap-
proved UIC program.
§145,33 Criteria for withdrawal of
State programs.
(a) The Administrator may withdraw
program approval when a State pro-
gram no longer complies with the re-
quirements of this part, and the State
fails to take corrective action. Such
circumstances include the following:
(1) When the State's legal authority
no longer meets their requirements of
this part, including:
(i) Failure of the State to promulgate
or enact new authorities when nec-
essary; or
(ii) Action by a State legislature or
court striking down or limiting State
authorities.
(2) When the operation of the State
program fails to comply with the re-
quirements of this part, including:
(i) Failure to exercise control over
activities required to be regulated
under this part, including failure to
issue permits;
(ii) Repeated issuance of permits
which do not conform to the require-
ments of this part; or
(iii) Failure to comply with the pub-
lic participation requirements of this
part.
(3) When the State's enforcement
program fails to comply with the re-
quirements of this part, including:
(i) Failure to act on violations of per-
mits or other program requirements;
(ii) Failure to seek adequate enforce-
ment penalties or to collect adminis-
trative fines when imposed: or
(iii) Failure to inspect and monitor
activities subject DO regulation.
(4) When the State program fails to
comply with the terms of the Memo-
randum of Agreement required under
§145.24.
§ 146.34 Procedures for withdrawal of
State programs.
(a) A State with a program approved
under this part may voluntarily trans-
fer program responsibilities required
by Federal law to EPA by taking the
following actions, or in such other
manner as may be agreed upon with
the Administrator.
(1) The State shall give the Adminis-
trator 180 days notice of the proposed
transfer and shall submit a plan for the
orderly transfer of all relevant pro-
gram information not in the possession
of EPA (such as permits, permit files,
compliance files, reports, permit appli-
cations) which are necessary for EPA
to administer the program.
(2) Within 60 days of receiving the no-
tice and transfer plan, the Adminis-
trator shall evaluate the State's trans-
fer plan and shall identify any addi-
tional information needed by the Fed-
eral government for program adminis-
tration and/or identify any other defi-
ciencies in the plan.
(3) At least 30 days before the trans-
fer is to occur the Administrator shall
publish notice of the transfer in the
FEDERAL REGISTER and in enough of
the largest, newspapers in the State to
provide Statewide coverage, and shall
mail notice to all permit holders, per-
mit applicants, other regulated persons
and other interested persons on appro-
priate EPA and State mailing lists,
(b) Approval of a State UIC program
may be withdrawn and a Federal pro-
gram established in its place when the
Administrator determines, after hold-
ing a public, hearing, that the State
695
203-160 D-23
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§145.52
program is not in compliance with the
requirements of SDWA and this part,
(1) Notice to State of public hearing. If
the Administrator has cause to believe
that a State is not administering' or en-
forcing its authorized program in com-
pliance with the requirements of
SDWA and this part, he or she shall in-
form the State by registered mail of
the specific areas of alleged noncompli-
ance. If the State demonstrates to the
Administrator within 30 days of such
notification that the State program is
in compliance, the Administrator shall
take no further action toward with-
drawal and shall so notify the State by
registered mail.
(2) Public hearing. If the State has not
demonstrated its compliance to the
satisfaction of the Administrator with-
in 30 days after notification, the Ad-
ministrator shall inform the State Di-
rector and schedule a public hearing to
discuss withdrawal of the State pro-
gram. Notice of such public hearing
shall be published in the FEDERAL REG-
ISTER and in enough of the largest
newspapers in the State to attract
statewide attention, and mailed to per-
sons on appropriate State and EPA
mailing lists. This hearing shall be
convened not less than 60 days nor
more than 75 days following the publi-
cation of the notice of the hearing. No-
tice of the hearing shall identify the
Administrator's concerns. All inter-
ested persons shall be given oppor-
tunity to make written or oral presen-
tation on the State's program at the
public hearing.
(3) Notice to State of findings. When
the Administrator finds after the pub-
lic hearing that the State is not in
compliance, he or she shall notify the
State by registered mail of the specific
deficiencies in the State program and
of necessary remedial actions. Within
90 days of receipt of the above letter,
the State shall either carry out the re-
quired remedial action or the Adminis-
trator shall withdraw program ap-
proval. If the State carries out the re-
medial action or, as a result of the
hearing is found to be in compliance,
the Administrator shall so notify the
State by registered mail and conclude
the withdrawal proceedings.
40 CFR Ch, I (7-1-04 Edition)
Subpart E—Indian Tribes
SOURCE: 53 FR 37412, Sept. 26, 1988, unless
otherwise noted.
§ 145.52 Requirements for Tribal eligi-
bility.
The Administrator is authorized to
treat an Indian Tribe as eligible to
apply for primary enforcement respon-
sibility for the Underground Injection
Control Program if it meets the fol-
lowing criteria:
(a) The Indian Tribe is recognized by
the Secretary of the Interior.
(b) The Indian Tribe has a Tribal gov-
erning body which is currently "car-
rying out substantial governmental du-
ties and powers" over a defined area,
(i.e., is currently performing govern-
mental functions to promote the
health, safety, and welfare of the af-
fected population within a defined geo-
graphic area).
(c) The Indian Tribe demonstrates
that the functions to be performed in
regulating the underground injection
wells that the applicant intends to reg-
ulate are within the area of the Indian
Tribal government's jurisdiction.
(d) The Indian Tribe is reasonably ex-
pected to be capable, in the Adminis-
trator's judgment, of administering (in
a manner consistent with the terms
and purposes of the Act and all applica-
ble regulations) an effective Under-
ground Injection Control Program.
[53 FR 37412, Sept. 26, 1988, as amended at 59
PE 64345, Dec. 14, 1994]
§ 145.56 Request by an Indian Tribe
for a determination of eligibility.
An Indian Tribe may apply to the Ad-
ministrator for a determination that it
meets the criteria of section 1451 of the
Act. The application shall be concise
and describe how the Indian Tribe will
meet each of the requirements of
§ 145.52. The application shall consist of
the following:
(a) A statement that the Tribe is rec-
ognized by the Secretary of the
Interior.
(b) A descriptive statement dem-
onstrating that the Tribal governing
body is currently carrying out substan-
tial governmental duties and powers
over a defined area. The statement
should:
696
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Environmental Protection Agency
§145.58
(1) Describe the form of the Tribal
government;
(2) Describe the types of govern-
mental functions currently performed
by the Tribal governing body such as,
but not limited to, the exercise of po-
lice powers affecting (or relating to)
the health, safety, and welfare of the
affected population; taxation; and the
exercise of the power of eminent do-
main; and
(3) Identify the sources of the Tribal
government's authority to carry out
the governmental functions currently
being performed,
(c) A map or legal description of the
area over which the Indian Tribe as-
serts jurisdiction; a statement by the
Tribal Attorney General (or equivalent
official) which describes the basis for
the Tribe's jurisdictional assertion (in-
cluding the nature or subject matter of
the asserted jurisdiction); a copy of
those documents such as Triba.l con-
stitutions, by-laws, charters, executive
orders, codes, ordinances, and/or reso-
lutions which the Tribe believes are
relevant to its assertions regarding ju-
risdiction; and a description of the lo-
cations of the underground injection
wells the Tribe proposes to regulate,
(d) A narrative statement describing
the capability of the Indian Tribe to
administer an effective "Underground
Injection Control program which
should include:
(1) A description of the Indian Tribe's
previous management experience
which may include, the administration
of programs and services authorized
under the Indian Self-Determination
and Education Assistance Act (25
U.S.C. 450 et seq,), the Indian Mineral
Development Act (25 U.S.C. 2101 et seq.),
or the Indian Sanitation Facilities
Construction Activity Act (42 U.S.C.
2004a).
(2) A list of existing environmental
or public health programs adminis-
tered by the Tribal governing body and
a copy of related Tribal laws, regula-
tions and policies.
(3) A description of the Indian Tribe's
accounting' and procurement systems.
(4) A description of the entity (or en-
tities) which exercise the executive,
legislative, and judicial functions of
the Tribal government.
(5) A description of the existing, or
proposed, agency of the Indian Tribe
which will assume primary enforce-
ment responsibility, including a de-
scription of the relationship between
owners/operators of the underground
injection wells and the agency.
(6) A description of the technical and
administrative capabilities of the staff
to administer and manage an effective
Underground Injection Control Pro-
gram or a plan which proposes how the
Tribe will acquire additional adminis-
trative and/or technical expertise. The
plan must address how the Tribe will
obtain the funds to acquire the addi-
tional administrative and technical
expertise.
te) The Adminstrator may. in his dis-
cretion, request further documentation
necessary to support a Tribe's eligi-
bility.
(f) If the Administrator has pre-
viously determined that a Tribe has
met the prerequisites that make it eli-
gible to assume a role similar to that
of a State as provided by statute under
the Safe Drinking Water Act, the Clean
Water Act. or the Clean Air Act, then
that Tribe need provide only that in-
formation unique to the Underground
Injection Control program (§145.76Cc)
and (d)(6)).
[53 FR 37412, Sept. 26. 3988. as amended at 59
PR 64345. Dec. 14, 1994]
1145.58 Procedure for processing an
Indian Tribe's application.
(a) The Administrator shall process a
completed application of an Indian
Tribe in a timely manner. He shall
promptly notify the Indian Tribe of re-
ceipt of the application.
(b) A tribe that meets the require-
ments of §145.52 is eligible to apply for
development grants and primary en-
forcement responsibility for an Under-
ground Injection Control program and
the associated funding under section
1443
-------
Pf. 146
40 CFi Ch. I (7-1-04 Edition)
PART 146-UNDERGROUND INJEC-
TION CONTROL PROGRAM: CRI-
TERIA AND STANDARDS
Subpart A—General Provisions
Sec.
146.1
146.2
146.3
146.4
146.5
146.6
146,7
146.8
146.9
Applicability and scope.
Law authorizing these regulations.
Definitions.
Criteria for exempted aquifers.
Classification of injection wells.
Area of review.
Corrective action.
Mechanical integrity.
Criteria for establishing permitting
priorities.
146.10 Plugging and abandoning Class I-III
wells.
Subpart B—Criteria and Standards
Applicable to Class I Wells
146.11 Criteria and standards applicable to
Class I nonhazardous wells.
146.12 Construction requirements.
146,13 Operating, monitoring and reporting
requirements.
146.14 Information to be considered by the
Director.
Subpart C—Criteria and Standards
Applicable to Class II Wells
146.21 Applicability.
146,22 Construction requirements.
146.23 Operating, monitoring, and reporting
requirements.
146.24 Information to be considered by the
Director.
Subpart D—Criteria and Standards
Applicable to Class III Wells
146,31 Applicability.
146.32 Construction requirements.
146.33 Operating, monitoring, and reporting
requirements.
148.34 Information to be considered by the
Director.
Subpart E—Criteria and Standards Appli-
cable to Class IV Injection Wells [Re-
served]
Subpart F—Criteria and Standards
Applicable to Class V Injection Wells
146,51 Applicability.
Subpart G—Criteria and Standards Appli-
cable to Class I Hazardous Waste In-
jection Wells
146.61
146.62
Applicability.
Minimum criteria for siting.
146,63 Area of review.
146.64 Corrective action for wells in the area
of review.
146.65 Construction requirements.
146.66 Logging;, sampling, and testing prior
to new well operation.
146.67 Operating requirements.
146.68 Testing and monitoring require-
ments.
146.69 Reporting: requirements.
146.70 Information to be evaluated by the
Director.
146.71 Closure.
146.72 Post-closure care.
146.73 Financial responsibility for post-clo-
sure care,
AUTHORITY: Safe Drinking Water Act, 42
U.S.C. 300f et sect.; Resource Conservation and
Recovery Act, 42 U.S.C, 6901 et seg.
SOURCE: 45 FR 42500, June 24, 1980, unless
otherwise noted.
Subpart A—General Provisions
§ 146.1 Applicability and scope.
(a) This part sets forth technical cri-
teria and standards for the Under-
ground Injection Control Program.
This part should be read in conjunction
with 40 CPR parts 124, 144, and 145,
which also apply to UIC programs. 40
CPR part 144 defines the regulatory
framework of EPA administered per-
mit programs, 40 CPR part 145 de-
scribes the elements of an approvable
State program and procedures for EPA
approval of State participation in the
permit programs, 40 CPB part 124 de-
scribes the procedures the Agency will
use for issuing permits under the cov-
ered programs. Certain of these proce-
dures will also apply to State-adminis-
tered programs as specified in 40 CFR
part 145.
(b) Upon the approval, partial ap-
proval or promulgation, of a State UIC
program by the Administrator, any un-
derground injection which is not au-
thorized by the Director by rule or by
permit is unlawful.
(Clean Water Act, Safe Drinking Water Act,
Glean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 FR 42500, June 24, 1980, as amended at 48
FR 14293, Apr. 1, 1983]
698
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Environmental Protection Agency
§146.3
§ 146.2 Law authorizing these regula-
tions.
The Safe Drinking Water Act, 42
U.S.C. SOOf et seg. authorizes these regu-
lations and all other UIC program reg-
ulations referenced in 40 CFR part 144-
Certain regulations relating to the in-
jection of hazardous waste are also au-
thorized by the Resource Conservation
and Recovery Act, 42 U.S.C. 6901 et seq.
[58 FR 6389B, Dec. 3, 1993]
§ 146.3 Definitions.
The following definitions apply to
the underground injection control pro-
gram.
Abandoned well means a well whose
use has been permanently discontinued
or which is in a state of disrepair such
that it cannot be used for its intended
purpose or for observation purposes.
Administrator means the Adminis-
trator of the United States Environ-
mental Protection Agency, or an au-
thorized representative.
Application means the EPA standard
national forms for applying for a per-
mit, including any additions, revisions
or modifications to the forms; or forms
approved by EPA for use in approved
States, including any approved modi-
fications or revisions. For RCRA, appli-
cation also includes the information
required by the Director under §122.25
{contents of Part B of the RCRA appli-
cation).
Aquifer means a geological forma-
tion, group of formations, or part of a
formation that is capable of yielding a
significant amount of water to a well
or spring.
Area of review means the area sur-
rounding an injection well described
according to the criteria set forth in
§146.06 or in the case of an area permit,
the project area plus a circumscribing
area the width of which is either lh of
a mile or a number calculated accord-
ing to the criteria set forth in §148.06.
Casing means a pipe or tubing of ap-
propriate material, of varying diame-
ter and weight, lowered into a borehole
during or after drilling in order to sup-
port the sides of the hole and thus pre-
vent the walls from caving, to prevent
loss of drilling mud into porous ground,
or to prevent water, gas, or other fluid
from entering or leaving the hole.
Catastrophic collapse means the sud-
den and utter failure of overlying
"strata" caused by removal of under-
lying materials.
Cementing means the operation
whereby a cement slurry is pumped
into a drilled hole and/or forced behind
the casing.
Cesspool means a "drywell" that re-
ceives untreated sanitary waste con-
taining human excreta, and which
sometimes has an open bottom and/or
perforated sides,
Confining bed means a body of imper-
meable or distinctly less permeable
material stratigrapliieally adjacent to
one or more aquifers.
Confining zone means a geological
formation, group of formations, or part
of a formation that is capable of lim-
iting fluid movement above an injec-
tion zone.
Contaminant means any physical.
chemical, biological, or radiological
substance or matter in water.
Conventional mine means an open pit
or underground excavation for the pro-
duction of minerals.
Director means the Regional Adminis-
trator, the State director or the Tribal
director as the context requires, or an
authorized representative. When there
is no approved State or Tribal pro-
gram, and there is an EPA adminis-
tered program, "Director" means the
Regional Administrator. When there is
an approved State or Tribal program.
"Director" normally means the State or
Tribal director. In some circumstances.
however, EPA retains the authority to
take certain actions even when there is
an approved State or Tribal program.
(For example, when EPA has issued an
NPDES permit prior to the approval of
a State program, EPA may retain ju-
risdiction over that permit after pro-
gram approval: see §123.69). In such
cases, the term Director means the Re-
gional Administrator and not the State
or Tribal director.
Disposal well means a well used for
the disposal of waste into a subsurface
stratum.
Dry wail means a well, other than an
improved sinkhole or subsurface fluid
distribution system, completed above
the water table so that its bottom and
sides are typically dry except when re-
ceiving fluids.
699
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§146.3
40 CFR Ch. i (7-1-04 Edition)
Effective date of a UIC program means
the date that a State "UIC program is
approved or established by the Admin-
istrator.
Environmental Protection Agency
("EPA") means the United States Envi-
ronmental Protection Agency.
EPA means the United States "Envi-
ronmental Protection Agency."
Exempted aquifer means an aquifer or
its portion that meets the criteria in
the definition of "underground source
of drinking water" but which has been
exempted according to the procedures
of §144.8(b).
Existing injection well means an "in-
jection well" other than a "new injec-
tion well."
Experimental technology means a tech-
nology which has not been proven fea-
sible under the conditions in which it
is being tested.
Facility or activity means any "HWM
facility," UIC "injection well," NPDES
"point source," or State 404 dredge and
fill activity, or any other facility or ac-
tivity (including land or appurtenances
thereto) that is subject to regulation
under the BORA, UIC, NPDES, or 404
programs.
Fault means a surface or zone of rock
fracture along which there has been
displacement.
Flow rate means the volume per time
unit given to the flow of gases or other
fluid substance which emerges from an
orifice, pump, turbine or passes along a
conduit or channel.
Fluid means material or substance
which flows or moves whether in a
semisolid, liquid, sludge, gas, or any
other form or state.
Formation means a body of rock char-
acterized by a degree of lithologic ho-
mogeneity which is prevailingly, but
not necessarily, tabular and is
mappable on the earth's surface or
traceable in the subsurface.
Formation fluid means "fluid" present
in a "formation" under natural condi-
tions as opposed to introduced fluids,
such as drilling' mud.
Generator means any person, by site
location, whose act or process produces
hazardous waste identified or listed in
40 CFR part 261.
Ground water means water below the
land surface in a zone of saturation.
Hazardous waste means a hazardous
waste as defined in 40 OPR 261.3.
Hazardous Waste Management facility
("HWM facility") means all contiguous
land, and structures, other appur-
tenances, and improvements on the
land used for treating, storing, or dis-
posing of hazardous waste. A facility
may consist of several treatment, stor-
age, or disposal operational units (for
example, one or more landfills, surface
impoundments, or combination of
them).
HWM facility means "Hazardous
Waste Management facility."
Improved sinkhole means a naturally
occurring karst depression or other
natural crevice found in volcanic ter-
rain and other geologic settings which
have been modified by man for the pur-
pose of directing- and emplacing fluids
into the subsurface,
Indian Tribe means any Indian Tribe
having a Federally recognized gov-
erning body carrying out substantial
governmental duties and powers over a
defined area.
Injection well means a "well" into
which "fluids" are being injected,
Injection zone means a geological
"formation", group of formations, or
part of a formation receiving: fluids
through a well.
Lithology means the description of
rocks on the basis of their physical and
chemical characteristics.
Owner or operator means the owner or
operator of any facility or activity sub-
ject to regulation under the RCRA,
UIC, NPDES, or 404 programs.
Packer means a device lowered into a
well to produce a fluid-tight seal.
Permit means an authorization, li-
cense, or equivalent control document
issued by EPA or an "approved State"
to implement the requirements of this
part and parts 124, 144, and 145. Permit
does not include RCRA interim status
(§122.23), UIC authorization by rule
(§§144.21 to 144.26 and 144.15), or any
permit which has not yet been the sub-
ject of final agency action, such as a
"draft permit" or a "proposed permit."
Plugging means the act or process of
stopping the flow of water, oil or gas
into or out of a formation through a
borehole or well penetrating that for-
mation.
700
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Environmental Protection Agency
§146.3
Plugging record means a systematic
listing of permanent or temporary
abandonment of water, oil, gas, test,
exploration and waste injection wells,
and may contain a well log. description
of amounts and types of plugging mate-
rial used, the method employed for
plugging, a description of formations
which are sealed and a graphic log of
the well showing formation location,
formation thickness, and location of
plugging structures,
Point of injection for Class V wells
means the last accessible sampling
point prior to waste fluids being re-
leased Into the subsurface environment
through a Class V injection well. For
example, the point of Injection of a
Class V septic system might be the dis-
tribution box—the last accessible sam-
pling point before the waste fluids
dram into the underlying soils. For a
dry well, it is likely to be the well bore
itself.
Pressure means the total load or force
per unit area acting on a surface,
Project means a group of wells in a
single operation.
Radioactive waste means any waste
which contains radioactive material in
concentrations which exceed those list-
ed in 10 CFR part 20, appendix B, table
II column 2.
RCRA means the Solid Waste Dis-
posal Act as amended by the Resource
Conservation and Recovery Act of 1976
(Pub. L. 94-580, as amended by Pub. L,
95-609, 42 U.S.C, 6901 et seq.).
Sanitary waste means liquid or solid
wastes originating solely from humans
and human activities, such as wastes
collected from toilets, showers, wash
basins, sinks used for cleaning domes-
tic areas, sinks used for food prepara-
tion, clothes washing operations, and
sinks or washing machines where food
and beverage serving dishes, glasses,
and utensils are cleaned. Sources of
these wastes may include single or
multiple residences, hotels and motels,
restaurants, bunkhouses, schools, rang-
er stations, crew quarters, guard sta-
tions, campgrounds, picnic grounds,
day-use recreation areas, other com-
mercial facilities, and industrial facili-
ties provided the waste is not mixed
with industrial waste.
SOW A means the Safe Drinking
Water Act (Pub. L. 95-523, as amended
by Pub. L. 95-190, 42 U.S.C. 300(0 et
seq.).
Septic system means a "well" that is
used to emplace sanitary waste below
the surface and is typically comprised
of a septic tank and subsurface fluid
distribution system or disposal system.
Site means the land or water area
where any facility or activity is phys-
ically located or conducted, including
adjacent land used in connection with
the facility or activity.
Sole or principal source aquifer means
an aquifer which has been designated
by the Administrator pursuant to sec-
tion 1424 (a) or (e) of the SDWA.
State Director means the chief admin-
istrative officer of any State, inter-
state, or Tribal agency operating an
"approved program," or the delegated
representative of the State Director. If
the responsibility is divided among two
or more State, interstate, or Tribal
agencies, "State Director" means the
chief administrative officer of the
State, interstate, or Tribal agency au-
thorized to perform the particular pro-
cedure or function to which reference
is made.
Stratum (plural strata) means a single
sedimentary bed or layer, regardless of
thickness, that consists of generally
the same kind of rock material.
Subsidence means the lowering of the
natural land surface in response to:
Earth movements; lowering of fluid
pressure; removal of underlying sup-
porting material by mining or solution
of solids, either artificially or from
natural causes; compaction due to wet-
ting (Hydrocompaction); oxidation of
organic matter in soils; or added load
on the land surface.
Subsurface fluid distribution system
means an assemblage of perforated
pipes, drain tiles, or other similar
mechanisms intended to distribute
fluids below the surface of the ground.
Surface casing means the first string
of well casing to be Installed in the
well.
Total dissolved solids ("TDS") means
the total dissolved (filterable) solids as
determined by use of the method speci-
fied in 40 CPR part 136.
UIC means the Underground Injec-
tion Control program under Part C of
the Safe Drinking Water Act, including
an "approved program."
701
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§146.4
40 CFR Ch. I (7-1-04 Edition)
Underground injection means a "well
Injection."
Underground source of drinking water
(USDW) means an aquifer or its
portion:
(l)(i) Which supplies any public water
system; or
(ii) Which contains a sufficient quan-
tity of ground water to supply a public
water system; and
(A) Currently supplies drinking water
for human consumption; or
(B) Contains fewer than 10,000 mgr/1
total dissolved solids; and
(2) Which Is not an exempted aquifer.
USDW means "underground source of
drinking water."
Well means: A bored, drilled, or driv-
en shaft whose depth is greater than
the largest surface dimension; or, a dug
hole whose depth is greater than the
largest surface dimension; or, an Im-
proved sinkhole; or, a subsurface fluid
distribution system.
Well injection means the subsurface
emplacement of fluids through a well.
Well plug means a watertight and
gastight seal installed in a borehole or
well to prevent movement of fluids.
Well stimulation means several proc-
esses used to clean the well bore, en-
large channels, and increase pore space
in the interval to be injected thus mak-
ing it possible for wastewater to move
more readily into the formation, and
includes (1) surging, (2) jetting, (3)
blasting, (4) acidizing, (5) hydraulic
fracturing,
Well monitoring means the measure-
ment, by on-site instruments or labora-
tory methods, of the quality of water
in a well.
(Clean Water Act, Safe Drinking Water Act,
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 FR 42500, June 24, 1980, as amended at 46
FB 43161, Aug. 27, 1981; 47 FR 4998, Feb. 3,
1982; 48 FE 14293, Apr. 1, 1983; 53 FR 37414.
Sept. 26, 1988; 64 FR 68573, Dec. 7, 1999]
§ 146.4 Criteria for exempted aquifers.
An aquifer or a portion thereof which
meets the criteria for an "underground
source of drinking water" in §146.3 may
be determined under 40 CFR 144.8 to be
an "exempted aquifer" if it meets the
following criteria:
(a) It does not currently serve as a
source of drinking water; and
(b) It cannot now and will not in the
future serve as a source of drinking
water because:
(1) It is mineral, hydrocarbon or geo-
thermal energy producing, or can be
demonstrated by a permit applicant as
part of a permit application for a Class
II or III operation to contain minerals
or hydrocarbons that considering their
quantity and location are expected to
be commercially producible.
(2) It is situated at a depth or loca-
tion which makes recovery of water for
drinking water purposes economically
or technologically impractical;
(3) It is so contaminated that it
would be economically or techno-
logically impractical to render that
water fit for human consumption; or
(4) It is located over a Class III well
mining area subject to subsidence or
catastrophic collapse; or
(c) The total dissolved solids content
of the ground water is more than 3,000
and less than 10,000 mg/1 and it is not
reasonably expected to supply a public
water system.
(Clean Water Act, Safe Drinking' Water Act,
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 FR 42500, June 24, 1980, as amended at 47
FR 4998, Feb. 3, 1982; 48 FR 14293, Apr. 1, 1983]
§ 146.5 Classification of injection wells.
Injection wells are classified as
follows:
(a) Class I. (1) Wells used by genera-
tors of hazardous waste or owners or
operators of hazardous waste manage-
ment facilities to inject hazardous
waste beneath the lowermost forma-
tion containing, within one quarter (Vi)
mile of the well bore, an underground
source of drinking water.
(2) Other industrial and municipal
disposal wells which inject fluids be-
neath the lowermost formation con-
taining, within one quarter mile of the
well bore, an underground source of
drinking water.
(3) Radioactive waste disposal wells
which inject fluids below the lower-
most formation containing an under-
ground source of drinking water within
one quarter mile of the well bore.
(b) Class II. Wells which inject fluids:
702
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Environmental Protection Agency
§146.5
(1) Which are brought to the surface
in connection with conventional oil or
natural gas production and may be
commingled with waste waters from
gas plants which are an integral part of
production operations, unless those wa-
ters are classified as a hazardous waste
at the time of injection.
(2) For enhanced recovery of oil or
natural gas; and
(3) For storage of hydrocarbons
which are liquid at standard tempera-
ture and pressure.
(c) Class III. Wells which inject for
extraction of minerals including:
(1) Mining of sulfur by the Frasch
process;
(2) In situ production of uranium or
other metals. This category includes
only in-situ production from ore bodies
which have not been conventionally
mined. Solution mining of conven-
tional mines such as stopes leaching is
included in Class V.
(3) Solution mining of salts or pot-
ash.
(d) Class IV, (1) Wells used by genera-
tors of hazardous waste or of radio-
active waste, by owners or operators of
hazardous waste management facili-
ties, or by owners or operators of radio-
active waste disposal sites to dispose of
hazardous waste or radioactive waste
into a formation which within one
quarter (Vi) mile of the well contains
an underground source of drinking
water.
(2) Wells used by generators of haz-
ardous waste or of radioactive waste,
by owners or operators of hazardous
waste management facilities, or by
owners or operators of radioactive
waste disposal sites to dispose of haz-
ardous waste or radioactive waste
above a formation which within one
quarter (Vi) mile of the well contains
an underground source of drinking
water.
(3) Wells used by generators of haz-
ardous waste or owners or operators of
hazardous waste management facilities
to dispose of hazardous waste, which
cannot be classified under §146.05(a)(l)
or §146.05(d) (1) and (2) (e.g., wells used
to dispose of hazardous wastes into or
above a formation which contains an
aquifer which has been exempted pur-
suant to §146.04).
(e) Class V. Injection wells not in-
cluded in Class I, II, III, or IV. Specific
types of Class V injection wells are also
described in 40 CFR 144.81. Class V
wells include:
(1) Air conditioning return flow wells
used to return to the supply aquifer the
water used for heating or cooling in a
heat pump;
(2) Cesspools including- multiple
dwelling, community or regional cess-
pools, or other devices that receive
wastes which have an open bottom and
sometimes have perforated sides. The
DIC requirements do not apply to sin-
gle family residential cesspools nor to
non-residential cesspools which receive
solely sanitary wastes and have the ca-
pacity to serve fewer than 20 persons a
day.
(3) Cooling water return flow wells
used to inject water previously used for
cooling;
(4) Drainage wells used to drain sur-
face fluid, primarily storm runoff, into
a subsurface formation;
(5) Dry wells used for the injection of
wastes into a subsurface formation:
(6) Recharge wells used to replenish
the water in an aquifer;
(7) Salt water intrusion barrier wells
used to inject water into a fresh water
aquifer to prevent the intrusion of salt
water into the fresh water;
(8) Sand backfill and other backfill
wells used to inject a mixture of water
and sand, mill tailings or other solids
into mined out portions of subsurface
mines whether what is injected is a ra-
dioactive waste or not.
(9) Septic system wells used to inject
the waste or effluent from a multiple
dwelling, business establishment, com-
munity or regional business establish-
ment septic tank. The UIC require-
ments do not apply to single family
residential septic system wells, nor to
non-residential septic system wells
which are used solely for the disposal
of sanitary waste and have the capac-
ity to serve fewer than 20 persons a
day.
(10) Subsidence control wells (not
used for the purpose of oil or natural
gas production) used to inject fluids
into a non-oil or gas producing zone to
reduce or eliminate subsidence associ-
ated with the overdraft of fresh water;
703
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§146,6
40 CFR Ch. I (7-1-04 Edition)
(11) Radioactive waste disposal wells
other than Class IV;
(12) Injection wells associated with
the recovery of geothermal energy for
heating, aquaculture and production of
electric power.
(13) Wells used for solution mining of
conventional mines such as stopes
leaching;
(14) Wells used to inject spent brine
into the same formation from which it
was withdrawn after extraction of
halogens or their salts;
(15) Injection wells used in experi-
mental technologies,
(16) Injection wells used for in situ
recovery of lignite, coal, tar sands, and
oil shale.
[45 FR 42500, June 24, 1980, as amended at 46
FR 43161, Aug. 27, 1981; 47 PE 4899, Feb. 3,
1982; 64 PR 68573, Dec, 7, 1999]
§ 146.6 Area of review.
The area of review for each injection
well or each field, project or area of the
State shall be determined according to
either paragraph (a) or (b) of this sec-
tion. The Director may solicit input
from the owners or operators of injec-
tion wells within the State as to which
method is most appropriate for each
geographic area or field.
(a) Zone of endangering influence. (1)
The zone of endangering influence shall
be:
(i) In the case of application(s) for
well permit(s) under §122.38 that area
the radius of which is the lateral dis-
tance in which the pressures in the in-
jection zone may cause the migration
of the injection and/or formation fluid
into an underground source of drinking
water; or
(ii) In the case of an application for
an area permit under §122.39, the proj-
ect area plus a circumscribing area the
width of which is the lateral distance
from the perimeter of the project area,
in which the pressures in the injection
zone may cause the migration of the
injection and/or formation fluid into an
underground source of drinking water.
(2) Computation of the zone of endan-
gering influence may be based upon the
parameters listed below and should be
calculated for an injection time period
equal to the expected life of the injec-
tion well or pattern. The following
modified Theis equation illustrates one
form which the mathematical model
may take.
2.25 KHQ
S10"
1/2
where;
_47iKH(hw-hboxSpGb)
_ _
r=Radius of endangering influence from in-
jection well (length)
k=Hydraulic conductivity of the injection
zone (length/time)
H=Thickness of the injection zone (length)
t=Time of injection (time)
S=Storage coefficient (dimensionless)
Q=Injection rate (volume/time)
ht*,=Ob8erved original hydrostatic head of in-
jection zone (length) measured from the
base of the lowermost underground source
of drinking water
h»=Hydrostatic head of underground source
of drinking water (length) measured from
the base of the lowest underground source
of drinking water
Sp Gh=Specific gravity of fluid in the injec-
tion zone (dimensionless)
jt=3.142 (dimensionless)
The above equation is based on the fol-
lowing assumptions:
(i) The injection zone is homogenous
and isotropic;
(ii) The injection zone has infinite
area extent;
(ill) The injection well penetrates the
entire thickness of the injection zone;
(iv) The well diameter is infinites-
imal compared to "r" when injection
time is longer than a few minutes; and
(v) The emplacement of fluid into the
injection zone creates instantaneous
increase in pressure.
(b) Fixed radius. (1) In the case of ap-
plication^) for well permit(s) under
§122.38 a fixed radius around the well of
not less than one-fourth (Vi) mile may
be used.
(2) In the case of an application for
an area permit under §122.39 a fixed
width of not less than one-fourth (Vt)
mile for the circumscribing area may
be used.
In determining the fixed radius, the
following factors shall be taken into
consideration: Chemistry of injected
and formation fluids; hydrogeology;
population and ground-water use and
704
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Environmental Protection Agency
§146.8
dependence; and historical practices in
the area.
(c) If the area of review is determined
by a mathematical model pursuant to
paragraph (a) of this section, the per-
missible radius is the result of such
calculation even if it is less than one-
fourth (Vi) mile,
[45 PR 42500, June 24, 1980, as amended at 46
FR 43161, Aug. 27. 1981; 47 FR 4999, Feb. 3,
1982]
§ 146.7 Corrective action.
In determining the adequacy of cor-
rective action proposed by the appli-
cant under 40 CPB 144.55 and in deter-
mining the additional steps needed to
prevent fluid movement into under-
ground sources of drinking water, the
following criteria and factors shall be
considered by the Director:
(a) Nature and volume of injected
fluid;
(b) Nature of native fluids or by-prod-
ucts of injection;
(.c) Potentially affected population;
(d) Geology;
(e) Hydrology;
(f) History of the injection operation;
(g) Completion and plugging records;
(h) Abandonment procedures in effect
at the time the well was abandoned;
and
(i) Hydraulic connections with under-
ground sources of drinking water.
(Clean Water Act. Safe Drinking Water Act,
Clean Air Act, Resource Conservation a.nd
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927.
6974)
[45 PR 42500. June 24, 1980, as amended at 46
FR 43162, Aug. 27. 1981: 48 FR 14293, Apr. 1,
1983]
§ 146.8 Mechanical integrity.
(a) An injection well has mechanical
integrity if:
(1) There is no significant leak in the
casing, tubing or packer; and
(2) There is no significant fluid move-
ment into an underground source of
drinking water through vertical chan-
nels adjacent to the injection well
bore.
(ta) One of the following methods
must be used to evaluate the absence of
significant leaks under paragraph (a)(l)
of this section:
(1) Following an initial pressure test.
monitoring of the tubing-casing annu-
lus pressure with sufficient frequency
to be representative, as determined by
the Director, while maintaining an an-
nulus pressure different from atmos-
pheric pressure measured at the sur-
face:
(2) Pressure test with liquid or gas;
or
(3) Records of monitoring showing
the absence of significant changes in
the relationship between injection
pressure and injection flow rate for the
following Class II enhanced recovery
wells:
(i) Existing wells completed without
a packer provided that a pressure test
has been performed and the data is
available and provided further that one
pressure test shall be performed at a
time when the well is shut down and if
the running of such a test will not
cause further loss of significant
amounts of oil or gas; or
(ii) Existing wells constructed with-
out a long string casing, but with sur-
face casing which terminates at the
base of fresh water provided that local
geological and hydrological features
allow such construction and provided
further that the annular space shall be
visually inspected. For these wells, the
Director shall prescribe a monitoring
program which will verify the absence
of significant fluid movement from the
injection zone into an USDW.
(c) One of the following methods
must be used to determine the absence
of significant fluid movement under
paragraph (a)(2) of this section:
(1) The results of a temperature or
noise log; or
(2) For Class II only, cementing
records demonstrating the presence of
adequate cement to prevent such mi-
gration; or
(3) For Class III wells where the na-
ture of the casing precludes the use of
the logging techniques prescribed at
paragraph (c)(l) of this section, ce-
menting records demonstrating the
presence of adequate cement to prevent
such migration;
(4) For Class III wells where the Di-
rector elects to rely on cementing
records to demonstrate the absence of
significant fluid movement, the moni-
toring program prescribed by §146.33(bj
705
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§146.9
40 CFR Ch. 1 (7-1-04 Edition)
shall be designed to verify the absence
of significant fluid movement.
(d) The Director may allow the use of
a test to demonstrate mechanical in-
tegrity other than those listed in para-
graphs (b) and (c)(2) of this section
with the written approval of the Ad-
ministrator. To obtain approval, the
Director shall submit a written request
to the Administrator, which shall set
forth the proposed test and all tech-
nical data supporting its use. The Ad-
ministrator shall approve the request if
it will reliably demonstrate the me-
chanical integrity of wells for which its
use is proposed. Any alternate method
approved by the Administrator shall be
published in the FEDERAL REGISTER
and may be used in all States unless its
use is restricted at the time of ap-
proval by the Administrator.
(e) In conducting and evaluating the
tests enumerated in this section or
others to be allowed by the Director,
the owner or operator and the Director
shall apply methods and standards gen-
erally accepted in the industry. When
the owner or operator reports the re-
sults of mechanical integrity tests to
the Director, he shall include a descrip-
tion of the test(s) and the method(s)
used. In making his/her evaluation, the
Director shall review monitoring and
other test data submitted since the
previous evaluation.
(f) The Director may require addi-
tional or alternative tests if the results
presented by the owner or operator
under §146.8(e) are not satisfactory to
the Director to demonstrate that there
is no movement of fluid into or be-
tween USDWs resulting from the injec-
tion activity.
[45 FR 42500, June 24, 1980, as amended at 46
FB 43162, Aug. 27, 1981; 47 PB 4999, Feb. 3,
1982; 58 FR 63898, Dec. 3, 1993]
§146.9 Criteria for establishing per-
mitting priorities.
In determining prioritiea for setting
times for owners or operators to sub-
mit applications for authorization to
inject under the procedures of §144.31
(a), (c), (g) or §144.22(f), the Director
shall base these priorities upon consid-
eration of the following factors:
(a) Injection wells known or sus-
pected to be contaminating under-
ground sources of drinking water;
(b) Injection wells known to be in-
jecting fluids containing hazardous
contaminants;
(c) Likelihood of contamination of
underground sources of drinking water;
(d) Potentially affected population;
(e) Injection wells violating existing
State requirements;
(f) Coordination with the issuance of
permits required by other State or Fed-
eral permit programs;
(g) Age and depth of the injection
well; and
(h) Expiration dates of existing State
permits, if any.
(Clean Water Act, Safe Drinking Water Act,
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912. 6925, 6927,
6974)
[45 FR 42500, June 24, 1980, as amended at 48
FR 14293, Apr. 1, 1983]
§146.10 Plugging and abandoning
Class I, II, HI, IV, and V wells.
(a) Requirements for Class I, II and
III wells. (1) Prior to abandoning Class
I, II and III wells, the well shall be
plugged with cement in a manner
which will not allow the movement of
fluids either into or between under-
ground sources of drinking water. The
Director may allow Class III wells to
use other plugging materials if the Di-
rector is satisfied that such materials
will prevent movement of fluids into or
between underground sources of drink-
ing water.
(2) Placement of the cement plugs
shall be accomplished by one of the fol-
lowing:
(i) The Balance method;
(ii) The Dump Bailer method;
(ill) The Two-Plug method; or
(iv) An alternative method approved
by the Director, which will reliably
provide a comparable level of protec-
tion to underground sources of drink-
ing water.
(3) The well to be abandoned shall be
in a state of static equilibrium with
the mud weight equalized top to bot-
tom, either by circulating the mud in
the well at least once or by a com-
parable method prescribed by the Di-
rector, prior to the placement of the
cement plug(s).
(4) The plugging and abandonment
plan required in 40 CFR 144.51(o) and
144.52(a)(6) shall, in the case of a Class
706
-------
Environmental Protection Agency
§146,12
III project which underlies or is in an
aquifer which has been exempted under
§146.04, also demonstrate adequate pro-
tection of USDWs. The Director shall
prescribe aquifer cleanup and moni-
toring' where he deems it necessary and
feasible to insure adequate protection
of USDWs.
(b) Requirements for Class IV wells.
Prior to abandoning a Class IV well,
the owner or operator shall close the
well in accordance with 40 OPR
144.2303).
(c) Requirements for Class V wells.
(1) Prior to abandoning a Class V well,
the owner or operator shall close the
well in a manner that prevents the
movement of fluid containing any con-
taminant into an underground source
of drinking water, if the presence of
that contaminant may cause a viola-
tion of any primary drinking water
regulation under 40 CFR part 141 or
may otherwise adversely affect the
health of persons. Closure require-
ments for motor vehicle waste disposal
wells and large-capacity cesspools are
reiterated at § 144.89.
(2) The owner or operator shall dis-
pose of or otherwise manage any soil,
gravel, sludge, liquids, or other mate-
rials removed from or adjacent to the
well in accordance with all applicable
Federal, State, and local regulations
and requirements.
[64 FR 88573. Dec. 7. 1999)
Subpart B—Criteria and Standards
Applicable to Class 1 Wells
§ 146.11 Criteria and standards appli-
cable to Class I nonhazardous wells.
This subpart establishes criteria and
standards for underground Injection
control programs to regulate Class I
nonhazardous wells.
[53 PR 28148. July 26. 1988]
§ 146,12 Construction requirements.
(a) All Class I wells shall be sited in
such a fashion that they inject into a
formation which is beneath the lower-
most formation containing, within one
quarter mile of the well bore, an under-
ground source of drinking water.
(b) All Class I wells shall be cased
and cemented to prevent the movement
of fluids into or between underground
sources of drinking water. The casing
and cement used in the construction of
each newly drilled well shall be de-
signed for the life expectancy of the
well. In determining and specifying
casing and cementing requirements,
the following factors shall be consid-
ered:
(1) Depth to the injection zone;
(2) Injection pressure, external pres-
sure, internal pressure, and axial load-
ing;
(3) Hole size;
(4) Size and grade of all casing
strings (wall thickness, diameter,
nominal weight, length, joint, specifica-
tion, and construction material);
(5) Corrosiveness of injected fluid,
formation fluids, and temperatures;
(6) Lithology of injection and con-
fining intervals; and
(7) Type or grade of cement.
(c) All Class I injection wells, except
those municipal wells injecting non-
corrosive wastes, shall inject fluids
through tubing with a packer set im-
mediately above the injection zone, or
tubing- with an approved fluid seal as
an alternative. The tubing, packer, and
fluid seal shall be designed for the ex-
pected service.
(1) The use of other alternatives to a
packer may be allowed with the writ-
ten approval of the Director. To obtain
approval, the operator shall submit a
written request to the Director, which
shall set forth the proposed alternative
and all technical data supporting its
use. The Director shall approve the re-
quest if the alternative method will re-
liably provide a comparable level of
protection to underground sources of
drinking water. The Director may ap-
prove an alternative method solely for
an individual well or for general use.
(2) In determining' and specifying re-
quirements for tubing, packer, or alter-
natives the following factors shall be
considered:
(i) Depth of setting;
(ii) Characteristics of injection fluid
(chemical content, corrosiveness, and
density):
(iii) Injection pressure;
(iv) Annular pressure;
(v) Rate, temperature and volume of
injected fluid; and
(vi) Size of casing.
707
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§146.13
40 CFR Ch. I (7-1-04 Edition)
(d) Appropriate logs and other tests
shall be conducted during the drilling
and construction of new Class I wells.
A descriptive report interpreting the
results of such logs and tests shall be
prepared by a knowledgeable log ana-
lyst and submitted to the Director. At
a minimum, such logs and tests shall
include:
(1) Deviation checks on all holes con-
structed by first drilling a pilot hole,
and then enlarging the pilot hole by
reaming or another method. Such
checks shall be at sufficiently frequent
intervals to assure that vertical ave-
nues for fluid migration in the form of
diverging holes are not created during
drilling.
(2) Such other logs and tests as may
be needed after taking into account the
availability of similar data in the area
of the drilling site, the construction
plan, and the need for additional infor-
mation, that may arise from time to
time as the construction of the well
progresses. In determining which logs
and tests shall be required, the fol-
lowing logs shall be considered for use
in the following situations:
(i) For surface casing intended to
protect underground sources of drink-
ing water:
(A) Resistivity, spontaneous poten-
tial, and caliper logs before the casing
is installed; and
(B) A cement bond, temperature, or
density log after the casing is set and
cemented.
(ii) For intermediate and long strings
of casing intended to facilitate
injection:
(A) Resistivity, spontaneous poten-
tial, porosity, and gamma ray logs be-
fore the casing is installed;
(B) Fracture finder logs; and
(C) A cement bond, temperature, or
density log after the casing is set and
cemented.
(e) At a minimum, the following in-
formation concerning the injection for-
mation shall be determined or cal-
culated for new Class I wells:
(1) Fluid pressure:
(2) Temperature;
(3) Fracture pressure;
(4) Other physical and chemical char-
acteristics of the injection matrix; and
(5) Physical and chemical character-
istics of the formation fluids.
[45 FB 42500, June 24, 1980, as amended at 46
FR 43162, Aug. 27, 1981]
§146.13 Operating, monitoring and re-
porting requirements.
(a) Operating requirements. Operating
requirements shall at a minimum,
specify that:
(1) Except during stimulation injec-
tion pressure at the wellhead shall not
exceed a maximum which shall be cal-
culated so as to assure that the pres-
sure in the injection zone during injec-
tion does not initiate new fractures or
propagate existing fractures in the in-
jection zone. In no case shall injection
pressure initiate fractures in the con-
fining zone or cause the movement of
injection or formation fluids into an
underground source of drinking water.
(2) Injection between the outermost
casing protecting underground sources
of drinking water and the well bore is
prohibited.
(3) Unless an alternative to a packer
has been approved under §146.12(c), the
annulus between the tubing and the
long string of casings shall be filled
with a fluid approved by the Director
and a pressure, also approved by the
Director, shall be maintained on the
annulus.
(b) Monitoring requirements. Moni-
toring requirements shall, at a min-
imum, include:
(1) The analysis of the injected fluids
with sufficient frequency to yield rep-
resentative data of their characteris-
tics:
(2) Installation and use of continuous
recording devices to monitor injection
pressure, flow rate and volume, and the
pressure on the annulus between the
tubing and the long string of casing;
(3) A demonstration of mechanical
integrity pursuant to §146,8 at least
once every five years during the life of
the well: and
(4) The type, number and location of
wells within the area of review to be
used to monitor any migration of fluids
into and pressure in the underground
sources of drinking water, the param-
eters to be measured and the frequency
of monitoring.
708
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Environmental Protection Agency
§146.14
(c) Reporting requirements. Reporting
requirements shall, at a minimum, in-
clude:
(1) Quarterly reports to the Director
on:
(i) The physical, chemical and other
relevant characteristics of injection
fluids;
(ti) Monthly average, maximum and
minimum values for injection pressure,
flow rate and volume, and annular
pressure; and
(iii) The results of monitoring pre-
scribed under paragraph (b)(4) of this
section,
(2) Reporting the results, with the
first quarterly report after the comple-
tion, of:
(i) Periodic tests of mechanical in-
tegrity;
(ii) Any other test of the injection
well conducted by the permittee if re-
quired by the Director; and
(iii) Any well work over.
(d) Ambient monitoring, (I) Based on a
site-specific assessment of the poten-
tial for fluid movement from the well
or injection zone and on the potential
value of monitoring wells to detect
such movement, the Director shall re-
quire the owner or operator to develop
a monitoring program. At a minimum,
the Director shall require monitoring
of the pressure buildup in the injection
zone annually, including at a min-
imum, a shut down of the well for a
time sufficient to conduct a valid ob-
servation of the pressure fall-off curve.
(2) When prescribing a monitoring
system the Director may also require:
(i) Continuous monitoring for pres-
sure changes in the first aquifer over-
lying the confining zone. When such a
well is installed, the owner or operator
shall, on a quarterly basis, sample the
aquifer and analyze for constituents
specified by the Director;
(ii) The use of indirect, geophysical
techniques to determine the position of
the waste front, the water quality in a
formation designated by the Director,
or to provide other site specific data;
(iii) Periodic monitoring of the
ground water quality in the first aqui-
fer overlying the injection zone;
(iv) Periodic monitoring of the
ground water quality in the lowermost
USDW: and
(v) Any additional monitoring nec-
essary to determine whether fluids are
moving into or between USDWs.
[45 PR 42500, June 24. 1980. as amended at 46
FR 43162, Aug. 27, 1981; 47 FR 32129, July 26.
1982; 53 PB 28148, July 26, 1988J
§ 146.14 Information to be considered
by the Director.
This section sets forth the informa-
tion which must be considered by the
Director in authorizing Class I wells.
For an existing or converted new Class
I well the Director may rely on the ex-
isting permit file for those items of in-
formation listed below which are cur-
rent and accurate in the file. For a
newly drilled Class I well, the Director
shall require the submission of all the
information listed below. For both ex-
isting and new Class I wells certain
maps, cross-sections, tabulations of
wells within the area of review and
other data may be included in the ap-
plication by reference provided they
are current, readily available to the Di-
rector (for example, in the permitting
agency's files) and sufficiently identi-
fied to be retrieved. In cases where
EPA issues the permit all the informa-
tion in this section must be submitted
to the Administrator.
(a) Prior to the issuance of a permit
for an existing Class I well to operate
or the construction or conversion of a
new Class I well the Director shall con-
sider the following:
(1) Information required in 40 CFR
144.31 and 144.31(gr);
(2) A map showing the injection
well(s) for which a permit is sought and
the applicable area of review. Within
the area of review, the map must show
the number, or name, and location of
all producing wells, dry holes, surface
bodies of water, springs, mines (surface
and subsurface), quarries, water wells
and other pertinent surface features in-
cluding residences and roads. The map
should also show faults, if known or
suspected. Only information of public
record is required to be included on
this map;
(3) A tabulation of data on all wells
within the area of review which pene-
trate into the proposed injection zone.
Such data shall include a description of
each well's type, construction, date
709
-------
§146.21
40 CFR Ch. I (7-1-04 Edition)
drilled, location, depth, record of plug-
ging and/or completion, and any addi-
tional information the Director may
require:
(4) Maps and cross sections indicating
the general vertical and lateral limits
of all underground sources of drinking
water within the area of review, their
position relative to the injection for-
mation and the direction of water
movement, where known, in each un-
derground source of drinking water
which may be affected by the proposed
injection;
(5) Maps and cross sections detailing
the geologic structure of the local area;
(6) Generalized maps and cross sec-
tions illustrating the regional geologic
setting;
(7) Proposed operating data:
(i) Average and maximum daily rate
and volume of the fluid to be injected;
(ii) Average and maximum injection
pressure; and
(iii) Source and an analysis of the
chemical, physical, radiological and bi-
ological characteristics of injection
fluids;
(8) Proposed formation testing pro-
gram to obtain an analysis of the
chemical, physical and radiological
characteristics of and other informa-
tion on the receiving formation;
(9) Proposed stimulation program;
(10) Proposed injection procedure;
(11) Schematic or other appropriate
drawings of the surface and subsurface
construction details of the well.
(12) Contingency plans to cope with
all shut-ins or well failures so as to
prevent migration of fluids into any
underground source of drinking water;
(13) Plans (including maps) for meet-
ing the monitoring requirements in
§146.13(b):
(14) For wells within the area of re-
view which penetrate the injection
zone but are not properly completed or
plugged, the corrective action proposed
to be taken under 40 CFR 144.55;
(15) Construction procedures includ-
ing a cementing and casing program,
logging procedures, deviation checks,
and a drilling, testing, and coring pro-
gram; and
(16) A certificate that the applicant
has assured, through a performance
bond or other appropriate means, the
resources necessary to close, plug or
abandon the well as required by 40 CFR
122.42(g).
(b) Prior to granting approval for the
operation of a Class I well the Director
shall consider the following informa-
tion:
(1) All available logging and testing
program data on the well;
(2) A demonstration of mechanical
integrity pursuant to § 146.8;
(3) The anticipated maximum pres-
sure and flow rate at which the per-
mittee will operate;
(4) The results of the formation test-
ing program;
(5) The actual injection procedure;
(6) The compatibility of injected
waste with fluids in the injection zone
and minerals in both the injection zone
and the confining lone; and
(7) The status of corrective action on
defective wells in the area of review.
(c) Prior to granting approval for the
plugging and abandonment of a Class I
well the Director shall consider the fol-
lowing information:
(1) The type and number of plugs to
be used;
(2) The placement of each plug in-
cluding the elevation of the top and
bottom;
(3) The type and grade and quantity
of cement to be used;
(4) The method for placement of the
plugs; and
(5) The procedure to be used to meet
the requirement of § 146.10(c).
(Clean Water Act, Safe Drinking Water Act,
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6906, 6912, 6825, 6927,
6974)
[45 FR 42500, Jnae 24, 1980, as amended at 46
FE 43162, Aug. 27, 1981; 48 FR 14293, Apr. 1,
1983]
Subpart C—Criteria and Standards
Applicable to Class II Wells
§ 146.21 Applicability.
This subpart establishes criteria and
standards for underground injection
control programs to regulate Class II
wells.
§ 146.22 Construction requirements.
(a) All new Class II wells shall be
sited in such a fashion that they inject
into a formation which is separated
from any USDW by a confining zone
710
-------
Environmental Protection Agency
§ 146,22
that Is free of known open faults or
fractures within the area of review.
(b)(l) All Class II injection wells shall
be cased and cemented to prevent
movement of fluids into or between un-
derground sources of drinking water.
The casing and cement used in the con-
struction of each newly drilled well
shall he designed for the life expect-
ancy of the well. In determining and
specifying casing and cementing re-
quirements, the following factors shall
be considered:
(i) Depth to the injection zone;
(ii) Depth to the bottom of all
USDWs; and
(iii) Estimated maximum and aver-
age injection pressures;
(2) In addition the Director may con-
sider information on:
(i) Nature of formation fluids;
(ii) Lithology of injection and con-
fining zones;
(iii) External pressure, internal pres-
sure, and axial loading;
(iv) Hole size;
(v) Size and grade of all casing
strings; and
(vi) Class of cement.
(c) The requirements in paragraph (b)
of this section need not apply to exist-
ing or newly converted Class II wells
located in existing fields if:
(1) Regulatory controls for casing
and cementing existed for those wells
at the time of drilling and those wells
are in compliance with those controls;
and
(2) Well injection will not result in
the movement of fluids Into an under-
ground source of drinking water so as
to create a significant risk to the
health of persons.
(d) The requirements in paragraph (b)
of this section need not apply to newly
drilled wells in existing fields if;
(1) They meet the requirements of
the State for casing and cementing ap-
plicable to that field at the time of
submission of the State program to the
Administrator; and
(2) Well injection will not result in
the movement of fluids into an under-
ground source of drinking water so as
to create a significant risk to the
health of persons.
(e) Where a State did not have regu-
latory controls for casing- and cement-
ing prior to the time of the submission
of the State program to the Adminis-
trator, the Director need not apply the
casing and cementing requirements in
paragraph (b) of this section if he sub-
mits as a part of his application for pri-
macy, an appropriate plan for casing
and cementing of existing, newly con-
verted, and newly drilled wells in exist-
ing fields, and the Administrator ap-
proves the plan.
(f) Appropriate logs and other tests
shall be conducted during the drilling
and construction of new Class II wells.
A descriptive report interpreting the
results of that portion of those logs
and tests which specifically relate to
(1) an USDW and the confining zone ad-
jacent to it, and (2) the injection and
adjacent formations shall be prepared
by a knowledgeable log analyst and
submitted to the director. At a min-
imum, these logs and tests shall in-
clude:
(1) Deviation checks on all holes con-
structed by first drilling a pilot hole
and then enlarging the pilot hole, by
reaming or another method. Such
checks shall be at sufficiently frequent
intervals to assure that vertical ave-
nues for fluid movement in the form of
diverging holes are not created during
drilling.
(2) Such other logs and tests as may
be needed after taking into account the
availability of similar data in the area
of the drilling site, the construction
plan, and the need for additional
information that may arise from time
to time as the construction of the well
progresses. In determining which logs
and tests shall be required the fol-
lowing shall be considered by the Di-
rector in setting logging and testing
requirements:
(i) For surface casing intended to
protect underground sources of drink-
ing water in areas where the lithology
has not been determined:
(A) Electric and caliper logs before
casing is installed; and
(B) A cement bond, temperature, or
density log after the casing is set and
cemented.
(ii) for intermediate and long strings
of casing intended to facilitate injec-
tion:
(A) Electric porosity and gamma ray
logs before the casing is Installed;
(B) Fracture finder logs; and
711
-------
§146.23
40 CFR Ch. I (7-1-04 Edition)
(C) A cement bond, temperature, or
density log after the casing is set and
cemented,
(g) At a minimum, the following in-
formation concerning the injection for-
mation shall be determined or cal-
culated for new Class II wells or
projects:
(1) Fluid pressure;
(2) Estimated fracture pressure;
(3) Physical and chemical character-
istics of the injection zone.
[45 PR 42500, June 24, 1980, as amended at 46
PR 43162, Aug. 27, 1981; 47 PR 5000, Feb. 3,
1982]
§ 146,23 Operating, monitoring, and re-
porting requirements.
(a) Operating requirements. Operating
requirements shall, at a minimum,
specify that:
(1) Injection pressure at the wellhead
shall not exceed a maximum which
shall be calculated so as to assure that
the pressure during injection does not
initiate new fractures or propagate ex-
isting fractures in the confining zone
adjacent to the USDWs. In no case
shall injection pressure cause the
movement of injection or formation
fluids into an underground source of
drinking water
(2) Injection between the outermost
casing protecting underground sources
of drinking water and the well bore
shall be prohibited.
(b) Monitoring requirements. Moni-
toring requirements shall, at a min-
imum, include:
(1) Monitoring of the nature of in-
jected fluids at time intervals suffi-
ciently frequent to yield data rep-
resentative of their characteristics;
(2) Observation of injection pressure,
flow rate, and cumulative volume at
least with the following frequencies:
(i) Weekly for produced fluid disposal
operations:
(ii) Monthly for enhanced recovery
operations;
(ill) Daily during the injection of liq-
uid hydrocarbons and injection for
withdrawal of stored hydrocarbons; and
(Iv) Daily during the injection phase
of cyclic steam operations
And recording of one observation of in-
jection pressure, flow rate and cumu-
lative volume at reasonable intervals
no greater than 30 days.
(3) A demonstration of mechanical
integrity pursuant to §146.8 at least
once every five years during the life of
the injection well:
(4) Maintenance of the results of all
monitoring until the next permit re-
view (see 40 CPE 144.52(a)(5)): and
(5) Hydrocarbon storage and en-
hanced recovery may be monitored on
a field or project basis rather than on
an individual well basis by manifold
monitoring. Manifold monitoring may
be used in cases of facilities consisting
of more than one injection well, oper-
ating with a common manifold. Sepa-
rate monitoring systems for each well
are not required provided the owner/op-
erator demonstrates that manifold
monitoring is comparable to individual
well monitoring.
(c) Reporting requirements. (1) Report-
ing requirements shall at a minimum
include an annual report to the Direc-
tor summarizing the results of moni-
toring required under paragraph (b) of
this section. Such summary shall in-
clude monthly records of injected
fluids, and any major changes in char-
acteristics or sources of injected fluid.
Previously submitted information may
be included by reference.
(2) Owners or operators of hydro-
carbon storage and enhanced recovery
projects may report on a field or
project basis rather than an individual
well basis where manifold monitoring
is used.
(Clean Water Act, Sale Drinking Water Act.
Clean Air Act, Resource Conservation and
Recovery Act; 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 PR 42500, June 24, 1980, as amended at 46
FR 43162, Aug. 27, 1981; 47 FR 5000, Feb. 3,
1982; 48 PR 14293, Apr, 1. 1983; 48 PR 31404,
July 8. 1983]
§146.24 Information to be considered
by the Director,
This section sets forth the informa-
tion which must be considered by the
Director in authorizing Class II wells.
Certain maps, cross-sections, tabula-
tions of wells within the area of review,
and other data may be included in the
application by reference provided they
are current, readily available to the Di-
rector (for example, in the permitting
agency's files) and sufficiently identi-
fied to be retrieved. In cases where
712
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Environmental Protection Agency
§ 146.24
EPA issues the permit, all the informa-
tion in this section is to be submitted
to the Administrator.
(a) Prior to the issuance of a permit
for an existing Class II well to operate
or the construction or conversion of a
new Class II well the Director shall
consider the following':
(1) Information required in 40 CPE,
144.31 and 144.31(g);
(2) A map showing the injection well
or project area for which a permit is
sought and the applicable area of re-
view. Within the area of review, the
map must show the number or name
and location of all existing producing
wells, injection wells, abandoned wells,
dry holes, and water wells. The map
may also show surface bodies of waters,
mines (surface and subsurface), quar-
ries and other pertinent surface fea-
tures including residences and roads,
and faults if known or suspended. Only
information of public record and perti-
nent information known to the appli-
cant is required to be included on this
map. This requirement does not apply
to existing Class II wells; and
(3) A tabulation of data reasonably
available from public records or other-
wise known to the applicant on all
wells within the area of review in-
cluded on the map required under para-
graph (a)(2) of this section which pene-
trate the proposed injection zone or, in
the case of Class II wells operating over
the fracture pressure of the injection
formation, all known wells within the
area of review which penetrate forma-
tions affected by the increase in pres-
sure. Such data shall include a descrip-
tion of each well's type, construction,
date drilled, location, depth, record of
plugging and complete, and any addi-
tional information the Director may
require. In cases where the information
would be repetitive and the wells are of
similar age, type, and construction the
Director may elect to only require data
on a representative number of wells.
This requirement does not apply to ex-
isting Class II wells.
(t'i Proposed operating data:
(i) Average and maximum daily rate
and volume of fluids to be injected,
(ii) Average and maximum injection
pressure; and
(iii) Source and an appropriate anal-
ysis of the chemical and physical char-
acteristics of the injection fluid.
(5) Appropriate geological data on
the injection zone and confining zone
including lithologic description, geo-
logical name, thickness and depth;
(6) Geologic name and depth to bot-
tom of all underground sources of
drinking water which may be affected
by the injection;
(7) Schematic or other appropriate
drawings of the surface and subsurface
construction details of the well;
(8) In the case of new injection wells
the corrective action proposed to be
taken by the applicant under 40 CPB
122.44;
(9) A certificate that the applicant
has assured through a performance
bond or other appropriate means, the
resources necessary to close plug or
abandon the well as required by 40 CFB
122.42(g);
(b) In addition the Director may con-
sider the following:
(1) Proposed formation testing pro-
gram to obtain the information re-
quired by §146.22(g);
(2) Proposed stimulation program;
(3) Proposed injection procedure;
(4) Proposed contingency plans, if
any, to cope with well failures so as to
prevent migration of contaminating
fluids into an underground source of
drinking water;
(5) Plans for meeting the monitoring
requirements of §146.23(b).
(c) Prior to granting approval for the
operation of a Class II well the Direc-
tor shall consider the following infor-
mation:
(1) All available logging and testing
program data on the well;
(2) A demonstration of mechanical
integrity pursuant to §146.8;
(3) The anticipated maximum pres-
sure and flow rate at which the per-
mittee will operate.
(4) The results of the formation test-
ing program:
(5) The actual injection procedure;
and
(6) For new wells the status of correc-
tive action on defective wells in the
area of review.
(d) Prior to granting approval for the
plugging and abandonment of a Class II
713
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§146.31
40 CFR Ch. I (7-1-04 Edition)
well the Director shall consider the fol-
lowing information:
(1) The type, and number of plugs to
be used;
(2) The placement of each plug In-
cluding the elevation of top and bot-
tom;
(3) The type, grade, and quantity of
cement to be used;
(4) The method of placement of the
plugs; and
(5) The procedure to be used to meet
the requirements of §146.10(c).
(Clean Water Act, Safe Drinking Water Act.
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 FE 42500, June 24. 1980, as amended at 46
FR 43162, Aug. 27, 1981; 47 FR 5000, Feb. 3,
1982; 48 FR 14293, Apr. 1, 1983]
Subpart D—Criteria and Standards
Applicable to Class III Wells
§ 146.31 Applicability,
This subpart establishes criteria and
standards for underground injection
control programs to regulate Class III
wells.
§ 146.32 Construction requirements.
(a) All new Class III wells shall be
cased and cemented to prevent the mi-
gration of fluids into or between under-
ground sources of drinking water. The
Director may waive the cementing re-
quirement for new wells in existing
projects or portions of existing projects
where he has substantial evidence that
no contamination of underground
sources of drinking water would result.
The casing and cement used in the con-
struction of each newly drilled well
shall be designed for the life expect-
ancy of the well. In determining' and
specifying casing and cementing- re-
quirements, the following factors shall
be considered:
(1) Depth to the injection zone;
(2) Injection pressure, external pres-
sure, internal pressure, axial loading,
etc.;
(3) Hole size;
(4) Size and grade of all casing
strings (wall thickness, diameter,
nominal weight, length, joint specifica-
tion, and construction material);
(5) Corrosrveness of injected fluids
and formation fluids;
(6) Lithology of injection and con-
fining zones; and
(7) Type and grade of cement.
(b) Appropriate logs and other tests
shall be conducted during the drilling
and construction of new Class III wells,
A descriptive report interpreting the
results of such logs and tests shall be
prepared by a knowledgeable log ana-
lyst and submitted to the Director. The
logs and tests appropriate to each type
of Class III well shall be determined
based on the intended function, depth,
construction and other characteristics
of the well, availability of similar data
in the area of the drilling site and the
need for additional information that
may arise from time to time as the
construction of the well progresses. De-
viation checks shall be conducted on
all holes where pilot holes and reaming
are used, unless the hole will be cased
and cemented by circulating cement to
the surface. Where deviation checks
are necessary they shall be conducted
at sufficiently frequent intervals to as-
sure that vertical avenues for fluid mi-
gration in the form of diverging holes
are not created during drillings.
(c) Where the injection zone is a for-
mation which is naturally water-bear-
ing the following' information con-
cerning the injection zone shall be de-
termined or calculated for new Class
III wells or projects:
(1) Fluid pressure;
(2) Fracture pressure; and
(3) Physical and chemical character-
istics of the formation fluids.
(d) Where the injection formation is
not a water-bearing formation, the in-
formation in paragraph (c)(2) of this
section must be submitted.
(e) Where injection is into a forma-
tion which contains water with less
than 10.000 mg/1 TDS monitoring wells
shall be completed into the injection
zone and into any underground sources
of drinking water above the injection
aone which could be affected by the
mining operation. These wells shall be
located in such a fashion as to detect
any excursion of injection fluids, proc-
ess "by-products, or formation fluids
outside the mining area or zone. If the
operation may be affected by subsid-
ence or catastrophic collapse the moni-
toring wells shall be located so that
they will not be physically affected.
714
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Environmental Protection Agency
§ 146.33
(f) Where injection is into a forma-
tion which does not contain water with
less than 10,000 rng/1 TDS, no moni-
toring wells are necessary in the injec-
tion stratum.
(g) Where the injection wells pene-
trate an USDW in an area subject to
subsidence or catastrophic collapse an
adequate number of monitoring wells
shall be completed into the USDW to
detect any movement of injected
fluids, process by-products or forma-
tion fluids into the USDW. The moni-
toring wells shall be located outside
the physical influence of the subsid-
ence or catastrophic collapse.
(h) In determining; the number, loca-
tion, construction and frequency of
monitoring of the monitoring wells the
following criteria shall be considered:
(1) The population relying on the
USDW affected or potentially affected
by the injection operation;
(2) The proximity of the injection op-
eration to points of withdrawal of
drinking water;
(3) The local geology and hydrology;
(4) The operating pressures and
whether a negative pressure gradient is
being maintained;
(5) The nature and volume of the in-
jected fluid, the formation water, and
the process by-products; and
(6) The injection well density.
[45 PR 42500, June 24, 1980, as amended at 46
FK 43163, Aug. 27. 1981; 47 FR 5000, Feb. 3,
1982]
§ 146,33 Operating, monitoring, and re-
porting requirements.
(a) Operating requirements. Operating
requirements prescribed shall, at a
minimum, specify that:
(1) Except during well stimulation in-
jection pressure at the wellhead shall
be calculated so as to assure that the
pressure in the injection zone during
injection does not initiate new frac-
tures or propagate existing fractures in
the injection zone. In no case, shall in-
jection pressure initiate fractures in
the confining zone or cause the migra-
tion of injection or formation fluids
into an underground source of drinking
water.
(2) Injection between the outermost
casing protecting underground sources
of drinking water and the well bore is
prohibited.
(b) Monitoring requirements. Moni-
toring requirements shall, at a min-
imum, specify:
(1) Monitoring of the nature of in-
jected fluids with sufficient frequency
to yield representative data on its
characteristics. Whenever the injection
fluid is modified to the extent that the
analysis required by §146.34(a)(7)(iii) is
incorrect or incomplete, a new analysis
as required by §146.34(a)(7)(iii) shall be
provided to the Director.
(2) Monitoring of injection pressure
and either flow rate or volume semi-
monthly, or metering and daily record-
ing of injected and produced fluid vol-
umes as appropriate.
(3) Demonstration of mechanical in-
tegrity pursuant to §146.08 at least
once every five years during the life of
the well for salt solution mining.
(4) Monitoring of the fluid level in
the injection zone semi-monthly,
where appropriate and monitoring of
the parameters chosen to measure
water quality in the monitoring wells
required by § 146.32(e), semi-monthly.
(5) Quarterly monitoring of wells re-
quired by §146.32(g).
(6) All Class III wells may be mon-
itored on a field or project basis rather
than an individual well basis by mani-
fold monitoring. Manifold monitoring
may be used in cases of facilities con-
sisting of more than one injection well,
operating with a common manifold.
Separate monitoring systems for each
well are not required provided the
owner/operator demonstrates that
manifold monitoring is comparable to
individual well monitoring.
(c) Reporting requirements. Reporting
requirements shall, at a minimum, in-
clude:
(1) Quarterly reporting to the Direc-
tor on required monitoring;
(2) Results of mechanical integrity
and any other periodic test required by
the Director reported with the first
regular quarterly report after the com-
pletion of the test; and
(3) Monitoring may be reported on a
project or field basis rather than Indi-
vidual well basis where manifold moni-
toring is used,
[45 FR 42500, June 24, 1980, as amended at 46
FR 43163. Aug. 27, 1981: 46 PR 5001, Feb. 3.
1982; 48 FR 31404, July 8, 1983]
715
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§146.34
40 CFR Ch. I (7-1-04 Edition)
§ 146.34 Information to be considered
by the Director.
This section sets forth the informa-
tion which must be considered by the
Director in authorizing Class III wells.
Certain maps, cross sections, tabula-
tions of wells within the area of review,
and other data may be included in the
application by reference provided they
are current, readily available to the Di-
rector (for example, in the permitting
agency's files) and sufficiently identi-
fied to be retrieved. In cases where
EPA issues the permit, all the informa-
tion in this section must be submitted
to the Administrator,
(a) Prior to the issuance of a permit
for an existing Class III well or area to
operate or the construction of a new
Class III well the Director shall con-
sider the following:
(1) Information required in 40 CFR
144.31 and 144.31(g);
(2) A map showing the injection well
or project area for which a permit Is
sought and the applicable area of re-
view. Within the area of review, the
map must show the number or name
and location of all existing producing
wells, injection wells, abandoned wells,
dry holes, public water systems and
water wells. The map may also show
surface bodies of waters, mines (surface
and subsurface), quarries and other
pertinent surface features including
residences and roads, and faults if
known or suspected. Only information
of public record and pertinent informa-
tion known to the applicant is required
to be included on this map.
(3) A tabulation of data reasonably
available from public records or other-
wise known to the applicant on wells
within the area of review included on
the map required under paragraph
(a)(2) of this section which penetrate
the proposed injection zone. Such data
shall include a description of each
well's type, construction, date drilled,
location, depth, record of plugging and
completion, and any additional infor-
mation the Director may require. In
cases where the information would be
repetitive and the wells are of similar
age, type, and construction the Direc-
tor may elect to only require data on a
representative number of wells.
(4) Maps and cross sections indicating
the vertical limits of ail underground
sources of drinking water within the
area of review, their position relative
to the injection formation, and the di-
rection of water movement, where
known, in every underground source of
drinking water which may be affected
by the proposed injection:
(5) Maps and cross sections detailing
the geologic structure of the local area;
(6) Generalized map and cross sec-
tions illustrating the regional geologic
setting;
(7) Proposed operating data:
(i) Average and maximum daily rate
and volume of fluid to be injected;
(ii) Average and maximum Injection
pressure; and
(Hi) Qualitative analysis and ranges
in concentrations of all constituents of
Injected fluids. The applicant may re-
quest Federal confidentiality as speci-
fied in 40 CFR part 2. If the informa-
tion is proprietary an applicant may,
in lieu of the ranges in concentrations,
choose to submit maximum concentra-
tions which shall not be exceeded. In
such a case the applicant shall retain
records of the undisclosed concentra-
tions and provide them upon request to
the Director as part of any enforce-
ment investigation.
(8) Proposed formation testing pro-
gram to obtain the information re-
quired by §146.32(c).
(9) Proposed stimulation program;
(10) Proposed injection procedure;
(11) Schematic or other appropriate
drawings of the surface and subsurface
construction details of the well;
(12) Plans (including maps) for meet-
ing the monitoring requirements of
§146.33(b);
(13) Expected changes in pressure, na-
tive fluid displacement, direction of
movement of injection fluid;
(14) Contingency plans to cope with
all sliut-ins or well failures so as to
prevent the migration of contami-
nating fluids into underground sources
of drinking water;
(15) A certificate that the applicant
has assured, through a performance
bond, or other appropriate means, the
resources necessary to close, plug, or
abandon the well as required by 40 CFR
144.52(a)(7) and
(16) The corrective action proposed to
be taken under 40 CFR 144,55.
716
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Environmental Protection Agency
§146.61
(b) Prior to granting approval for the
operation of a Class III well the Direc-
tor shall consider the following infor-
mation:
(1) All available logging and testing
data on the well;
(2) A satisfactory demonstration of
mechanical integrity for all new wells
and for all existing salt solution wells
pursuant to §146.08;
(3) The anticipated maximum pres-
sure and flow rate at which the per-
mittee will operate;
(4) The results of the formation test-
ing program;
(5) The actual injection procedures;
and
(6) The status of corrective action on
defective wells in the area of review.
(c) Prior to granting approval for the
plugging and abandonment of a Class
III well the Director shall consider the
following information:
(1) The type and number of plugs to
be used;
(2) The placement of each plug in-
cluding the elevation of the top and
bottom;
(3) The type, grade, and quantity of
cement to be used;
(4) The method of placement of the
plugs; and
(5) The procedure to be used to meet
the requirements of §146.10(c).
(Clean Water Act, Safe Drinking Water Act,
Clean Air Act, Resource Conservation and
Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927,
6974)
[45 FR 42500, June 24, 1980, as amended at 46
FR 43163, Aug. 27, 1981; 47 FR 5001, Feb. 3,
1982; 48 FR 14293, Apr. 1. 1983]
Subpart E—Criteria and Standards
Applicable to Class IV Injec-
tion Wells [Reserved]
Subpart F—Criteria and Standards
Applicable to Class V Injec-
tion Wells
§ 146.51 Applicability.
This subpart sets forth criteria and
standards for underground injection
control programs to regulate all injec-
tion not regulated in subparts B, C, D,
and E.
(a) Generally, wells covered by this
sutopart inject non-hazardous fluids
into or above formations that contain
underground sources of drinking water.
It includes all wells listed in §146.5(e)
but is not limited to those types of in-
jection wells.
(b) It also includes wells not covered
in Class IV that inject radioactive ma-
terial listed in 10 CFE part 20, appendix
B, table II, column 2.
[45 FR 42500, June 24, 1980, as amended at 47
FR 5001, Feb. 3. 1982]
Subpart G—Criteria and Standards
Applicable to Class I Haz-
ardous Waste Injection Wells
SOURCE: 53 FR 28148, July 26, 1988, unless
otherwise noted.
§ 146.61 Applicability
(a) This subpart establishes criteria
and standards for underground injec-
tion control programs to regulate Class
I hazardous waste injection wells. Un-
less otherwise noted this subpart sup-
plements the requirements of subpart
A and applies instead of subpart B to
Class I hazardous waste injection wells.
(b) Definitions,
Cone of influence means that area
around the well within which increased
injection zone pressures caused by in-
jection into the hazardous waste injec-
tion well would be sufficient to drive
fluids into an underground source of
drinking water (USDW).
Existing well means a Class I well
which was authorized prior to August
25, 1988, by an approved State program,
or an EPA-administered program or a
well which has become a Class I well as
a result of a change in the definition of
the injected waste which would render
the waste hazardous under §261.3 of
this part.
Injection interval means that part of
the injection zone in which the well is
screened, or in which the waste is oth-
erwise directly emplaced.
New well means any Class I hazardous
waste injection well which is not an ex-
isting well.
Transmissive fault or fracture is a fault
or fracture that has sufficient perme-
ability and vertical extent to allow
fluids to move between formations.
717
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§146.62
40 CFR Ch. I (7-1-04 Edition)
§ 146.62 Minimum criteria for siting,
(a) All Class I hazardous waste injec-
tion wells shall be sited such that they
inject into a formation that is beneath
the lowermost formation containing'
within one quarter mile of the well
bore an underground source of drinking
water.
(b) The siting of Class I hazardous
waste injection wells shall be limited
to areas that are geologically suitable.
The Director shall determine geologic
suitability based upon:
(1) An analysis of the structural and
stratigraphic geology, the
hydrogeology, and the seismicity of the
region;
(2) An analysis of the local geology
and hydrogeology of the well site, in-
cluding, at a minimum, detailed infor-
mation regarding stratigraphy, struc-
ture and rock properties, aquifer
hydrodynamics and mineral resources:
and
(3) A determination that the geology
of the area can be described con-
fidently and that limits of waste fate
and transport can be accurately pre-
dicted through the use of models.
(c) Class I hazardous waste injection
wells shall be sited such that:
(1) The injection zone has sufficient
permeability, porosity, thickness and
areal extent to prevent migration of
fluids into USDWs,
(2) The confining zone:
(i) Is laterally continuous and free of
transecting, transmissive faults or
fractures over an area sufficient to
prevenet the movement of fluids into a
USDW; and
(ii) Contains at least one formation
of sufficient thickness and with litlio-
logie and stress characteristics capable
of preventing vertical propagation of
fractures.
(d) The owner or operator shall dem-
onstrate to the satisfaction of the Di-
rector that:
(1) The confining zone is separated
from the base of the lowermost USDW
by at least one sequence of permeable
and less permeable strata that will pro-
vide an added layer of protection for
the USDW in the event of fluid move-
ment in an unlocated borehole or
transmissive fault; or
(2) Within the area of review, the
piezometric surface of the fluid in the
injection zone is less than the
piezometric surface of the lowermost
USDW, considering density effects, in-
jection pressures and any significant
pumping in the overlying USDW; or
(3) There is no USDW present.
(4) The Director may approve a site
which does not meet the requirements
in paragraphs (d) (1). (2), or (3) of this
section if the owner or operator can
demonstrate to the Director that be-
cause of the geology, nature of the
waste, or other considerations, aban-
doned boreholes or other conduits
would not cause endangerment of
USDWs.
§ 146.63 Area of review.
For the purposes of Class I hazardous
waste wells, this section shall apply to
the exclusion of § 146.6. The area of re-
view for Class I hazardous waste injec-
tion wells shall be a 2-mile radius
around the well bore. The Director may
specify a larger area of review based on
the calculated cone of influence of the
well,
§ 146,64 Corrective action for wells in
the area of review.
For the purposes of Class I hazardous
waste wells, this section shall apply to
the exclusion of §§144.55 and 146.07.
(a) The owner or operator of a Class
I hazardous waste well shall as part of
the permit application submit a plan to
the Director outlining the protocol
used to:
(1) Identify all wells penetrating the
confining zone or injection zone within
the area of review; and
(2) Determine whether wells are ade-
quately completed or plugged.
(b) The owner or operator of a Class
I hazardous waste well shall identify
the location of all wells within the area
of review that penetrate the injection
zone or the confining zone and shall
submit as required in §146.70(a):
(1) A tabulation of all wells within
the area of review that penetrate the
injection zone or the confining zone;
and
(2) A description of each well or type
of well and any records of its plugging
or completion.
(c) For wells that the Director deter-
mines are improperly plugged, com-
pleted, or abandoned, or for which
718
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Environmental Protection Agency
§146.65
plugging or completion information is
unavailable, the applicant shall also
submit a plan consisting of such steps
or modification as are necessary to pre-
vent movement of fluids into or be-
tween USDWs. Where the plan is ade-
quate, the Director shall incorporate it
into the permit as a condition. Where
the Director's review of an application
indicates that the permittee's plan is
inadequate (based at a minimum on the
factors in paragraph (e) of this sec-
tion), the Director shall:
(1) Require the applicant to revise
the plan;
(2) Prescribe a plan for corrective ac-
tion as a condition of the permit; or
(3) Deny the application,
(d) Requirements:
(1) Existing injection wells. Any per-
mit issued for an existing: Class I haz-
ardous waste injection well requiring
corrective action other than pressure
limitations shall include a compliance
schedule requiring any corrective ac-
tion accepted or prescribed under para-
graph (c) of this section. Any such
compliance schedule shall provide for
compliance no later than 2 years fol-
lowing" issuance of the permit and shall
require observance of appropriate pres-
sure limitations under paragraph (d)(3)
until all other corrective action meas-
ures have been implemented.
(2) New injection wells. No owner or
operator of a new Class I hazardous
waste injection well may begin injec-
tion until all corrective actions re-
quired under this section have been
taken.
(3) The Director may require pressure
limitations in lieu of plugging. If pres-
sure limitations are used in lieu of
plugging, the Director shall require as
a permit condition that injection pres-
sure be so limited that pressure in the
injection zone at the site of any im-
properly completed or abandoned well
within the area of review would not be
sufficient to drive fluids into or be-
tween USDWs. This pressure limitation
shall satisfy the corrective action re-
quirement. Alternatively, such injec-
tion pressure limitation may be made
part of a compliance schedule and may
be required to be maintained until all
other required corrective actions have
been implemented.
(e) In determining the adequacy of
corrective action proposed by the ap-
plicant under paragraph (c) of this sec-
tion and in determining the additional
steps needed to prevent fluid move-
ment into and between USDWs, the fol-
lowing criteria and factors shall be
considered by the Director:
(1) Nature and volume of injected
fluid;
(2) Nature of native fluids or byprod-
ucts of injection;
(3) Geology;
(4) Hydrology;
(5) History of the injection operation;
(6) Completion and plugging records;
(7) Closure procedures in effect at the
time the well was closed;
(8) Hydraulic connections with
USDWs;
(9) Reliability of the procedures used
to identify abandoned wells; and
(10) Any other factors which might
affect the movement of fluids into or
between USDWs.
1146,65 Construction requirements.
(a) General. All existing and new
Class I hazardous waste injection wells
shall be constructed and completed to:
(1) Prevent the movement of fluids
into or between USDWs or into any un-
authorized zones;
(2) Permit tie use of appropriate
testing devices and workover tools: and
(3) Permit continuous monitoring of
injection tubing and long string- casing
as required pursuant to §146.67(f).
(b) Compatibility, All well materials
must be compatible with fluids with
which the materials may be expected
to come into contact. A well shall be
deemed to have compatibility as long
as the materials used in the construc-
tion of the well meet or exceed stand-
ards developed for such materials by
the American Petroleum Institute, The
American Society for Testing Mate-
rials, or comparable standards accept-
able to the Director.
(c) Casing and Cementing of New Wells.
(1) Casing and cement used in the con-
struction of each newly drilled well
shall be designed for the life expect-
ancy of the well, including the post-
closure care period. The casing and ce-
menting program shall be designed to
prevent the movement of fluids into or
719
-------
§146.65
40 CFR Ch. I (7-1-04 Edition)
between USDWs, and to prevent poten-
tial leaks of fluids from the well. In de-
termining and specifying casing and
cementing requirements, the Director
shall consider the following informa-
tion as required by §146.70:
(i) Depth to the injection zone;
(ii) Injection pressure, external pres-
sure, internal pressure and axial load-
ing;
(iii) Hole size;
(iv) Size and grade of all casing
strings (well thickness, diameter,
nominal weight, length, joint specifica-
tion and construction material);
(v) Corrosiveness of injected fluid,
formation fluids and temperature;
(vi) Lithology of injection and con-
fining zones;
(vii) Type or grade of cement; and
(viii) Quantity and chemical com-
position of the injected fluid.
(2) One surface casing string shall, at
a minimum, extend Into the confining
bed below the lowest formation that
contains a USDW and be cemented by
circulating cement from the base of
the casing' to the surface, using a min-
imum of 120% of the calculated annual
volume. The Director may require
more than 120% when the geology or
other circumstances warrant it.
(3) At least one long string casing,
using a sufficient number of
centralizers, shall extend to the injec-
tion zone and shall be cemented by cir-
culating cement to the surface in one
or more stages:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure; and
(ii) In a quantity no less than 120% of
the calculated volume necessary to fill
the annular space. The Director may
require more than 120% when the geol-
ogy or other circumstances warrant it.
(4) Circulation of cement may be ac-
complished by staging. The Director
may approve an alternative method of
cementing in cases where the cement
cannot be reeirculated to the surface,
provided the owner or operator can
demonstrate by using logs that the ce-
ment is continuous and does not allow
fluid movement behind the well bore.
(5) Casings, including any casing con-
nections, must be rated to have suffi-
cient structural strength to withstand,
for the design life of the well:
(i) The maximum burst and collapse
pressures which may be experienced
during the construction, operation and
closure of the well; and
(Ii) The maximum tensile stress
which may be experienced at any point
along the length of the casing during
the construction, operation, and clo-
sure of the well.
(6) At a minimum, cement and ce-
ment additivies must be of sufficient
quality and quantity to maintain in-
tegrity over the design life of the well.
(d) Tubing and packer. (1) All Class I
hazardous waste injection wells shall
inject fluids through tubing with a
packer set at a point specified by the
Director.
(2) In determining and specifying re-
quirements for tubing and packer, the
following factors shall be considered:
(i) Depth of setting;
(ii) Characteristics of injection fluid
(chemical content, corrosiveness, tem-
perature and density);
(iii) Injection pressure;
(iv) Annular pressure;
(v) Bate (Intermittent or contin-
uous), temperature and volume of in-
jected fluid;
(vi) Size of casing; and
(vii) Tubing tensile, burst, and col-
lapse strengths.
(3) The Director may approve the use
of a fluid seal if he determines that the
following conditions are met:
(i) The operator demonstrates that
the seal will provide a level of protec-
tion comparable to a packer;
(ii) The operator demonstrates that
the staff is, and will remain, ade-
quately trained to operate and main-
tain the well and to identify and inter-
pret variations in parameters of con-
cern;
(iii) The permit contains specific lim-
itations on variations in annular pres-
sure and loss of annular fluid;
(iv) The design and construction of
the well allows continuous monitoring
of the annular pressure and mass bal-
ance of annular fluid; and
(v) A secondary system is used to
monitor the interface between the an-
nulus fluid and the injection fluid and
the permit contains requirements for
testing the system every three months
and recording the results.
720
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Environmental Protection Agency
§146.67
§ 146.66 Logging, sampling, and testing
prior to new well operation.
(a) During the drilling and construc-
tion of a new Class I hazardous waste
injection well, appropriate logs and
tests shall be run to determine or
verify the depth, thickness, porosity,
permeability, and rock type of, and the
salinity of any entrained fluids in, all
relevant geologic units to assure eon-
formanee with performance standards
in §146.65, and to establish accurate
baseline data against which future
measurements may be compared. A de-
scriptive report interpreting results of
such logs and tests shall be prepared by
a knowledgeable log analyst and sub-
mitted to the Director. At a minimum,
such logs and tests shall include:
(1) Deviation checks during drilling
on all holes constructed by drilling a
pilot hole which are enlarged by ream-
ing or another method. Such checks
shall be at sufficiently frequent inter-
vals to determine the location of the
borehole and to assure that vertical
avenues for fluid movement in the
form of diverging holes are not created
during drilling; and
(2) Such other logs and tests as may
be needed after taking into account the
availability of similar data in the area
of the drilling site, the construction
plan, and the need for additional infor-
mation that may arise from time to
time as the construction of the well
progresses. At a minimum, the fol-
lowing logs shall be required in the fol-
lowing situations:
(i) Upon installation of the surface
casing:
(A) Resistivity, spontaneous poten-
tial, and oaliper logs before the casing
is installed; and
(B) A cement bond and variable den-
sity log, and a temperature log after
the casing is set and cemented.
(ii) Upon installation of the long
string casing:
(A) Resistivity, spontaneous poten-
tial, porosity, caliper, gamma ray, and
fracture finder logs before the casing is
installed; and
(B) A cement bond and variable den-
sity log, and a temperature log after
the casing is set and cemented.
(iii) The Director may allow the use
of an alternative to the above logs
when an alternative will provide equiv-
alent or better information; and
(3) A mechanical integrity test con-
sisting of:
(i) A pressure test with liquid or gas;
(ii) A radioactive tracer survey;
(iii) A temperature or noise log;
(iv) A casing inspection log, if re-
quired by the Director; and
(v) Any other test required by the Di-
rector,
(b) Whole cores or sidewall cores of
the confining and injection zones and
formation fluid samples from the injec-
tion zone shall be taken. The Director
may accept cores from nearby wells if
the owner or operator can demonstrate
that core retrieval is not possible and
that such cores are representative of
conditions at the well. The Director
may require the owner or operator to
core other formations in the borehole.
(c) The fluid temperature, pH, con-
ductivity, pressure and the static fluid
level of the injection zone must be re-
corded.
(d) At a minimum, the following in-
formation concerning the injection and
confining zones shall be determined or
calculated for Class I hazardous waste
injection wells:
(1) Fracture pressure;
(2) Other physical and chemical char-
acteristics of the injection and con-
fining zones; and
(3) Physical and chemical character-
istics of the formation fluids in tile in-
jection zone.
(e) Upon completion, but prior to op-
eration, the owner or operator shall
conduct the following tests to verify
hydrogeologic characteristics of the in-
jection zone:
(1) A pump test; or
(2) Injectivity tests,
(f) The Director shall have the oppor-
tunity to witness all logging and test-
ing by this subpart. The owner or oper-
ator shall submit a schedule of such ac-
tivities to the Director 30 days prior to
conducting the first test.
i 146.67 Operating requirements.
(a) Except during stimulation, the
owner or operator shall assure that in-
jection pressure at the wellhead does
not exceed a maximum which shall be
calculated so as to assure that the
pressure in the injection zone during
721
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§146.67
40 CFR Ch. I (7-1-04 Edition)
injection does not initiate new frac-
tures or propagate existing fractures in
the injection zone. The owner or oper-
ator shall assure that the injection
pressure does not initiate fractures or
propagate existing fractures in the con-
fining zone, nor cause the movement of
injection or formation fluids into a
USDW.
(b) Injection between the outermost
casing protecting USDWs and the well
bore is prohibited.
(c) The owner or operator shall main-
tain an annulus pressure that exceeds
the operating injection pressure, unless
the Director determines that such a re-
quirement might harm the integrity of
the well. The fluid in the annulus shall
be noneorrosive, or shall contain a cor-
rosion inhibitor.
(d) The owner or operator shall main-
tain mechanical integrity of the injec-
tion well at all times.
(e) Permit requirements for owners
or operators of hazardous waste wells
which inject wastes which have the po-
tential to react with the injection for-
mation to generate gases shall include:
(1) Conditions limiting the tempera-
ture, pH or acidity of the injected
waste; and
(2) Procedures necessary to assure
that pressure imbalances which might
cause a backflow or blowout do not
occur.
(f) The owner or operator shall in-
stall and use continuous recording de-
vices to monitor: the injection pres-
sure; the flow rate, volume, and tem-
perature of injected fluids; and the
pressure on the annulus between the
tubing and the long string casing, and
shall install and use:
(1) Automatic alarm and automatic
shut-off systems, designed to sound and
shut-in the well when pressures and
flow rates or other parameters ap-
proved by the Director exceed a range
and/or gradient specified in the permit;
or
(2) Automatic alarms, designed to
sound when the pressures and flow
rates or other parameters approved by
the Director exceed a rate and/or gra-
dient specified in the permit, in cases
where the owner or operator certifies
that a trained operator will be on-site
at all times when the well is operating.
(g) If an automatic alarm or shut-
down is triggered, the owner or oper-
ator shall immediately investigate and
identify as expeditiously as possible
the cause of the alarm or shutoff. If,
upon such investigation, the well ap-
pears to be lacking mechanical integ-
rity, or if monitoring required under
paragraph (f) of this section otherwise
indicates that the well may be lacking
mechanical integrity, the owner or op-
erator shall;
(1) Cease injection of waste fluids un-
less authorized by the Director to con-
tinue or resume injection.
(2) Take all necessary steps to deter-
mine the presence or absence of a leak;
and
(3) Notify the Director within 24
hours after the alarm or shutdown.
(h) If a loss of mechanical integrity is
discovered pursuant to paragraph (g) of
this section or during periodic mechan-
ical integrity testing, the owner or op-
erator shall:
(1) Immediately cease injection of
waste fluids;
(2) Take all steps reasonably nec-
essary to determine whether there may
have been a release of hazardous wastes
or hazardous waste constituents into
any unauthorized zone;
(3) Notify the Director within 24
hours after loss of mechanical integ-
rity is discovered;
(4) Notify the Director when injec-
tion can be expected to resume; and
(5) Restore and demonstrate mechan-
ical integrity to the satisfaction of the
Director prior to resuming injection of
waste fluids.
(i) Whenever the owner or operator
obtains evidence that there may have
been a release of injected wastes into
an unauthorized zone:
(1) The owner or operator shall im-
mediately case injection of waste
fluids, and:
(i) Notify the Director within 24
hours of obtaining such evidence;
(ii) Take all necessary steps to iden-
tify and characterize the extent of any
release;
(iiii Comply with any remediation
plan specified by the Director;
(iv) Implement any remediation plan
approved by the Director; and
(v) Where such release is into a
USDW currently serving as a water
722
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Environmental Protection Agency
§146.68
supply, place a notice In a newspaper of
general circulation,
(2) The Director may allow the oper-
ator to resume injection prior to com-
pleting cleanup action if the owner or
operator demonstrates that the injec-
tion operation will not endanger
USDWs.
(j) The owner or operator shall notify
the Director and obtain his approval
prior to conducting any well workover.
§ 146.68 Testing and monitoring re-
quirements.
Testing and monitoring requirements
shall at a minimum include:
(a) Monitoring of the injected wastes,
(1) The owner or operator shall develop
and follow an approved written waste
analysis plan that describes the proce-
dures to be carried out to obtain a de-
tailed chemical and physical analysis
of a representative sample of the
waste, including the quality assurance
procedures used. At a minimum, the
plan shall specify:
(i) The paramenters for which the
waste will be analyzed and the ration-
ale for the selection of these param-
eters;
(ii) The test methods that will be
used to test for these parameters; and
(ill) The sampling method that will
be used to obtain a representative sam-
ple of the waste to be analyzed.
(2) The owner or operator shall re-
peat the analysis of the injected wastes
as described in the waste analysis plan
at frequencies specified in the waste
analysis plan and when process or oper-
ating changes occur that may signifi-
cantly alter the characteristics of the
waste stream.
(3) The owner or operator shall con-
duct continuous or periodic monitoring
of selected parameters as required by
the Director.
(4) The owner or operator shall as-
sure that the plan remains accurate
and the analyses remain representa-
tive.
(b) Hydrogeologic compatibility de-
termination. The owner or operator
shall submit information dem-
onstrating to the satisfaction of the
Director that the waste stream and its
anticipated reaction products will not
alter the permeability, thickness or
other relevant characteristics of the
confining or injection zones such that
they would no longer meet the require-
ments specified in § 146.62.
(c) Compatibility of well materials.
(1) The owner or operator shall dem-
onstrate that the waste stream will be
compatible with the well materials
with which the waste is expected to
come into contact, and submit to the
Director a description of the method-
ology used to make that determina-
tion. Oompatibility for purposes of this
requirement is established if contact
with injected fluids will not cause the
well materials to fail to satisfy any de-
sign requirement imposed under
§146.65(b).
(2) The Director shall require contin-
uous corrosion monitoring of the con-
struction materials used in the well for
wells injecting corrosive waste, and
may require such monitoring for other
waste, by:
(i) Placing coupons of the well con-
struction materials in contact with the
waste stream; or
(ii) Routing the waste stream
through a loop constructed with the
material used in the well; or
(iii) Using an alternative method ap-
proved by the Director.
(3) If a corrosion monitoring program
is required:
(i) The test shall use materials iden-
tical to those used in the construction
of the well, and such materials must be
continuously exposed to the operating
pressures and temperatures (measured
at the well head) and flow rates of the
injection operation; and
(ii) The owner or operator shall mon-
itor the materials for loss of mass,
thickness, cracking, pitting and other
signs of corrosion on a quarterly basis
to ensure that the well components
meet the minimum standards for mate-
rial strength and performance set forth
in§148.65(b).
(d) Periodic mechanical integrity test-
ing. In fulfilling the requirements of
§ 146.8, the owner or operator of a Class
I hazardous waste injection well shall
conduct the mechanical integrity test-
ing as follows:
(1) The long string casing, injection
tube, and annular seal shall be tested
by means of an approved pressure test
with a liquid or gas annually and when-
ever there has been a well workover;
723
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§146.69
40 CFRCh. I (7-1-04 Edition)
(2) The bottom-hole cement shall be
tested by means of an approved radio-
active tracer survey annually;
(3) An approved temperature, noise,
or other approved log shall be run at
least once every five years to test for
movement of fluid along the borehole.
The Director may require such tests
whenever the well is worked over;
(4) Casing inspection logs shall be run
whenever the owner or operator con-
ducts a workover in which the injec-
tion string Is pulled, unless the Direc-
tor waives this requirement due to well
construction or other factors which
limit the test's reliability, or based
upon the satisfactory results of a cas-
ing inspection log run within the pre-
vious five years. The Director may re-
quire that a casing inspection log be
run every five years, if he has reason to
believe that the integrity of the long
string casing of the well may be ad-
versely affected by naturally-occurring
or man-made events;
(5) Any other test approved by the
Director in accordance with the proce-
dures in §146.8(d) may also be used,
(e) Ambient monitoring. (1) Based on a
site-specific assessment of the poten-
tial for fluid movement from the well
or injection zone, and on the potential
value of monitoring wells to detect
such movement, the Director shall re-
quire the owner or operator to develop
a monitoring program. At a minimum,
the Director shall require monitoring
of the pressure buildup in the injection
zone annually, including at a min-
imum, a shut down of the well for a
time sufficient to conduct a valid ob-
servation of the pressure fall-off curve.
(2) When prescribing a monitoring
system the Director may also require:
(i) Continuous monitoring for pres-
sure changes in the first aquifer over-
lying the confining zone. When such a
well is installed, the owner or operator
shall, on a quarterly basis, sample the
aquifer and analyze for constituents
specified by the Director;
(ii) The use of indirect, geophysical
techniques to determine the position of
the waste front, the water quality in a
formation designated by the Director,
or to provide other site specific data;
(ill) Periodic monitoring" of the
ground water quality in the first aqui-
fer overlying the injection zone;
(iv) Periodic monitoring of the
ground water quality in the lowermost
USDW; and
(v) Any additional monitoring nec-
essary to determine whether fluids are
moving into or between USDWs.
(f) The Director may require seis-
micity monitoring when he has reason
to believe that the injection activity
may have the capacity to cause seismic
disturbances.
[53 PR 28148, July 26, 1988, as amended at 57
FR 46294, Oct. 7. 1992]
§ 146.69 Reporting requirements.
Reporting requirements shall, at a
minimum, include:
(a) Quarterly reports to the Director
containing:
(1) The maximum injection pressure;
(2) A description of any event that
exceeds operating parameters for annu-
lus pressure or injection pressure as
specified in the permit;
(3) A description of any event which
triggers an alarm or shutdown device
required pursuant to §146.67(f) and the
response taken;
(4) The total volume of fluid injected;
(5) Any change in the annular fluid
volume;
(6) The physical, chemical and other
relevant characteristics of injected
fluids; and
(7) The results of monitoring pre-
scribed tinder § 146.68.
(b) Reporting, within 30 days or with
the next quarterly report whichever
comes later, the results of:
(1) Periodic tests of mechanical in-
tegrity;
(2) Any other test of the injection
well conducted by the permittee if re-
quired by the Director: and
(3) Any well workover,
1146.70 Information to be evaluated
by the Director.
This section sets forth the informa-
tion which must be evaluated by the
Director in authorizing Class I haz-
ardous waste injection wells. For a new
Class I hazardous waste injection well,
the owner or operator shall submit all
the information listed below as part of
the permit application. For an existing
or converted Class I hazardous waste
injection well, the owner or operator
shall submit all information listed
724
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Environmental Protection Agency
§146.70
below as part of the permit application
except for those items of information
which are current, accurate, and avail-
able in the existing permit file. For
both existing and new Class I haz-
ardous waste injection wells, certain
maps, cross-sections, tabulations of
wells within the area of review and
other data may be included in the ap-
plication by reference provided they
are current and readily available to the
Director (for example, in the permit-
ting agency's files) and sufficiently
identifiable to be retrieved. In cases
where EPA issues the permit, all the
information in this section must be
submitted to the Administrator or his
designee.
(a) Prior to the issuance of a permit
for an existing Class I hazardous waste
injection well to operate or the con-
struction or conversion of a new Class
I hazardous waste injection well, the
Director shall review the following to
assure that the requirements of this
part and part 144 are met:
(1) Information required in §144.31;
(2) A map showing the injection well
for which a permit is sought and the
applicable area of review. Within the
area of review, the map must show the
number or name and location of all
producing wells, injection wells, aban-
doned wells, dry holes, surface bodies
of water, springs, mines (surface and
subsurface), quarries, water wells and
other pertinent surface features, in-
cluding residences and roads. The map
should also show faults, if known or
suspected:
(3) A tabulation of all wells within
the area of review which penetrate the
proposed injection zone or confining
zone. Such data shall include a descrip-
tion of each well's type, construction,
date drilled, location, depth, record of
plugging and/or completion and any ad-
ditional information the Director may
require;
(4) The protocol followed to identify,
locate and ascertain the condition of
abandoned wells within the area of re-
view which penetrate the injection or
the confining zones;
(5) Maps and cross-sections indi-
cating the general vertical and lateral
limits of all underground sources of
drinking water within the area of re-
view, their position relative to the in-
jection formation and the direction of
water movement, where known, in each
underground source of drinking water
which may be affected by the proposed
injection;
(6) Maps and cross-sections detailing
the geologic structure of the local area;
(7) Maps and cross-sections illus-
trating the regional geologic setting;
(8) Proposed operating data;
(i) Average and maximum daily rate
and volume of the fluid to be injected;
and
(ii) Average and maximum injection
pressure;
(9) Proposed formation testing pro-
gram to obtain an analysis of the
chemical, physical and radiological
characteristics of and other informa-
tion on the injection formation and the
confining zone;
(10) Proposed stimulation program;
(11) Proposed injection procedure;
(12) Schematic or other appropriate
drawings of the surface and subsurface
construction details of the well;
(13) Contingency plans to cope with
all shut-ins or well failures so as to
prevent migration of fluids into any
USDW;
(14) Plans (including maps) for meet-
ing monitoring requirements of § 146.68;
(15) For wells within the area of re-
view which penetrate the injection
zone or the confining zone but are not
properly completed or plugged, the cor-
rective action to be taken under
§146.64;
(16) Construction procedures includ-
ing a cementing" and casing program,
well materials specifications and their
life expectancy, logging procedures, de-
viation checks, and a drilling, testing
and coring program; and
(17) A demonstration pursuant to
part 144, subpart F, that the applicant
has the resources necessary to close,
plug or abandon the well and for post-
closure care.
(b) Prior to the Director's granting
approval for the operation of a Class I
hazardous waste injection well, the
owner or operator shall submit and the
Director shall review the following in-
formation, which shall be included in
the completion report:
(1) All available logging and testing
program data on the well;
725
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§146.71
40 CFR Ch. I (7-1-04 Edition)
(2) A demonstration of mechanical
integrity pursuant to §146.68;
(3) The anticipated maximum pres-
sure and flow rate at which the per-
mittee will operate:
(4) The results of the injection zone
and confining zone testing program as
required in §146.70(a)(9):
(5) The actual injection procedure;
(6) The compatibility of injected
waste with fluids in the injection zone
and minerals in both the injection zone
and the confining zone and with the
materials used to construct the well;
(7) The calculated area of review
based on data obtained during logging
and testing of the well and the forma-
tion, and where necessary revisions to
the information submitted under
§146.70(a) (2) and (3).
(8) The status of corrective action on
wells identified in §146.70(a)(15).
fc) Prior to granting approval for the
plugging and abandonment (i.e., clo-
sure) of a Class I hazardous waste in-
jection well, the Director shall review
the information required in
§§146.71(a)(4) and 146.72(a).
(d) Any permit issued for a Class I
hazardous waste injection well for dis-
posal on the premises where the waste
is generated shall contain a certifi-
cation by the owner or operator that:
(1) The generator of the hazardous
waste has a program to reduce the vol-
ume or quantity and toxicity of such
waste to the degree determined by the
generator to be economically prac-
ticable; and
(2) Injection of the waste is that
practicable method of disposal cur-
rently available to the generator which
minimizes the present and future
threat to human health and the envi-
ronment.
§ 146.71 Closure.
(a) Closure Plan. The owner or oper-
ator of a Class I hazardous waste injec-
tion well shall prepare, maintain, and
comply with a plan for closure of the
well that meets the requirements of
paragraph (d) of this section and is ac-
ceptable to the Director. The obliga-
tion to implement the closure plan sur-
vives the termination of a permit or
the cessation of injection activities.
The requirement to maintain and
implement an approved plan is directly
enforceable regardless of whether the
requirement is a condition of the per-
mit.
(1) The owner or operator shall sub-
mit the plan as a part of the permit
application and, upon approval by the
Director, such plan shall be a condition
of any permit issued.
(2) The owner or operator shall sub-
mit any proposed significant revision
to the method of closure reflected in
the plan for approval by the Director
no later than the date on which notice
of closure is required to be submitted
to the Director under paragraph (b) of
this section.
(3) The plan shall assure financial re-
sponsibility as required in §144.52(a)(7).
(4) The plan shall include the fol-
lowing information:
(1) The type and number of plugs to
be used;
(ii) The placement of each plug in-
cluding the elevation of the top and
bottom of each plug;
(ill) The type and grade and quantity
of material to be used in plugging;
(iv) The method of placement of the
plugs;
(v) Any proposed test or measure to
be made;
(vi) The amount, size, and location
(by depth) of casing and any other ma-
terials to be left in the well;
(vii) The method and location where
casing is to be parted, if applicable;
(viii) The procedure to be used to
meet the requirements of paragraph
(d)(5) of this section;
(ix) The estimated cost of closure;
and
(x) Any proposed test or measure to
be made.
(5) The Director may modify a clo-
sure plan following the procedures of
§124,5.
(6) An owner or operator of a Class I
hazardous waste injection well who
ceases injection temporarily, may keep
the well open provided he:
(i) Has received authorization from
the Director; and
(ii) Has described actions or proce-
dures, satisfactory to the Director,
that the owner or operator will take to
ensure that the well will not endanger
USDWs during the period of temporary
disuse. These actions and procedures
726
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Environmental Protection Agency
§146,72
shall include compliance with the tech-
nical requirements applicable to active
injection wells unless waived by the Di-
rector,
(7) The owner or operator of a well
that has ceased operations for more
than two years shall notify the Direc-
tor 30 days prior to resuming operation
of the well.
(b) Notice of intent to close. The owner
or operator shall notify the Director at
least 60 days before closure of a well,
At the discretion of the Director, a
shorter notice period may be allowed.
(c) Closure report. Within 60 days after
closure or at the time of the next quar-
terly report (whichever is less) the
owner or operator shall submit a clo-
sure report to the Director. If the quar-
terly report is due less than 15 days
after completion of closure, then the
report shall be submitted within 60
days after closure. The report shall be
certified as accurate by the owner or
operator and by the person who per-
formed the closure operation (if other
than the owner or operator). Such re-
port shall consist of either:
(1) A statement that the well was
closed in accordance with the closure
plan previously submitted and ap-
proved by the Director; or
(2) Where actual closure differed from
the plan previously submitted, a writ-
ten statement specifying the dif-
ferences between the previous plan and
the actual closure.
I'd) Standards for well closure. (1) Prior
to closing the well, the owner or oper-
ator shall observe and record the pres-
sure decay for a time specified by the
Director. The Director shall analyze
the pressure decay and the transient
pressure observations conducted pursu-
ant to §146.68(eXlXi) and determine
whether the injection activity has con-
formed with predicted values,
(2) Prior to well closure, appropriate
mechanical integrity testing shall be
conducted to ensure the integrity of
that portion of the long string casing
and cement that will be left in the
ground after closure. Testing- methods
may include:
(ii Pressure tests with liquid or gas:
(11) Radioactive tracer surveys;
(iii) Noise, temperature, pipe evalua-
tion, or cement bond logs; and
(iv) Any other test required by the
Director.
(3) Prior to well closure, the well
shall be flushed with a buffer fluid.
(4) Upon closure, a Class I hazardous
waste well shall be plugged with ce-
ment in a manner that will not allow
the movement of fluids into or between
USDWs.
(5) Placement of the cement plugs
shall be accomplished by one of the fol-
lowing:
(i) The Balance Method;
(ii) The Dump Bailer Method:
(iii) The Two-Plug Method: or
(iv) An alternate method, approved
by the Director, that will reliably pro-
vide a comparable level of protection.
(6) Bach plug used shall be appro-
priately tagged and tested for seal and
stability before closure is completed.
(7) The well to be closed shall be in a
state of static equilibrium with the
mud weight equalized top to bottom.
either by circulating the mud in the
well at least once or by a comparable
method prescribed by the Director,
prior to the placement of the cement
plug-(s).
§ 146.72 Post-closure care.
(a) The owner or operator of a Class
I hazardous waste well shall prepare,
maintain, and comply with a plan for
post-closui'e care that meets the re-
quirements of paragraph (b) of this sec-
tion and is acceptable to the Director.
The obligation to implement the post-
closure plan survives the termination
of a permit or the cessation of injec-
tion activities. The requirement to
maintain an approved plan is directly
enforceable regardless of whether the
requirement is a condition of the per-
mit.
(1) The owner or operator shall sub-
mit the plan as a part of the permit ap-
plication and, upon approval by the Di-
rector, such plan shall be a condition of
any permit issued.
(2) The owner or operator shall sub-
mit any proposed significant revision
to the plan as appropriate over the life
of the well, but no later than the date
of the closure report required under
§146.71(c).
(3) The plan shall assure financial re-
sponsibility as required in § 146.73,
72?
203-160 D-24
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§146.73
40 CFR Ch. I (7-1-04 Edition)
(4) The plan shall include the fol-
lowing information:
(i) The pressure in the injection zone
before injection began;
(ii) The anticipated pressure in the
injection zone at the time of closure;
(iii) The predicted time until pres-
sure in the injection zone decays to the
point that the well's cone of influence
no longer intersects the base of the
lowermost USDW;
(iv) Predicted position of the waste
front at closure;
(v) The status of any cleanups re-
quired under § 146.64; and
(vi) The estimated cost of proposed
post-closure care.
(5) At the request of the owner or op-
erator, or on his own initiative, the Di-
rector may modify the post-closure
plan after submission of the closure re-
port following the procedures in §124.5.
(b) The owner or operator shall:
(1) Continue and complete any clean-
up action required under §146.64, if ap-
plicable;
(2) Continue to conduct any ground-
water monitoring required under the
permit until pressure in the injection
zone decays to the point that the well's
cone of influence no longer intersects
the base of the lowermost USDW. The
Director may extend the period of post-
closure monitoring if he determines
that the well may endanger a USDW.
(3) Submit a survey plat to the local
zoning authority designated by the Di-
rector. The plat shall indicate the loca-
tion of the well relative to perma-
nently surveyed benchmarks. A copy of
the plat shall be submitted to the Re-
gional Administrator of the appro-
priate EPA Regional Office.
(4) Provide appropriate notification
and information to such State and
local authorities as have cognizance
over drilling activities to enable such
State and local authorities to impose
appropriate conditions on subsequent
drilling activities that may penetrate
the well's confining or injection zone.
(5) Retain, for a period of three years
following well closure, records reflect-
ing the nature, composition and vol-
ume of all injected fluids. The Director
shall require the owner or operator to
deliver the records to the Director at
the conclusion of the retention period,
and the records shall thereafter be re-
tained at a location designated by the
Director for that purpose.
(c) Each owner of a Class I hazardous
waste injection well, and the owner of
the surface or subsurface property on
or in which a Class I hazardous waste
injection well is located, must record a
notation on the deed to the facility
property or on some other instrument
which is normally examined during
title search that will in perpetuity pro-
vide any potential purchaser of the
property the following information:
(1) The fact that land has been used
to manage hazardous waste;
(2) The name of the State agency or
local authority with which the plat
was filed, as well as the address of the
Regional Environmental Protection
Agency Office to which it was sub-
mitted;
(3) The type and volume of waste in-
jected, the injection interval or inter-
vals into which it was injected, and the
period over which injection occurred.
§ 146.73 Financial responsibility for
post-closure care.
The owner or operator shall dem-
onstrate and maintain financial re-
sponsibility for post-closure by using a
trust fund, surety bond, letter of cred-
it, financial test, insurance or cor-
porate guarantee that meets the speci-
fications for the mechanisms and in-
struments revised as appropriate to
cover closure and post-closure care in
40 OPR part 144, subpart P. The amount
of the funds available shall be no less
than the amount identified in
§146.72(a)(4)(vi). The obligation to
maintain financial responsibility for
post-closure care survives the termi-
nation of a permit or the cessation of
injection. The requirement to maintain
financial responsibility is enforceable
regardless of whether the requirement
is a condition of the permit.
PART 147—STATE UNDERGROUND
INJECTION CONTROL PROGRAMS
Subpart A—General Provisions
Sec.
147,1 Purpose and scope.
147.2 Severability of provisions.
728
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Environmental Protection Agency
Pt. 147
Subpart B—Alabama
147,50 State-administered program—Class II
wells.
147.51 State-administered program—Class I.
Ill, IV, and V wells.
147.52 State-administered program—Hy-
draulic Fracturing' of Coal Beds.
147.60 EPA-administered program—Indian
lands.
Subpart C—Alaska
147,100 State-administered program—Class
II wells.
147.101 EPA-administered program.
147.102 Aquifer exemptions.
147.103 Existing1 Class I. II (except enhanced
recovery and hydrocarbon storage) and
III wells authorized by rule.
147.104 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
Subpart D—Arizona
147.150 State-administered program. [Re-
served]
147,151 EPA-administered program,
147,152 Aquifer exemptions. [Reserved]
Subpart E—Arkansas
147.200 State-administered program—Class
I. III. IV, and V wells.
147.201 State-administered program—Class
II wells. [Reserved]
147.205 EPA-administered program—Indian
lands.
Subpart F—California
147.250 State-administered program—Class
II wells.
147.251 EPA-administered program—Class I.
Ill, IV, and V wells and Indian lands.
147.252 Aquifer exemptions. [Reserved]
147.253 Existing Class I, II (except enhanced
recovery and hydrocarbon storage) and
III wells authorized by rule.
Subpart G—Colorado
147.300 State-administered program—Class
II wells.
147.301 EPA-administered program—Class I,
III, IV. V wells and Indian lands.
147.302 Aquifer exemptions.
147,303 Existing Class I, II (except enhanced
recovery and hydrocarbon storage) and
III wells authorized by rule.
147.304 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.305 Requirements for all wells.
Subpart H—Connecticut
147.350 State-administered program.
147.351-147.352 [Reserved]
147.353 EPA-administered program—Indian
lands.
147.354-147.359 [Reserved]
Subpart I—Delaware
147.400 State-administered program.
147.40.1-147.402 [Reserved]
147.403 EPA-administered program—Indian
lands.
147.404-147.449 [Reserved]
Subpart J—District of Columbia
147.450 State-administered program. [Re-
served]
147.451 EPA-administered program.
147.452 Aquifer exemptions. [Reserved]
Subpart K—Florida
147.500 Stat9-administered program—Class
I, III, IV. and V wells.
147.501 EPA-ad?ninistered program—Class II
wells and Indian lands.
147.502 Aquifer exemptions. [Reserved]
147.503 Existing Class II (except enhanced
recovery and hydrocarbon storage) wells
authorized by rule,
147.504 Existing' Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
Subpart L—Georgia
147.550 State-administered program,
147.551-147.552 (Reserved]
147.553 EPA-administered program—Indian
lands.
147.554-147.559 [Reserved]
Subpart M—Hawaii
147.600 State-administered program. [Re-
served]
147.601 EPA-administered program.
Subpart N—Idaho
147.650 State-administrative program—
Class I, II. III. IV. and V wells.
147.651 EPA-administered program—Indian
lands,
147.652 Aquifer exemptions. [Reserved]
Subpart O—Illinois
147.700 State-administered program—Class
I, III, IV. and V wells.
147.701 State-administered program—Class
II wells,
147.703 EPA-administered program—Indian
lands.
Subpart P—Indiana
147.750 State-administered program—Class
II wells.
729
-------
Pt, 147
40 CFR Ch. 1 (7-1-04 Edition)
147,751 EPA-admirdstered program.
147,752 Aquifer exemptions, [Reserved]
147,753 Existing Class I and III wells author-
ized by rule,
Subpart Q—Iowa
147,800 State-administered program. [Re-
served]
147,801 EPA-administered program.
147.802 Aquifer exemptions. [Reserved]
Subpart R—Kansas
147,850 State-administered program—Class
I, III, IV and V wells.
147,851 State-administered program—Class
II wells,
147.852~147.859 [Reserved]
147.860 EPA-administered program—Indian
lands.
Subpart S— Kentucky
147.900 State-administered program. [Re-
served]
147.901 BPA-administered program,
147,902 Aquifer exemptions. [Reserved]
147.903 Existing Class I, II (except enhanced
recovery and hydrocarbon storage) and
III wells authorized by rule.
147.904 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.905 Requirements for all wells—area of
review,
Subpart T—Louisiana
147.950 State-administered program.
147.951 EPA-administered program—Indian
lands.
Subpart U—Maine
147.1000 State-administered program,
147.1001 BPA-administered program—Indian
lands.
Subpart V—Maryland
147,1050 State-administered program—Class
I, II, III, IV, and V wells.
147.1051-147.1052 [Reserved]
147.1053 EPA-administered program—Indian
lands.
147.1054-147.1099 [Reserved]
Subpart W—Massachusetts
147.1100 State-administered program.
147.1101 BPA-administered program—Indian
lands.
Subpart X—Michigan
147.1150 State-administered program. [Re-
served]
147.1151 BPA-administered program.
147.1152 Aquifer exemptions, [Reserved]
147.1153 Existing Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147.1154 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.1155 Requirements for all wells.
Subpart Y—Minnesota
147.1200 State-administered program. [Re-
served]
147.1201 BPA-administered program,
147.1202 Aquifer exemptions. [Reserved]
147.1210 Requirements for Indian lands,
Subpart Z—Mississippi
147,1250 State-administered program—Class
I, III, IV, and V wells.
147.1251 State-administered program—Class
II wells.
147.1252 EPA-administered program—Indian
lands.
Subpart AA—Missouri
147.1300 State-administered program,
147,1301 State-administered program—Class
I, III, IV, and V wells.
147.1302 Aquifer exemptions. [Reserved]
147.1303 EPA-administered program—Indian
lands,
Subpart BB—Montana
147,1350 State-administered programs—
Class II wells
147,1351 EPA-administered program.
147.1352 Aquifer exemptions.
147.1353 Existing Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147,1354 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.1355 Requirements for all wells.
APPENDIX A TO SUBPART BB OF PART 147—
STATE REQUIREMENTS INCORPORATED BY
REFERENCE IN SUBPART BB OP PART 147
OF THE CODE OF FEDERAL REGULATIONS,
Subpart CC—Nebraska
147.1400 State-administered program—Class
II wells.
147.1401 State-administered program—Class
I, in, IV, and V wells.
147.1402 Aquifer exemptions. [Reserved]
147.1403 EPA-administered program—Indian
lands.
Subpart DD—Nevada
147,1450 State-administered program.
147,1451 EPA-administered program—Indian
lands.
730
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Environmental Protection Agency
Pt, 147
147,1452 Aquifer exemptions. [Reserved]
147.1453 Existing Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147.1454 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
Subparf EE—New Hampshire
147,1500 State-administered program.
147,1501 EPA-administered program—Indian
lands.
Subpart FF—New Jersey
147.1550 State-administered program.
147.1551 EPA-administered program—Indian
lands.
Subpart GG—New Mexico
147,1600 State-administered program—Class
II wells.
147,1601 State-administered prog'rarn—Class
I, III, IV and V wells.
147.1603 EPA-administered program—Indian
lands.
Subpart HH—New York
147.1650 State-administered program, [Re-
served]
147.1651 EPA-administered program.
147.1652 Aquifer exemptions.
147.1653 Existing Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147.1654 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147,1655 Requirements for wells authorized
by permit.
Subpart II—North Carolina
147.1700 State-administered program.
147.1701-147.1702 [Reserved]
147.1703 EPA-administered program—Indian
lands.
147.1704-147.1749 [Reserved]
Subpart JJ—North Dakota
147.1750 State-administered program—Class
II wells.
147,1751 State-administered program—Class
I, III, IV and V wells.
147.1752 EPA-administered program—Indian
lands.
Subpart KK—Ohio
147.1800 State-administered program—Class
II wells.
147.1801 State-administered program—Class
I, III, IV and V wells.
147.1802 Aquifer exemptions. [Reserved]
147.1803 Existing Class I and III wells au-
thorized by rule—maximum injection
pressure.
147.1805 EPA-administered program—Indian
lands.
Subpart LL—Oklahoma
147.1850 State-administered program—Class
I, III, IV and V wells.
147.1851 State-administered program—Class
II wells.
147.1852 EPA-administered program—Indian
lands.
Subpart MM—Oregon
147.1900 State-administered program,
147.1901 EPA-administered program—Indian
lands.
Subpart NN—Pennsylvania
147.1950 State-administered program. [Re-
served]
147.1951 EPA-administered program.
147.1952 Aquifer exemptions.
147.1953 Existing Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147.1954 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.1955 Requirements for wells authorized
by permit.
Subpart OO—Rhode Island
147.2000 State-administered program—Class
I, II, III, IV, and V wells.
147.2001 EPA-administered program—Indian
lands.
Subpart PP—South Carolina
147.2050 State-administered program.
147.2051 EPA-administered program—Indian
lands.
Subpart QQ—South Dakota
147.2100 State-administered program—Class
II wells.
147.2101 EPA-administered program—Class
I, III, IV and V wells and all wells on In-
dian lands.
147.2102 Aquifer exemptions.
147.2103 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule,
147,2104 Requirements for all wells.
Subpart RR—Tennessee
147.2150 State-administered program. [Re-
served]
147.2151 EPA-administered program,
147.2152 Aquifer exemptions. [Reserved]
731
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Pf. 147
40 CFR Ch. I (7-1-04 Edition)
147.2153 Existing- Class I, II (except en-
hanced recovery and hydrocarbon stor-
age) and III wells authorized by rule.
147.2154 Existing Class II enhanced recovery
and hydrocarbon storage wells author-
ized by rule.
147.2155 Requirements for all wells—area of
review.
Subpart SS—Texas
147.2200 State-administered program—Class
I, III, IV, and V wells.
147.2201 State-administered program—Class
II wells.
147.2205 EPA-administered program—Indian
lands.
Subpart TT—Utah
147.2250 State-administered program—Class
I, III, IV, and V wells.
147.2251 State-administered program—Class
II wells.
147.2253 EPA-administered program—Indian
lands.
Subpart UU—Vermont
147.2300 State-administered program.
147.2301-147.2302 [Reserved]
147.2303 EPA-administered program—Indian
lands.
147.2304-147.2349 [Reserved]
Subpart W—Virginia
147.2350 State-administered program. [Re-
served]
147.2351 EPA-administered program.
147.2352 Aquifer exemptions. [Reserved]
Subpart WW—Washington
147.2400 State-administered program—Class
I, II, III, IV, and V wells.
147.2403 BPA-administered program—Indian
lands.
147.2404 EPA-administered program—
Colville Reservation.
Subpart XX—West Virginia
147.2450-147.2452 [Reserved]
147.2453 EPA-administered program—Indian
lands.
147.2454-147.2499 [Reserved]
Subpart YY—Wisconsin
147.2500 State-administered program.
147.2510 EPA-administered program—Indian
lands,
Subpart ZZ—Wyoming
147.2550 State-administered program—Class
I, III, IV, and V wells.
147.2551 State-administered program—Class
II wells.
147.2553 EPA-administered program—Indian
lands.
147.2554 Aquifer exemptions.
147.2555 Aquifer exemptions since January
1. 1998,
Subpart AAA—Guam
147.2600 State-administered program.
147.2601 EPA-administered program—Indian
lands.
Subpart BBB—Puerto Rico
147.2650 State-administered program—Class
I, II, III, IV, and V wells.
147.2651 EPA-administered program—Indian
lands.
Subpart CCC—Virgin Islands
147.2700 State-administered program. [Re-
served]
147.2701 BPA-administered program.
Subpart ODD—American Samoa
147.2750 State administered program. [Re-
served]
147.2751 EPA-administered program.
147.2752 Aquifer exemptions. [Reserved]
Subpart EIE—Commonwealth of the
Northern Mariana Islands
147.2800 State-administered program—Class
I, II, III, IV, and V wells.
147.2801 EPA-administered program.
147.2802 Aquifer exemptions. [Reserved]
Subpart FFF—Trust Territory of the Pacific
Islands
147,2850 State-administered program. [Re-
served]
147.2851 BPA-administered program.
147.2852 Aquifer exemptions. [Reserved]
Subpart ©<3G—Osage Mineral Reserve-
Class II Wells
147.2901 Applicability and scope.
147.2902 Definitions.
147.2903 Prohibition of unauthorized injec-
tion.
147.2904 Area of review.
147.2905 Plugging and abandonment.
147.2906 Emergency permits.
147.2907 Confidentiality of information.
147.2908 Aquifer exemptions.
147.2909 Authorization of existing wells by
rule.
147.2910 Duration of authorization by rule.
147.2911 Construction requirements for wells
authorized by rule.
732
-------
Environmental Protection Agency
§147.1
147.2912 Operating requirements for wells
authorized by rule.
147.2913 Monitoring and reporting require-
ments for wells authorized "by rule.
147.2914 Corrective action for wells author-
ized by rule.
147.2915 Requiring a permit for wells au-
thorized by rule.
147.2916 Coverage of permitting- require-
ments,
147.2917 Duration of permits.
147.2918 Permit application information.
147.2919 Construction requirements for wells
authorized by permit.
147.2920 Operating requirements for wells
authorized by permit.
147.2921 Schedule of compliance.
147.2922 Monitoring and reporting require-
ments for wells authorized by permit.
147.2923 Corrective action for wells author-
ized by permit.
147.2924 Area permits.
147.2925 Standard permit conditions.
147.2926 Permit transfers.
147.2927 Permit modification.
147.2928 Permit termination.
147.2929 Administrative permitting proce-
dures.
Subpart HHH—Lands of the Navajo, Ute
Mountain Ute, and All Other New Mex-
ico Tribes
147.3000 EPA-administered program.
147.3001 Definition.
147.3002 Public notice of permit actions.
147,3003 Aquifer exemptions.
147.3004 Duration of rule authorization for
existing Class I and III wells.
147.3005 Radioactive waste injection wells.
147.3006 Injection pressure for existing Class
II wells authorized by rule.
147,3007 Application for a permit.
147.3008 Criteria for aquifer exemptions.
147.3009 Area of review.
147.3010 Mechanical integrity tests.
147.3011 Plugging- and abandonment of Class
III wells.
147,3012 Construction requirements for
Class I wells.
147.3013 Information to be considered for
Class I wells,
147.3014 Construction requirements for
Class III wells.
147.3015 Information to be considered for
Class III wells.
147.3016 Criteria and standards applicable to
Class V wells.
APPENDIX A TO SUBPART HHH OF PART 147—
EXEMPTED AQUIFERS IN NEW MEXICO.
Subpart III—Lands of Certain Oklahoma
Indian Tribes
147.3100 EPA-adffiiaistered program.
147.3101 Public notice of permit actions.
1-17.3102 Plugging and abandonment plans.
147.3103 Fluid seals.
147.3104 Notice of abandonment,
147.3105 Flagging and abandonment report.
147.3106 Area of review,
147.3107 Mechanical integrity.
147,3108 Plugging Class I, II, and III wells.
147.3109 Timing1 of mechanical integrity
test.
AUTHORITY: 42 U.S.C. 300h, and 42 U.S.C.
6901 et seg.
SOURCE: 49 FB 20197. May 11, 1984, unless
otherwise noted.
EDITORIAL NOTE: Nomenclature changes to
part 147 appear at 69 FR 18803, Apr. 9, 2004.
Subpart A—General Provisions
§ 147.1 Purpose and scope.
(a) This part sets forth the applicable
Underground Injection Control (UIC)
programs for each of the states, terri-
tories, and possessions identified pur-
suant to the Safe Drinking Water Act
(SDWA) as needing a UIC program.
(b) The applicable UIC program for a
State Is either a State-administered
program approved by EPA, or a feder-
ally-administered program promul-
gated by EPA. In some cases, the UIC
program may consist of a State-admin-
istered program applicable to some
classes of wells and a federally-admin-
istered program applicable to other
classes of wells. Approval of a State
program Is based upon a determination
by the Administrator that the program
meets the requirements of section 1422
or section 1425 of the Safe Drinking
Water Act and the applicable provi-
sions of parts 124, 144, and 146 of this
chapter. A federally-administered pro-
gram is promulgated in those instances
where the state has failed to submit a
program for approval or where the sub-
mitted program does not meet the min-
imum statutory and regulatory re-
quirements.
(c) In the case of State programs ap-
proved by EPA pursuant to section 1422
of the SDWA, each State subpart de-
scribes the major elements of such pro-
grams, including State statutes and
regulations, Statement of Legal Au-
thority, Memorandum of Agreement.
and Program Description. State stat-
utes and regulations that contain
standards, requirements, and proce-
dures applicable to owners or operators
have been incorporated by reference
733
-------
§147.2
40 CFR Ch. I (7-1-04 Edition)
pursuant to regulations of the Office of
the Federal Register. Material incor-
porated by reference is available for in-
spection In the appropriate EPA Re-
gional Office, in EPA Headquarters,
and at the National Archives and
Records Administration (NARA). For
information on the availability of this
material at NARA, call 202-741-6030, or
go to: http://www.archives.gov/
federal^j-egister/
code of_ federal regulations/
ibr locationsMml, Other State statutes
and regulations containing standards
and procedures that constitute ele-
ments of the State program but do not
apply directly to owners or operators
have been listed but have not been in-
corporated by reference.
(d) In the case of State programs pro-
mulgated under section 1422 that are to
be administered by EPA, the State sub-
part makes applicable the provisions of
parts 124, 144, and 146, and provides ad-
ditional requirements pertinent to the
specific State program.
(e) Regulatory provisions Incor-
porated by reference (in the case of ap-
proved State programs) or promulgated
by EPA (in the case of EPA-adminis-
tered programs), and all permit condi-
tions or permit denials issued pursuant
to such regulations, are enforceable by
the Administrator pursuant to section
1423 of the SDWA.
(f) The Information requirements lo-
cated in the following sections have
been cleared by the Office of Manage-
ment and Budget: Sections 147.104,
147.304, 147.754, 147.904, 147.1154, 147.1354,
147.1454, 147.1654, 147.1954, and 147.2154.
The OMB clearance number is No.
2040-0042.
§ 147.2 Severability of provisions.
The provisions in this part and the
various applications thereof are dis-
tinct and severable. If any provision of
this part or the application thereof to
any person or circumstances is held in-
valid, such invalidity shall not affect
other provisions or application of such
provision to other persons or cir-
cumstances which can be given effect
without the invalid provision or appli-
cation.
Subpart B—Alabama
§ 147.50 State-administered program—
Class II wells.
The UIC program for Class II wells in
the State of Alabama, except those on
Indian lands, is the program adminis-
tered by the State Oil and Gas Board of
Alabama, approved by EPA pursuant to
section 1425 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on August 2, 1982 (47 FR
33268); the effective date of this pro-
gram is August 2, 1982. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Alabama. This Incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Code of Alabama Sections 9-17-1
through 9-17-109 (Cumm. Supp. 1989);
(2) State Oil and Gas Board of Ala-
bama Administrative Code, Oil and G-as
Report 1 (supplemented through May
1989), Rules and Regulations Governing
the Conservation of Oil and Gas in Ala-
bama, and Oil and Gas Statutes of Ala-
bama with Oil and Gas Board Forms,
§400-1-2 and §400-l-5-.04.
(b) The Memorandum of Agreement
between EPA Region IV and the Ala-
bama Oil and Gas Board, signed by the
EPA Regional Administrator on June
15, 1982.
(c) Statement of legal authority. "State
Oil and Gas Board has Authority to
Carry Out Underground Injection Con-
trol Program Relating to Class II Wells
as Described in Federal Safe Drinking
Water Act—Opinion by Assistant At-
torney General," May 28,1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43086, Oct. 25, 1988; 56 FR 9411, Mar. 6,
1991]
734
-------
Environmental Protection Agency
§ 147.52
§ 147.51 State-administered program—
Class I, III, IV, and V wells.
The UIC program for Class I, III, IV
and V wells in the State of Alabama,
except those on Indian lands, is the
program administered by the Alabama
Department of Environmental Manage-
ment, approved by EPA pursuant to
section 1422 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on August 25. 1983 (48
PR 38640S: the effective date of this pro-
gram is August 25, 1983. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application:
(a.) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Alabama. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25. 1984.
(1) Alabama Water Pollution Control
Act, Code of Alabama 1975, sections 22-
22^1 through 22-22-14 (1980 and Supp.
1983);
(2) Regulations, Policies and Proce-
dures of the Alabama Water Im-
provement Commission, Title I (Regu-
lations) (Rev. December 1980), as
amended May 17, 1982, to add Chapter 9,
Underground Injection Control Regula-
tions (effective June 10, 1982), as
amended April 6, 1983 (effective May 11,
1983).
(b) The Memorandum of Agreement
between EPA Region IV and the Ala-
bama Department of Environment
Management, signed by the EPA Re-
gional Administrator on May 24, 1983.
(c) Statement of legal authority. (1)
"Water Pollution^Public Health^
State has Authority to Carry Out Un-
derground Injection Control Program
Described in Federal Safe Drinking
Water Act—Opinion by Legal Counsel
for the W'ater Improvement Commis-
sion," June 25, 1982;
(2) Letter from Attorney, Alabama
Water Improvement Commission, to
Regional Administrator, EPA Region
IV, "Re; AWIC Response to Phillip
Tate's (U.S. EPA, Washington) Com-
ments on AWIC's Final Application for
Class I, III, IV, and V UIC Program."
September 21, 1982:
(3) Letter from Alabama Chief Assist-
ant Attorney General to Regional
Counsel, EPA Region IV, "Re: Status of
Independent Legal Counsel in Alabama
Water Improvement Commission's Un-
derground Injection Control Program,"
September 14. 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
(4P FR 20197. May 11, 1984. as amended at 53
FR 43086, Oct. 25,
§ 147.52 State-administered program—
Hydraulic Fracturing of Coal Beds.
The UIC program for hydraulic frac-
turing of coal beds in the State of Ala-
bama, except those on Indian lands, is
the program administered by the State
Oil and Gas Board of Alabama, ap-
proved by EPA pursuant to Section
1425 of the SDWA on December 22, 1999
and effective on January 19, 2000. The
Alabama program consists of the fol-
lowing elements, as submitted to EPA
in the State's program application:
(a) Incorporation by reference. The re-
quirements set forth in State Oil and
Gas Board of Alabama Rule 400-4--1-.02,
Definitions, and Rule 400-4 5-.04, Pro-
tection of Underground Sources of
Drinking Water during the Hydraulic
Fracturing of Coal Beds, are hereby in-
corporated by reference and made a
part of the applicable UIO program
under the SDWA for the State of Ala-
bama. This incorporation by reference
was approved by the Director of the
Federal Register on January 19, 2000 in
accordance with 5 U.S.C. 552(a) and 1
CPR Part 51. Copies may be obtained at
the State Oil and Gas Board of Ala-
bama, 420 Hackberry Lane, Tuscaloosa,
AL 35489-9780, Copies may be inspected
at the Environmental Protection Agen-
cy, Region 4, Water Management Divi-
sion, Ground Water/Drinking Water
Branch, Ground Water & UIO Section,
Sam Nunn Atlanta Federal Center, 61
Forsyth Street, S.W., Rooml5-T53. At-
lanta, GA 30303-8960. or at the National
Archives and Records Administration
(NARA). For information on the avail-
ability of this material at NARA, call
202-741-6030, or go to: http://
www.archives.gov/fede.ral ^register/
735
-------
§147.60
40 CFR Ch, I (7-1-04 Edition)
code of_ federal regulations/
ibr_ locations.html.
(b) Addendum One, Underground In-
jection Control Program, Memorandum
of Agreement Between the State of
Alabama and the USEPA Region 4,
signed by the Supervisor, Alabama
State Oil and Gas Board on December
10, 1999, and the Regional Adminis-
trator, U.S. Environmental Protection
Agency Region 4, on December 13, 1999.
(c) Statement of Legal Authority. "I
hereby certify, pursuant to my author-
ity as Attorney General for the State
of Alabama and for reasons set forth in
this statement, that in my opinion, the
laws of the State of Alabama provide
the State Oil and Gas Board (herein-
after referred to as "the Board") ade-
quate authority to carry out an Under-
ground Injection Program for the con-
trol of underground injection activity
related to the hydraulic fracturing of
coal beds." Opinion by Alabama's At-
torney General Office, extracted from
Letter from R. Craig Kneisel, Chief,
Environmental Division, Office of the
Attorney General, dated October 8,
1999, to Dr. Donald P. Oltz, Supervisor,
State Oil and Gas Board of Alabama,
Subject: Attorney General's Statement
for Final Authorization of Alabama
Class II Underground injection Control
Program.
(d) The Program Description for the
Regulation of Hydraulic Fracturing' of
Coal Beds As required by 40 CPR
145.23—State Oil and Gas Board of Ala-
bama, including Appendices A through
P.
[65 PR 2897, Jan. 19, 2000]
§ 147.60 IPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in Ala-
bama is administered by EPA. This
program consists of the UIC program
requirements of 40 CFR parts 124, 144,
146, 148 and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Alabama is November 25, 1988.
[53 PR 43086, Oct. 25, 1988, as amended at 56
FR 9411, Mar. 6, 1991]
Subpart C—Alaska
§ 147.100 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Alaska, other than those
on Indian lands, is the program admin-
istered by the Alaska Oil and Gas Con-
servation Commission approved by
EPA pursuant to section 1425 of the
SDWA. Notice of this approval was
published in the FEDERAL REGISTER
[May 6, 1986]; the effective date of this
program is June 19, 1986. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Alaska. This incorporation
by reference was approved by the Di-
rector of the Federal Register effective
June 19, 1986.
(1) Alaska Statutes, Alaska Oil and
Gas Conservation Act, Title 31,
§§31.05,005 through 31.30.010 (1979 and
Cum. Supp. 1984);
(2) Alaska Statutes, Administrative
Procedures Act, Title 44, §§44.62.010
through 44.62.650 (1984);
(3) Alaska Administrative Code, Alas-
ka Oil and Gas Conservation Commis-
sion, 20 AAC 25.005 through 20 AAC
25.570 (Supp. 1986).
(b) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region 10, and the Alaska Oil and
Gas Conservation Commission, signed
by the EPA Regional Administrator on
January 29. 1986, as amended on June
21, 1988.
(c) Statement of Legal Authority.
Statement from the Attorney General
of the State of Alaska, signed by the
Assistant Attorney General on Decem-
ber 10,1985.
(d) The Program Description and any
other materials submitted as part of
736
-------
Environmental Protection Agency
§147,104
the original application or as supple-
ments thereto.
[51 FR 16684, May 6. 1986, as amended at 56
FR 9411. Mar. 6. 1991]
§ 147.101 EPA-administered program.
(a) Contents. The UIC program in the
State of Alaska for Class I. in, IV. and
V wells, and for all classes of wells on
Indian lands, is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CFR parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
of the UIC program for all non-Class II
wells in Alaska and for all wells on In-
dian lands, is June 25, 1984.
[52 PR 17680, May 11, 1987, as amended at 56
FR 9412, Mar. 6, 1991]
§ 147.102 Aquifer exemptions.
(a) This section identifies any
aquifers or their portions exempted in
accordance with §§144.7(b) and 146.4 of
this chapter at the time of program
promulgation. EPA may in the future
exempt other aquifers or portions, ac-
cording to applicable procedures, with-
out codifying such exemptions in this
section. An updated list of exemptions
will be maintained in the Regional of-
fice.
(b) The following aquifers are ex-
empted in accordance with the provi-
sions of §§144.7(b) and 146,4 of this chap-
ter for Class II injection activities
only:
(1) The portions of aquifers in the
Kenai Peninsula, greater than the indi-
cated depths below the ground surface.
and described by a Vi mile area beyond
and lying directly below the following
oil and gas producing fields:
(i) Swanson River Field^l700 feet.
(ii) Beaver Creek Field—1650 feet,
(iii) Kenai Gas Field—1300 feet.
(2) The portion of aquifers beneath
Cook Inlet described by a J/i mile area
beyond and lying directly below the
following oil and gas producing fields:
(i) Granite Point,
(ii) Me Arthur River Field.
(iii) Middle Ground Shoal Field.
(iv) Trading Bay Field.
(3) The portions of aquifers on the
North Slope described by a l/>\ mile area
beyond and lying directly below the
Kuparuk River Unit oil and gas pro-
ducing field.
1147.108 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144.28(0(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.733-0,433 Sg)d
wliere:
Pm=injection pressure at the well bead in
pounds per square inch
Sg—specific gravity of inject fluid (unitless)
d=injection depth in feet.
§147.104 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§144.28(0(3X11) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish maximum injection
pressures after notice, opportunity for
comment, and opportunity for a public
hearing, according to the provisions of
part 124. subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(aXD(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
737
-------
§147.150
40 CFR Ch. I (7-1-04 Edition)
to the provisions of part 124, subpart A
of this chapter,
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(ii) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within 1 year of the effective date of
this program,
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§ 144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most TJSDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure:
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
as needed to protect USDWs.
Subpart D—Arizona
§ 147.160 State-administered program.
[Reserved]
§ 147.151 EPA-administered program.
(a) Contents. The UIC program that
applies to all injection activities in Ar-
izona, including those on Indian lands,
is administered by EPA. The UIC pro-
gram for Navajo Indian lands consists
of the requirements contained in sub-
part HHH of this part. The program for
all injection activity except that on
Navajo Indian lands consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
for the UIC program in Arizona, except
for the lands of the Navajo Indians, is
June 25, 1984. The effective date for the
UIC program on the lands of the Nav-
ajo is November 25, 1988.
[53 FR 43086, Oct. 25. 1988, as amended at 56
FE 9412, Mar. 6, 1991]
§ 147.152 Aquifer exemptions. [Re-
served]
Subpart E—Arkansas
§ 147.200 State-administered pro-
gram—Class I, III, IV, and V wells.
The UIC program for Class I, III, IV
and V wells in the State of Arkansas,
except those wells on Indian lands, is
the program administered by the Ar-
kansas Department of Pollution Con-
trol and Ecology approved by EPA pur-
suant to section 1422 of the SDWA. No-
tice of this approval was published in
the FEDERAL REGISTER, on July 6, 1982
(47 PR 29236); the effective date of this
program is July 6, 1982. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application.
(a) Incorporation by reference. The
requirements set forth in the State
statutes and regulations cited in this
paragraph are hereby incorporated by
738
-------
Environmental Protection Agency
§147.205
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Arkansas. This Incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25. 1984.
(1) Arkansas Water and Air Pollution
Control Act, Act 472 of 1949 as amend-
ed, Arkansas Statutes Annotated sec-
tions 82-1901 through 82-1943 (1976);
(2) Act 105 of 1939, Arkansas Statutes
Annotated sections 53-101 through 53-
130 (1971 and Supp. 1981); Act 937 of 1979,
Arkansas Statutes Annotated sections
53-1301 through 53-1320 (Supp. 1981); Act
523 of 1981;
(3) Arkansas Underground Injection
Control Code, Department of Pollution
Control and Ecology, promulgated Jan-
uary 22, 1982;
(4) General Rule and Regulations, Ar-
kansas Oil and Gas Commission (Order
No. 2-39, revised July 1972);
(5) Arkansas Hazardous Waste Man-
agement Code, Department of Pollu-
tion Control and Ecology, promulgated
August 21. 1981.
(b) The Memorandum of Agreement
and Addendum No. 1 to the Memo-
randum of Agreement, between EPA
Region VI and the Arkansas Depart-
ment of Pollution Control and Ecology
and the Arkansas Oil and Gas Commis-
sion, signed by the EPA Regional Ad-
ministrator on May 25, 1982.
(c) Statement of legal authority, (1)
Letter from Chief Attorney, Arkansas
Department of Pollution Control and
Ecology, to Acting Regional Adminis-
trator, EPA Region VI, "Re: Legal Au-
thority of the Department of Pollution
Control and Ecology of the State of Ar-
kansas to Administer an Underground
Injection Control Program." July 29,
1981;
(2) Letter from Chief Attorney, Ar-
kansas Department of Pollution Con-
trol and Ecology, to Acting Regional
Counsel. EPA Region VI, "Re: Adden-
dum to Legal Statement,—Underground
Injection Control Program," October 13.
1981;
(3) Letter from General Counsel. Ar-
kansas Oil and Gas Commission, to
Acting Regional Counsel, EPA Region
VI, "Re: Supplemental Addendum to
Legal Statement—Underground Injec-
tion Control Program." October 20.
1981;
(4) Letter from Chief Attorney. Ar-
kansas Department of Pollution Con-
trol and Ecology, to Attorney, Office of
Regional Counsel, EPA Region VI (re:
status as independent legal counsel),
December 31,1981:
(5) Letter from General Counsel, Ar-
kansas Oil and Gas Commission, to
Acting Regional Counsel, EPA Region
VI, "Re: Supplemental Addendum to
Legal Statement—Underground Injec-
tion Control Program," January 13,
1982;
(6) Letter from Chief Counsel, Arkan-
sas Department of Pollution Control
and Ecology, to Acting Regional Coun-
sel, EPA Region VI, "Re: Addendum to
Legal Statement—Underground Injec-
tion Control Program," February 15.
1982;
(7) Letter from Chief Counsel, Arkan-
sas Department of Pollution Control
and Ecology, to Acting Regional Coun-
sel, EPA Region VI, "Re: Addendum to
Legal Statement—Underground Injec-
tion Control Program," May 13, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43086, Oct. 25, 1988]
§ 147,201 State-administered pro-
gram—Class II wells. [Reserved]
i 147.205 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in Ar-
kansas is administered by EPA. This
program consists of the UIC program
requirements of 40 CFR parts 124. 144,
146, 148 and any additional require-
ments set forth in this subpart. Injec-
tion well owners and operators, and
EPA shall comply with these require-
ments.
(b) Effective dale. The effective date
of the UIC program for Indian lands in
Arkansas is November 25, 1988.
[53 FR 43086. Oct. 25. 1988. as amended at 56
PR 9412. Mar. 6, 1991]
739
-------
§147.250
40 CFR Ch. 1 (7-1-04 Edition)
Subpart F—California
§ 147.250 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of California, except those on
Indian lands, is the program adminis-
tered by the California Division of Oil
and Gas, approved bjr EPA pursuant to
SDWA section 1425.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of California. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984,
(1) California Laws for Conservation
of Petroleum and Gas, California Pub-
lic Resources Code Div. 3, Chapt. 1,
§§3000-3359(1989);
(2) California Administrative Code,
title 14, §§1710 to 1724.10 (May 28, 1988).
(b) The Memorandum of Agreement
between EPA Region IX and the Cali-
fornia Division of Oil and Gas, signed
by the EPA Regional Administrator on
September 29, 1982.
(c) Statement of legal authority. (1)
Letter from California Deputy Attor-
ney General to the Administrator of
EPA, "Re: Legal Authority of Cali-
fornia Division of Oil and Gas to Carry
Out Class II Injection Well Program,"
April 1, 1981;
(2) Letter from California Deputy At-
torney General to Chief of California
Branch, EPA Region IX, "Re; California
Application for Primacy, Class II UIC
Program," December 3, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 52
FB 17681, May 11, 1987; 56 FR 9412, Mar. 6.
1991]
§147,251 EPA-administered program—
Class I, III, IV and V wells and In-
dian lands.
(a) Contents. The UIC program in the
State of California for Class I, HI, IV
and V wells, and for all classes of wells
on Indian lands, is administered by
EPA. The program consists of the UIC
program requirements of 40 OFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
for the UIC program for all lands in
California, including Indian lands, is
June 25, 1984.
[52 FR, 17681, May 11, 1987, as amended at 56
FB 9412, Mar. 6, 1991]
§ 147.252 Aquifer exemptions. [Re-
served]
§147.253 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule,
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0,733~ 0.433 Sg)d
where;
Pm=injection pressure at the well head in
pounds per square inch
Sg=speeific gravity of inject fluid (anitless)
d=injection depth In feet.
Subpart G—Colorado
§ 147.300 State-administered pro-
gram—Class II wells,
The UIC program for Class II wells in
the State of Colorado, except those
wells on Indian Lands, is the program
administered by the Colorado Oil and
Gas Commission approved toy EPA pur-
suant to section 1425 of the SDWA. No-
tice of this approval was published in
the FR on April 2, 1984 (49 PR 13040);
the effective date of this program is
April 2, 1984. This program consists of
the following elements, as submitted to
EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
740
-------
Environmental Protection Agency
§ 147.301
the State of Colorado. This incorpora-
tion by reference was approved by the
Director of the OFR in accordance with
5 U.S.C. 552(a) and 1 CPR part 51. Cop-
ies may be obtained at the State of
Colorado Oil and Gas Conservation
Commission, Department of Natural
Resources, Suite 380 Logan Tower
Building, 1580 Logan Street, Denver,
Colorado, 80203, Copies may be in-
spected at the Environmental Protec-
tion Agency, Region VIII, 999 18th
Street. Suite 500, Denver, Colorado,
80202-2405, or at the National Archives
and Records Administration (NARA).
For information on the availability of
this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/
federal_register/
code of federal^ regulations/
ibr locations, html.
(1) Colorado Revised Statutes, 1989
replacement volume, Section 34-60-101
through 34-60-123;
(2) Colorado Revised Statutes. 1989
replacement volume, Section 25-8-101
through 25-8-612;
(3) Rules and Regulations, Rules of
Practice and Procedure, and Oil and
Gas Conservation Act (As Amended)
Department of Natural Resources, Oil
and Gas Conservation Commission of
the State of Colorado (revised July
1989);
(4) Oil and Gas Conservation Commis-
sion Revised Rules and Regulations in
the 300, 400, 500, and 600 series, effective
March 20, 1989.
(b) Memorandum of agreement. The
Memorandum of Agreement between
EPA Region VIII and the Colorado Oil
and Gas Conservation Commission,
signed by the EPA Regional Adminis-
trator on March 3, 1984 and amended on
August 30, 1989.
(c) Statement of legal authority. (1)
Letter from Colorado Assistant Attor-
ney General to the Acting Regional
Counsel, EPA Region VIII, "Re; Class II
Well Underground Injection Control
Program of Colorado Oil and Gas Con-
servation Commission", March 15, 1983;
(2) Letter from Colorado Assistant
Attorney General to the Acting" Re-
gional Counsel, EPA Region VIII, "Re:
Class II Well Injection Control Pro-
gram of Colorado Oil and Gas Con-
servation Commission", April 29, 1983;
(3) Letter from Colorado Assistant
Attorney General to the Acting Re-
gional Counsel, EPA Region VIII, "Re:
Class II Underground Injection Control
Program of Colorado Oil and Gas Con-
servation Commission, interpretation
of C.R.S. 1973, 34-80-110", July 11, 1983;
(4) Letter from Colorado Assistant
Attorney General to the Acting Re-
gional Counsel, EPA Region VIII, "Re:
Class II Well Underground Injection
Control Program of Colorado Oil and
Gas Conservation Commission", Feb-
ruary 17, 1984;
(5) Memorandum from Colorado As-
sistant Attorney General to the Acting
Regional Counsel, EPA Region VIII,
"Re; Authority to set and enforce max-
imum pressure for injecting fluids into
Class II wells with existing permits",
March 7, 1984.
(d) Program description. The Program
Description and any other materials
submitted as part of the application or
as supplements thereto:
(1) Application and accompanying
materials for approval of Colorado's
UIC program for Class II wells sub-
mitted by the Director of the Colorado
Oil and Gas Conservation Commission
to the Regional Administrator. May 3.
1983;
(2) Supplemental amendment to
Colorado's application for primacy for
the UIC program for Class II wells de-
scribing the process through which the
State will ensure enforceable limits for
maximum injection pressure, describ-
ing the Commission's plan of adminis-
tration for Class II wells, and describ-
ing Mechanical Integrity Test proce-
dures for Class II wells, March 7, 1984;
(3) Official correspondence con-
cerning various program issues be-
tween the Colorado Oil and Gas Con-
servation Commission and EPA Region
VIII. for the period from March 7, 1984
to May 8, 1989.
[56 FB 9412, Mar. 6, 1991]
§ 147,301 EPA-administered program—
Class I, III, IV, V wells and Indian
lands.
(a) Contents, The UIC program for
Class I, III, IV and V wells on all lands
in Colorado, including Indian lands,
and for Class II wells on Indian lands,
is administered by EPA. The program
741
-------
§147.302
40 CFR Ch. 1 (7-1-04 Edition)
for all EPA-administered wells in Colo-
rado other than Class II wells on the
lands of the Ute Mountain Ute consists
of the UIC program requirements of 40
CPE parts 124, 144, 146, 148, and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements.
(b) Effective dates. The effective date
for the UIC program on all lands in
Colorado, including Indian lands, ex-
cept for Class II wells on lands of the
Ute Mountain Ute, is June 25, 1984.
[52 FR 17681, May 11, 1987, as amended at 56
FR 9413, Mar. 6, 1991]
§ 147.302 Aquifer exemptions.
(a) This section identifies any
aquifers of their portions exempted in
accordance with §§144.7(b) and 146.4 of
this chapter at the time of program
promulgation. EPA may in the future
exempt other aquifers or portions ac-
cording to applicable procedures with-
out codifying such exemptions in this
section. An updated list of exemptions
will be maintained in the Regional of-
fice.
(b) For all aquifers into which exist-
ing Class II wells are injecting, those
portions within a Vt mile radius of the
well are exempted for the purpose of
Class II injection activities only.
§147.303 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for wellhead pressure cal-
culated by using the following formula;
Pm=(0.733~Q.433 Sg)d
where:
Pm=injeetlon pressure at the wellhead in
pounds per square inch
Sg=speoific gravity of injected fluid
(unitless)
d=injection depth in feet.
§147.304 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirements of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter.
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressures based on
data provided pursuant to paragraph
(a)(2)(ii) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within one year of the effective date of
this program.
742
-------
Environmental Protection Agency
§147.305
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by reeir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistent to deteriora-
tion from formation and injection
fluids; and
(iii) In quantity no less than 120% of
the calculated volume necessary to ce-
ment off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
as needed to protect USDWs,
§ 147.305 Requirements for all wells.
(a) The owner or operator converting
an existing well to an injection well
shall check the condition of the casing
with one of the following logging tools:
(IS A Pipe analysis log; or
(2) A Caliper log.
(b) The owner or operator of a new
injection well cased with plastic (PVC,
ABS, and others) casings shall:
(1) Not construct a well deeper than
500 feet;
(2) Use cement and additives compat-
ible with such casing material;
(3) Cement the annular space above
the injection interval from the bottom
of the blank casing to the surface.
(c) The owner or operator of a newly
drilled well shall install centralizers as
directed by the Regional Adminis-
trator,
(d) The owner or operator shall as re-
quired by the Regional Administrator:
(1) Protect USDWs by:
(i) Setting surface casing 50 feet
below the base of the lowermost
USDW;
(ii) Cementing surface casing by re-
circulating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(iii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
approve alternate casing and cement-
ing practices provided that the owner
or operator demonstrates that such
practices will adequately protect
USDWs.
(e) Area of review. Notwithstanding
the alternatives presented in §146.6 of
this chapter, the area of review shall be
a fixed radius as described in §146,6(b)
of this chapter.
(f) The applicant must give separate
notice of intent to apply for a permit
to each owner or tenant of the land
within one-quarter mile of the site.
The addresses of those to whom notice
is given, and a description of how no-
tice is given, shall be submitted with
the permit application. The notice
shall include:
(1) Name and address of applicant;
(2) A brief description of the planned
injection activities, including well lo-
cation, name and depth of the injection
zone, maximum injection pressure and
volume, and fluid to be injected;
(3) EPA contact person; and
(4) A statement that opportunity to
comment will be announced after EPA
743
-------
§147.350
40 CFR Ch. I (7-1-04 Edition)
prepares a draft permit. This require-
ment may be waived by the Regional
Administrator when he determines
that individual notice to all land own-
ers and tenants would be impractical.
Subpart H—Connecticut
§ 147.350 State-administered program.
The UIC program for all classes of
wells in the State of Connecticut.
except those wells on Indian lands, is
the program administered by the Con-
necticut Department of Environmental
Protection approved by EPA pursuant
to section 1422 of the SDWA. Notice of
this approval was published in the FR
on March 26, 1984 (49 PR 11179); the ef-
fective date of this program is March
26, 1984. This program consists of the
following elements, as submitted to
EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made part of the applicable
UIC program under the SDWA for the
State of Connecticut. This incorpora-
tion by reference was approved by the
Director of the OPR in accordance with
5 U.S.C. 552(a) and CPR part 51. Copies
may be obtained at the State of Con-
necticut, Department of Environ-
mental Protection, State Office Build-
ing, 165 Capitol Avenue, Hartford, Con-
necticut, 06106. Copies may be in-
spected at the Environmental Protec-
tion Agency, Region I, John P. Ken-
nedy Federal Building, room 2203, Bos-
ton, Massachusetts, 02203, or at the Na-
tional Archives and Records Adminis-
tration (NARA). For information on
the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.arcMves.gov/federal register/
code of__federal regulations/
ibr locations.html,
(1) Connecticut General Statutes An-
notated, title 22a (Environmental Pro-
tection), chapter 439, sections 22a~l
through 22a-27 (1985 and Cumm. Supp.
1990);
(2) Connecticut General Statutes An-
notated, Title 22a (Environmental Pro-
tection). Chapter 446K (1985 and Cumm.
Supp. 1990).
(b) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region I and the Connecticut De-
partment of Environmental Protection,
signed by the EPA Regional Adminis-
trator on August 9, 1983.
(c) Statement of legal authority. (1)
Statement from the Attorney General
of the State of Connecticut, signed by
the Attorney General on May 8, 1981:
(2) Addendum to the Statement from
the Attorney General of the State of
Connecticut, signed by the Attorney
General on May 10, 1983.
(d) Program Description. The Program
Description and any other materials
submitted as part of the application or
as supplements thereto.
[56 FR 9413, Mar. 6, 1991]
!§ 147.351-147J52 [Reserved]
§ 147.353 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in Con-
necticut is administered by EPA. This
program consists of the UIC program
requirements of 40 CFR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Connecticut is November 25, 1988.
[53 FE 43086, Oct. 25, 1988, as amended at 56
FR 9413, Mar. 6, 1991]
§§ 147.354-147.359 [Reserved]
Subpart I—Delaware
§ 147.400 State-administered program,
The UIC program for all classes of
wells in the State of Delaware, except
those wells on Indian lands, is the pro-
gram administered by the Delaware
Department of Natural Resources and
Environmental Control approved by
EPA pursuant to section 1422 of the
SDWA. Notice of this approval was
published in the FR on April 5, 1984 (49
FR 13525); the effective date of this pro-
gram is May 7, 1984. This program con-
sists of the following elements, as sub-
mitted to EPA in the State's program
application:
744
-------
Environmental Protection Agency
§147.500
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Delaware. This incorpora-
tion by reference was approved by the
Director of the OFB in accordance with
5 U.S.C. 552(a) and 1 CFR part 51. Copies
may be obtained at the Delaware De-
partment of Natural Resources and En-
vironmental Control, 89 Kings High-
way, P.O. Box 1401, Dover, Delaware.
19903. Copies may be inspected at the
Environmental Protection Agency, Re-
gion III, 841 Chestnut Street, Philadel-
phia, Pennsylvania, 19107, or at the Na-
tional Archives and Records Adminis-
tration (NARA). For information on
the availability of this material at
NARA, call 202-741-6030, or go to: http:ff
www.archives.gov/federal register/
code __of_federal regulations/
ibr _ locations.html.
(1) Delaware Environmental Protec-
tion Act, (Environmental Control) 7
Delaware Code Annotated, Chapter 60,
Sections 6001-6060 (Revised 1974 and
Cumm. Supp. 1988);
(2) State of Delaware Regulations
Governing Underground Injection Con-
trol, parts 122, 124 and 146 (Department
of Natural Resources and Environ-
mental Control}, effective August 15,
1983.
(b) Memorandum of agreement. The
Memorandum of Agreement between
EPA Region III and the Delaware De-
partment of Natural Resources and En-
vironmental Control, signed by the
EPA Regional Administrator on March
28, 1984.
(c) Statement of legal authority. State-
ment of the Delaware Attorney Gen-
eral for the Underground Injection
Control Program, signed by the Attor-
ney General on January 26, 1984.
(d) Program Description. The Program
Description and any other materials
submitted as part of the application
(August 10, 1983), or as supplements
thereto (October 14,1983).
[56 FB 9413, Mar. 6, 1991]
§§ 147.401-147.402 [Reserved]
§ 147.403 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in Dela-
ware is administered "by EPA. This pro-
gram consists of the UIC program re-
quirements of 40 CFR parts 124, 144, 146.
148, and any additional requirements
set forth in the remainder of this sub-
part. Injection well owners and opera-
tors and EPA shall comply with these
requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Delaware is November 25, 1988.
[53 FB 43086, Oct. 25, 1988, as amended at 56
PR 9413, Mar. 6, 1991]
§§ 147.404-147,449 [Reserved]
Subpart J—District of Columbia
§ 147.450 State-administered program.
[Reserved]
§ 147.451 EPA-administered program.
(a) Contents. The UIC program for the
District of Columbia, including any In-
dian lands in the District, is adminis-
tered by EPA. This program consists of
the UIC program requirements of 40
CFR parts 124. 144, 146, 148. and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements,
(b) Effective date. The effective date
of the UIC program for Indian lands in
the District of Columbia is November
25, 1988. The effective date for the UIC
program in the rest of the District is
June 25, 1984.
[53 FB 43087, Oct. 25, 1988. as amended at 56
PR 9413, Mar. 6. 1991 j
§147,452 Aquifer
served]
exemptions. [Re-
Subpart K—Florida
§ 147.500 State-administered pro-
gram—Class I, III, IV, and V wells.
The UIC program for Class I, III, IV.
and V wells in the State of Florida, ex-
cept for those on Indian lands is admin-
istered by the Florida Department of
Environmental Regulations, approved
745
-------
§147.501
40 CFR Ch. I (7-1-04 Edition)
by EPA pursuant to section 1422 of the
SDWA, Notice of this approval was
published in the FEDERAL REGISTER on
February ?, 1983 (48 PR 5556); the effec-
tive date of this program is March 9,
1983. This program consists of the fol-
lowing elements, as submitted to EPA
in the State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Florida. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Florida Air and Water Pollution
Control Act, Florida Statutes Anno-
tated sections 403.011 through 403.90
(1973 and Supp. 1983);
(2) Chapter 17-28, Underground Injec-
tion Control, Florida Administrative
Code (April 27,1989).
(b) Other laws. The following statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Administrative Procedures Act.
Florida Statutes Chapter 120;
(2) Florida Administrative Code,
Chapter 17-1 (1982) (Administrative
Procedures Act);
(3) Florida Administrative Code,
Chapter 17-3 (1982) (Water Quality
Standards);
(4) Florida Administrative Code.
Chapter 17-4 (1982) (Permits);
(5) Florida Administrative Code.
Chapter 28-5 (1982) (Decisions Deter-
mining Substantial Interests);
(6) Florida Administrative Code,
Chapter 28-6 (1982) (Licensing);
(c) The Memorandum of Agreement
between EPA Region IV and the Flor-
ida Department of Environmental Reg-
ulation, signed by the EPA Regional
Administrator on March 31, 1983.
(d) Statement of legal authority. (1)
"Statement of Legal Authority for Im-
plementation of Underground Injection
Control Program" and accompanying
certifications, signed by General Coun-
sel for the Florida Department of Envi-
ronmental Regulation, January 14,
1982;
(2) "Addendum to Statement of Legal
Authority for Implementation of Un-
derground Injection Control Program"
and accompanying certifications,
signed by Acting General Counsel for
the Florida Department of Environ-
mental Regulation, September 20, 1982,
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43087. Oct. 25, 1988; 56 FR 9414, Mar. 6,
1991]
§ 147.501 EPA-administered program—
Class II wells and Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands and for
Class II wells on non-Indian lands in
the State of Florida is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
of the UIC program for Indian lands in
Florida is November 25, 1988. The effec-
tive date for Class II wells on non-In-
dian lands is December 30, 1984.
[53 FR 43087, Oct. 25. 1988, as amended at 56
FR 9414, Mar, 6, 1991]
1147.502 Aquifer exemptions, [Re-
served]
§147.508 Existing Class II (except en-
hanced recovery and hydrocarbon
storage) wells authorized by rule,
Maximum injection pressure. To meet
the operating requirements of
§144.28(f)(3)(i) of this chapter, the
owner or operator shall use an injec-
tion pressure at the well head no great-
er than the pressure calculated using
the following formula:
Pm=(0.733-0,433 Sg)d
where:
Pm=injeetion pressure at the well head in
pounds per square inch
Sg=speoiflc gravity of injected fluid
(unitless)
d=injeetion depth In feet.
[49 FR 45306. Nov. 15, 1984]
746
-------
Environmental Protection Agency
§147.550
8147,504 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§H4.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressure greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter.
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(ii) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within 1 year of the effective date of
this program.
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§ 144.28(e) and
146.22, the owner or operator shall,
when required by the Regional Admin-
istrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore: and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure:
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of" the calculated volume necessary to
cement off a zone.
(4) Comply with other requirements
which the Regional Administrator may
specify either in addition to or in lieu
of the requirements set forth in para-
graphs (b)(l) through (3) of this section
as needed to protect USDWs.
(c) Area of review. Notwithstanding
the alternatives presented in §148,06 of
this chapter, the area of review shall be
a minimum fixed radius as described in
§146.06(b) of this chapter.
(The information collection requirements
contained in paragraph ia)(2)(ii) were
appoved by the Office of Management and
Budget under control number 2040-0042)
[49 FB 45306. Nov. 15. 1984]
Subpart L—Georgia
§ 147.550 State-administered program.
The UIC program for all classes of
wells in the State of Georgia, except
747
-------
§§147.551-147.552
40 CFR Ch. 1 (7-1-04 Edition)
those wells on Indian lands, is the pro-
gram administered by the Georgia De-
partment of Natural Resources, Envi-
ronmental Protection Division ap-
proved by EPA pursuant to section 1422
of the SDWA. Notice of this approval
was published in the FEDERAL REG-
ISTER on April 19, 1984 (49 PR 15553); the
effective date of this program is May
21, 1984. This program consists of the
following elements, as submitted to
EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Georgia. This incorpora-
tion by reference was approved by the
Director of the OFR in accordance with
5 U.S.C. 552(a) and 1 CFR part 51. Cop-
ies may be obtained at the Georgia De-
partment of Natural Resources, Envi-
ronmental Protection Division, 270
Washington Street, SW., Atlanta,
Georgia, 30334. Copies may he inspected
at the Environmental Protection Agen-
cy, Region IV, 345 Courtland Street,
NE., Atlanta, Georgia, 30365, or at the
National Archives and Records Admin-
istration (NARA). For information on
the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal ^register/
code of _federal regulations/
ibr locations.html.
(1) Oil and Gas and Deep Drilling Act
of 1975. Official Code of Georgia Anno-
tated (O.C.G.A.) §§12-4-40 through 12-4-
53 (1988);
(2) Ground Water Use Act of 1972,
O.C.G.A. §§12-5-90 through 12-5-107
(1988):
(3) Water Well Standards Act of 1985.
O.C.G.A. §§12-5-120, through 12-5-138
(1988);
(4) Georgia Administrative Procedure
Act. O.C.G.A. §§50-13-1 through 50-13-22
(Reprinted from the O.C.G.A. and 1988
Cumm. Supp.);
(5) Georgia Water Quality Control
Act. O.C.G.A. §§12-5-20 through 12-5-53
(1988);
(6) Georgia Hazardous Waste Manage-
ment Act. O.C.G.A. §§12-8-60 through
12-8-83 (1988);
(7) Georgia Safe Drinking Water Act
of 1977, O.C.G.A. §§12-5-170 through 12-
5-193 (1988);
(8) Rules of Georgia Department of
Natural Resources, Environmental
Protection Division, Water Quality
Control. GA. COMP. R. & REGS. Chap-
ter 391-3-6-.13 (Revised July 28, 1988).
(b) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region IV and the State of Geor-
gia, signed March 1, 1984.
(c) Statement of legal authority. (1) Un-
official Opinion of the Georgia Attor-
ney General, Op. Atty. Gen. 080-24,
June 12, 1980;
(2) Underground Injection Control
Program, Attorney General's State-
ment, February 4, 1982:
(3) Amended Attorney General's
Statement Relating to Authority of
the State of Georgia to Implement an
Underground Injection Control Pro-
gram. April 22, 1983;
(4) Letter to EPA Office of General
Counsel from Senior Assistant Attor-
ney General "Re; State UIC Program",
July 13, 1983.
(d) Program Description. The Program
Description and any other materials
submitted as part of the application or
as supplements thereto.
[56 FR 9414, Mar. 6, 1991: 56 FR 14150, Apr. 5,
1991]
§ § 147.551-147.552 [Reserved]
§ 147.553 EPA-administered program—
, Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Georgia is administered by
EPA. This program consists of the UIC
prog'ram requirements of 40 CPR parts
124, 144. 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC prog'ram for Indian lands in
Georgia is November 25. 1988.
[53 FR 43087, Oct. 25, 1988, as amended at 56
PR 9414, Mar. 6, 1991]
748
-------
Environmental Protection Agency
§§ 147,554-147.559 [Reserved]
Subpart M—Hawaii
§ 147.600 State-administered program,
[Reserved]
§ 147.601 EPA-administered program.
(a) Contents. The UIC program for the
State of Hawaii, Including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CFB parts 124, 144.
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Hawaii is November 25, 1988. The effec-
tive date for the UIC program for all
other lands in Hawaii is December 30,
1984.
[53 PR, 43087, Oct. 25, 1988. as amended at 58
FR 9414, Mar. 6, 1981]
Subpart N—Idaho
§ 147.650 State-administrative pro-
gram—Class I, II, III, IV, and V
wells.
The UIC program for Class I, II, III,
IV, and V wells in the State of Idaho,
other than those on Indian lands, is the
program administered by the Idaho De-
partment of Water Resources, approved
by EPA pursuant to section 1422 of the
SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
June 7, 1985; the effective date of this
program is July 22, 1985. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Idaho. This incorporation
by reference was approved by the Di-
rector of the Federal Register effective
July 22, 1985.
(1) Public Writings, Title 9, Chapter
3, Idaho Code, sections 9-301 through 9-
302 (Boobs-Merrill 1979);
§147.650
(2) Crimes and Punishments, Title 18.
Chapter 1, Idaho Code, sections 18-113
through 18-114 (Bobbs-Merrill 1979 and
Supp. 1984);
(3) Department of Health and Wel-
fare, Title 39, Chapter 1, Idaho Code,
Chapter 39-108 (Bobbs-Merrill 1977);
(4) Drainage-Water Rights and Rec-
lamation, Title 42, Chapter 2, Idaho
Code sections 42-237(e): section 42-238
(Bobbs-Merrill 1977 and Supp. 1984);
(5) Department of Water Resources-
Water Resources Board, Title 42, Chap-
ter 17. Idaho Code, sections 42-1701, 42-
1703, 42-1735 (Bobbs-Merrill 1977, section
42-1701A (Supp. 1984);
(6) Director of Department of Water
Resources, Title 42, Chapter 18, Idaho
Code, sections 42-1801 through 42-1805
(Bobbs-Merrill 1977);
(7) Waste Disposal and Injection
Wells, Title 42, Chapter 39, Idaho Code,
sections 42-3901 through 42-3914 (Bobbs-
Merrill 1977), sections 42-3915 through
42-3919 (Supp. 1984);
(8) Idaho Trade Secrets Act, Title 48,
Chapter 8, Idaho Code, sections 48-801
through 48-807 (Bobbs-Merrill 1977 and
Supp. 1984);
(9) Administrative Procedure, Title
67, Chapter 52, Idaho Code, sections
67-5201 through 67-5218 (Bobbs-Merrill
1980 and Supp. 1984);
(10) Idaho Radiation Control Regula-
tions (IRCR section 1-9002.70; sections
1-9100 through 1-9110. Department of
Health and Welfare (May 1981);
(11) Rules and Regulations: Construc-
tion and Use of Injection Wells. Idaho
Department of Water Resources, Rules
1 through 14 (August 1984);
(12) Rules and Regulations: Practice
and Procedures, Idaho Department of
Water Resources, Rules 1 through 14
(October 1983).
(b) The Memorandum of Agreement
between EPA and Region X and the
Idaho Department of Water Resources
signed by the EPA Regional Adminis-
trator on February 11, 1985.
(c) Statement of legal authority. (1) The
Idaho Attorney General's Statement
for the Underground Injection Control
Program, October 31, 1984.
(2) Letter from David J. Barber, Dep-
uty Attorney General, Idaho Depart-
ment of Water Resources to Harold
749
-------
§ 147.651
40 CFR Ch. I (7-1-04 Edition)
Scott, EPA, Region 10, revising the At-
torney General's Statement, February
14, 1985.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[50 PR 23957, June 7, 1985]
§ 147.651 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Idaho is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CFR parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements,
(b) Effective dates. The effective date
of the UIC program for Indian lands In
Idaho is June 11, 1984.
[52 PR 17881, May 11, 1987. as amended at 56
FE 9414, Mar. 6, 1991]
§ 147.652 Aquifer exemptions. [Re-
served]
Subpart O—Illinois
§ 147.700 State-administered pro-
gram—Class I, III, IV, and V wells,
The UIC program for Class I, III, IV
and V wells in the State of Illinois,
except those on Indian lands, is the
program administered by the Illinois
Environmental Protection Agency, ap-
proved by EPA pursuant to section 1422
of the SDWA. Notice of the approval
was published in the FEDERAL REG-
ISTER on February 1, 1984 (49 PR 3991);
the effective date of this program is
March 3, 1984. This program consists of
the following elements, as submitted to
EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the state stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Illinois. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Illinois Environmental Protection
Act, Illinois ch. lllVa, sections 1001 to
1051 (Smith-Kurd 1977 Revised Statutes
and Supp. 1983). as amended by Public
Act No. 83-431, 1983 Illinois Legislative
Service, pages 2910 to 2916 (West);
(2) Illinois Pollution Control Board
Rules and Regulations at Title 35. Illi-
nois Administrative Code, Chapter I,
Part 700, Outline of Waste Disposal
Regulations; Part 702, RCRA and UIC
Permit Programs; Part 704, UIC Permit
Program; Part 705. Procedures for Per-
mit Issuance and Part 730, Under-
ground Injection Control Operating- Re-
quirements as amended by IPCB Order
No. R-83039 on December 15, 1983.
(b) The Memorandum of Agreement
between EPA Region V and the Illinois
Environmental Protection Agency,
signed by the EPA Regional Adminis-
trator on March 22, 1984.
(c) Statement of legal authority. Letter
from Illinois Attorney General to Re-
gional Administrator, EPA Region V,
and attached statement, December 18,
1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 53
FB 43087, Oct. 25, 1988]
§ 147,701 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Illinois, except those on
Indian lands, is the program adminis-
tered by the Illinois Environmental
Protection Agency, approved by EPA
pursuant to section 1425 of the SDWA.
Notice of the approval was published in
the FEDERAL REGISTBB on February 1,
1984 (49 FR 3990); the effective date of
this program is March 3, 1984. This pro-
gram consists of the following ele-
ments, as submitted to EPA in the
state's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State Stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Illinois. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
750
-------
Environmental Protection Agency
§147.750
(1) Conservation of Oil and Gas, etc.,
Illinois Revised Statutes eh. 96%, sec-
tions 5401 to 5457 (Smith-Kurd 1979 and
Siipp. 1983). as amended by Public Act
No. 83-1074 1983 Illinois Legislative
Service pages 7183 to 7185 (West);
(2) Illinois Environmental Protection
Act, Illinois Revised Statutes ch. lll-Va,
sections 100H051 (Smith-Hurd 1977 and
Supp. 1983), as amended by Public Act
No. 83-431, 1983 Illinois Legislative
Services pages 2910 to 2918 (West);
(3) Illinois Revised Statutes ch. 100V2,
section 26 (Smith-Hurd Supp. 1983);
(4) Illinois Department of Mines and
Minerals Regulations for the Oil and
Gas Division, Rules I. II, IIA. Ill, V,
VII, and IX (1981).
(b) The Memorandum of Agreement
between EPA Reg-ion V and the Illinois
Department of Mines and Minerals.
signed by the EPA Regional Adminis-
trator on March 22,1984.
(c) Statement of legal authority. "Cer-
tification of Legal Authority," signed
by State Attorney, Richland County,
Illinois, May 5, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43087, Oct. 25, 1988]
§ 147.703 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Illinois is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
for the UIC program for Indian lands is
November 25, 1988.
[53 PR 43087. Oct. 25, 1988. as amended at 56
FR 9414, Mar. 6, 1991]
Subpart P—Indiana
§ 147.750 State-administered pro-
gram—Class II wells.
The UIC program for Class II injec-
tion wells in the State of Indiana on
non-Indian lands is the program admin-
istered by the Indiana Department of
Natural Resources (INDR) approved by
the EPA pursuant to section 1425 of the
SDWA. Notice of this approval was
published in the PR on August 19, 1991;
the effective date of this program is
August 19, 1991. This program consists
of the following elements, as submitted
to EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Indiana. This incorpora-
tion by reference was approved by the
Director of the FR in accordance with
5 U.S.C. 552(a) and 1 CFR part 51. Cop-
ies may be obtained at the Indiana De-
partment of Natural Resources, Divi-
sion of Oil and Gas, 402 West Wash-
ington Street, room 293, Indianapolis,
Indiana, 46204. Copies may be inspected
at the Environmental Protection Agen-
cy, Region Y, 77 West Jackson Boule-
vard, Chicago, Illinois, 60604, or at the
National Archives and Records Admin-
istration (NARA). For information on
the availability of this material at
NARA. call 202-741-6030, or go to: Mtp://
www.archives.gcr-/federal register/
code of__federal regulations/
ibr locations.html,
(1) Indiana Code, title 4. article 21.5,
chapters 1 through 6 (1988).
(2) West's Annotated Indiana Code.
title 13, article 8, chapters 1 through 15
(1990 and Cumm. Supp. 1990).
(3) Indiana Administrative Code, title
310. article 7, rules 1 through 3 (Cumm.
Supp. 1991).
(b) Memorandum of agreement. The
Memorandum of Agreement between
EPA Region V and the Indiana Depart-
ment of Natural Resources signed by
the EPA Regional Administrator on
February 18, 1991.
(c) Statement of legal authority. State-
ment and Amendment to the State-
ment from the Attorney General of the
State of Indiana, signed on July 12,
1890, and December 13. 1990, respec-
tively.
(d) The Program Description and any
other materials submitted as part of
751
-------
§147.751
40 CFR Ch. I (7-1-04 Edition)
the original application or as supple-
ments thereto.
[56 FB 41072, Aug. 19, 1991, as amended at 62
FR 1834, Jan. 14, 1997]
§ 147.751 EPA-administered program.
(a) Contents, The UIC program for all
classes of wells on Indian lands, and for
Class I, III, IV, and V wells on non-In-
dian lands in the State of Indiana is ad-
ministered by the EPA. The program
consists of the UIC program require-
ments of 40 CFR parts 124, 144, 146, and
148 and the additional requirements set
forth in the remainder of this subpart.
Injection well owners and operators,
and EPA shall comply with these re-
quirements.
(b) Effective dates. The effective date
for the UIC program on Indian lands is
November 25, 1988. The effective date of
the UIC program for the rest of Indiana
is June 25, 1984.
[53 PR 43087, Oct. 25. 1988, as amended at 56
FR 9414, Mar. 6, 1991: 56 FR 41072, Aug. 19,
1991]
§147.752 Aquifer exemptions. [Re-
served]
§ 147.753 Existing Class I and III wells
authorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lessor of:
(a) A value which will not exceed the
operating requirements of § 144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.800-0,433 Sg)d
where:
Pm=injeetion pressure at the wellhead in
pounds per square Inch
Sg-=specific gravity of injected fluid
(unitless)
d=injection depth in feet.
[49 FR 20197, May 11, 1984, as amended at 66
FR 41072. Aug. 19, 1991}
Subpart Q—Iowa
§ 147.800 State-administered program.
[Reserved]
§ 147.801 EPA-administered program.
(a) Contents. The UIC program for the
State of Iowa, including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CPR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
for the UIC program for all lands in
Iowa, including Indian la.nds, is June
25, 1984.
[52 FR 17681, May 11. 1987, as amended at 56
PR 9415, Mar. 6, 1991]
§ 147.802 Aquifer exemptions. [Re-
served]
Subpart R—Kansas
§ 147.850 State-administered pro-
gram—Class I, III, W and V wells.
The UIC program for Class I, HI, IV
and V wells in the State of Kansas, ex-
cept those on Indian lands as described
in §147.860, is the program adminis-
tered by the Kansas Department of
Health and Environment, approved by
EPA pursuant to section 1422 of the
SDWA, Notice of this approval was
published in the FEDERAL BEGISTER on
December 2, 1983 (48 PR 54350): the ef-
fective date of this program is Decem-
ber 2, 1983. This program, consists of the
following elements, as submitted to
EPA in the State's program applica-
tion.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Kansas. This incorporation
by reference was approved by the
Director of the OPR in accordance with
5 U.S.C. 552(a) and 1 CPR part 51. Cop-
ies may be obtained at the Kansas De-
partment of Health and Environment,
Forbes Field, Building 740, Topeka,
Kansas, 66620. Copies may be inspected
at the Environmental Protection Agen-
cy, Region VII, 726 Minnesota Avenue,
Kansas City, Kansas, 66101, or at the
National Archives and Records Admin-
istration (NARA). For information on
the availability of this material at
NARA, call 202-741^6030, or go to: http://
www.archives.gov/federal register/
752
-------
Environmental Protection Agency
§147.901
code_ of _federal regulations/
ibr locations.hind.
(1) Chapter 28, Article 46, Under-
ground Injection Control Regulations,
Kansas Administrative Regulations
§§28-46-1 through 28-46-42 (1986 and
Supp. 1987);
(2) Chapter 28, Article 43, Construc-
tion, operation, monitoring' and aban-
donment of salt solution mining wells,
Kansas Administrative Regulations
§§28-43-1 through 28-43-10 (1986);
(3) Kansas Statutes Annotated §§65-
161, 65-164 through 65~166a, 65-171(1 (1980
and Cumm. Supp. 1989).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for the se-
lect sections identified in paragraph (a)
of this section, are also part of the ap-
proved State-administered program:
Kansas Statutes Annotated §§65-161
through 65-171(w), (1980 and Supp. 1983).
(c) Memorandum of Agreement. (1) The
Memorandum of Agreement between
EPA Region VII and the Kansas De-
partment of Health and Environment,
signed by the EPA Regional Adminis-
trator on July 29, 1983;
(2) Addendum No. 1 of the Memo-
randum of Agreement, signed by the
EPA Regional Administrator on Au-
gust 29, 1983.
(d) Statement of legal authority. (1)
"Statement of Attorney General",
signed by the Attorney General of the
State of Kansas, November 25, 1981;
(2) "Supplemental Statement of At-
torney General", signed by the Attor-
ney General of the State of Kansas, un-
dated (one page).
(e) Program description. The program
description and any other materials
submitted as part of the application or
supplements thereto.
[49 FB 45306, Nov. 15. 1984, as amended at 56
FR 9415, Mar. 6, 1991]
§ 147.851 State-administered pro-
gram—Class II wells,
The UIC program for Class II wells in
the State of Kansas, except those on
Indian lands as described in §147.860, is
the program administered by the Kan-
sas Corporation Commission and the
Kansas Department of Health and En-
vironment, approved by EPA pursuant
to section 1425 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on February 8, 1984 (49
FR 4735); the effective date of this pro-
gram is February 8, 1984. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application.
[49 FR 45306, Nov. 15, 1984]
§§ 147.852-147.859 [Reserved]
§147.860 EPA-administered program-
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Kansas is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Kansas is December 30, 1984.
[49 FR 45307, Nov. 15, 1984, as amended at 56
FB 9415. Mar. 6, 1991]
Subpart S—Kentucky
§ 147.900 State-administered program.
[Reserved]
§ 147.901 EPA-administered program.
(a) Contents. The UIC program for the
Commonwealth of Kentucky, including
all Indian lands, is administered by
EPA. This program consists of the UIO
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
for the UIC program on Indian lands is
November 25, 1988. The effective date
for the UIC program in the remainder
of Kentucky is June 25, 1984.
[53 FB 43087, Oct. 25, 1988, as amended at 56
FR 9415, Mar, 6, 1991]
753
-------
§147.902
40 CFR Ch. 1 (7-1-04 Edition)
§147,902 Aquifer
served]
exemptions, [Re-
§147,903 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of § 144.28(f)(3)
(i) or (ii) as applicable or;
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.733-0.433 Sg-)d
where;
Pm=injeetion pressure at the well head in
pounds per square inch
Sg=speeific gravity of inject fluid (unitless)
d=lnjection depth in feet.
§147.904 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule,
(a) Maximum injection pressure. (I) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter,
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(il) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of § 144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within 1 year of the effective date of
this program.
(b) Casing and Cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs t>y:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between and the cas-
ing the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
754
-------
Environmental Protection Agency
§147,950
of this section, as needed to protect
USDWs.
§ 147.905 Requirements for all wells—
area of review.
Notwithstanding the alternatives
presented in §146.6 of this chapter, the
area of review shall be a minimum
fixed radius as described in §146.6(b) of
this chapter.
Subpart T—Louisiana
§ 147.950 State-administered program,
The UIC program for Class I, II, III,
IV, and V wells in the State of Lou-
isiana, except those wells on Indian
lands, is the program administered by
the Louisiana Department of Natural
Resources approved by EPA pursuant
to sections 1422 and 1425 of the SDWA.
Notice of this approval was published
in the FEDERAL REGISTER on April 23,
1982 (47 PR 17487); the effective date of
this program is March 23, 1982, This
program consists of the following ele-
ments, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Louisiana. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Louisiana Revised Statutes Anno-
tated sections 30:1-30:24 (1975 and Supp.
1982);
(2) Underground Injection Control
Program Regulations for Class I, III,
IV, and V wells. Statewide Order No.
29-N-l (February 20, 1982), as amended
June 1, 1985 and January 20, 1986;
(3)(i) Statewide Order Governing the
Drilling for and Producing of Oil and
Gas in the State of Louisiana, State-
wide Order No. 29-B (August 26, 1974)
(Composite Order Incorporating
Amendments through March 1, 1974);
(ii) Amendments to Statewide Order
No. 29-B (Off-site Disposal of Drilling
Mud and Salt Water Generated from
Drilling and Production of Oil and Gas
Wells) (effective July 20, 1980);
(ill) Amendment to Statewide Order
No. 29-B (Amendment concerning the
use of Tables 5A and 6A, etc.) (Decem-
ber 15, 1980, effective January 1, 1981);
(iv) Amendment to Statewide Order
No. 29-B (Amendment concerning the
underground injection control of salt-
water disposal wells, enhanced recov-
ery injection wells, and liquid hydro-
carbon storage wells) (effective Feb-
ruary 20, 1982);
(v) Amendment to Statewide Order
No. 29-B (Amendment concerning the
offsite disposal of drilling mud and
saltwater) (effective May 20, 1983);
(vi) Amendment to Statewide Order
No. 29-B (Amendment concerning dis-
posal of nonhazardous oilfield waste)
(March 20, 1984, effective May 20, 1984);
(vii) Amendment to Statewide Order
No. 29-B (Amendment concerning the
administrative approval of injectivity
tests and pilot projects in order to de-
termine the feasibility of proposed en-
hanced recovery projects) (June 20,
1985, effective July 1, 1985).
(4) (i) Statewide Order adopting rules
and regulations pertaining to the use
of salt dome cavities (i.e., storage
chambers) for storage of liquid and/or
gaseous hydrocarbons, etc., Statewide
Order No. 29-M (July 6, 1977, effective
July 20, 1977):
(ii) Supplement to Statewide Order
No. 29-M (October 2, 1978);
(iii) Second Supplement to Statewide
Order No. 29-M (June 8, 1979).
(b)(l) The Memorandum of Agree-
ment (Class I. Ill, IV, and V wells) be-
tween EPA Region VI and the Lou-
isiana Department of Natural Re-
sources, Office of Conservation, signed
by the EPA Regional Administrator on
March 17, 1982 and amended by Adden-
dum 1 and Addendum 2 on November 3.
1989;
(2) The Memorandum of Agreement
(Class II wells) between EPA Region VI
and the Louisiana Department of Nat-
ural Resources, Office of Conservation,
signed by the EPA Regional Adminis-
trator on March 17,1982.
(c) Statement of legal authority. (1)
Letter from Attorney General of Lou-
isiana to EPA, "Re: Louisiana Under-
ground Injection Control Program Au-
thorization for State of Louisiana"
(Class I, m, IV and V Wells), January
13, 1982, (10 pages);
755
-------
§147.951
40 CFR Ch. I (7-1-04 Edition)
(2) Letter from Attorney General of
Louisiana to EPA, "Re: Louisiana Un-
derground Injection Control Program
Authorization for State of Louisiana"
(Class II Wells), January 13, 1982 (5
pages).
(3) Letter from Attorney General of
Louisiana to EPA, "Re: Class I Haz-
ardous Waste Injection Well Regu-
latory Program; Attorney General's
Statement, October 9, 1989 (9 pages);
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 56
FR 9415. Mar. 6, 1991]
§147.951 EPA-administered program—
Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Louisiana is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
of the UIC program for Indian lands in
Louisiana is November 25, 1988.
[53 FR 43087, Oct. 25, 1988, as amended at 56
FR 9415, Mar. 6, 1991]
Subpart U—Maine
1147.1000 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of Maine, except
tho.se on Indian lands, is the program
administered by the Maine Department
of Environmental Protection approved
by EPA pursuant to section 1422 of the
SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
August 25, 1983 (48 FR 38641); the effec-
tive date of this program is September
26, 1983. This program consists of the
following elements, as submitted to
EPA in the State's program applica-
tion.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated toy ref-
erence and made part of the applicable
UIC program under the SDWA for the
State of Maine. This incorporation by
reference was approved by the Director
of the OFR on June 25, 1984.
(1) Maine Revised Statutes Anno-
tated title 38. sections 361-A, 363-B, 413.
414, 414-A, 420, and 1317^A (1978);
(2) Rules to Control the Subsurface
Discharge of Pollutants by Well Injec-
tion, Rules of the Department of Envi-
ronmental Protection, Chapter 543
(adopted June 22, 1983, effective July 4,
1983).
(b) The Memorandum of Agreement
between BPA Region I and the Maine
Department of Environmental Protec-
tion, signed toy the EPA Regional Ad-
ministrator on May 16, 1983,
(c) Statement of legal authority. Letter
from Attorney General of Maine to
EPA Regional Administrator, "Re: At-
torney General's Statement: Maine Un-
derground Injection Control Program
Primacy Application," June 30, 1983.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto,
[49 FR 20197, May 11. 1984. as amended at 53
FK 43088, Oct. 25, 1988: 56 FE 9415, Mar, 6.
1991]
§ 147.1001 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Maine is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CFR parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
of the UIC program for Indian lands in
Maine is November 25. 1988.
[53 FR 43088, Oct. 25, 1988, as amended at 56
FR 9416, Mar. 6, 1991]
Subpart V—Maryland
§ 147.1050 State-administered pro-
gram—Class I, II, HI, IV, and V
wells,
The UIC program for Class I, II, III,
IV, and V wells in the State of Mary-
land, except those wells on Indian
756
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Environmental Protection Agency
§ 147,1100
lands, is the program administered by
the Maryland Department of the Envi-
ronment approved by EPA pursuant to
section 1422 of the SDWA. Notice of
this approval was published in the FR
on April 19, 1984 (49 PR 15553); the effec-
tive date of this program is June 4,
1984. This program consists of the fol-
lowing- elements, as submitted to EPA
in the State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Maryland. This incorpora-
tion by reference was approved by the
Director of the OFB in accordance with
5 U.S.C. 552(a) and 1 CPR part 51. Cop-
ies may be obtained at the Maryland
Department of the Environment, 2500
Broening- Highway, Baltimore, Mary-
land, 21224. Copies may be inspected at
the Environmental Protection Agency,
Region HI, 841 Chestnut Street, Phila-
delphia, Pennsylvania, 19107. or at the
National Archives and Records Admin-
istration (NARA). For information on
the availability of this material at
NARA, call 202-741^6030. or go to: Mtp://
www.archives.gov/federal register/
code__af_Jederal regulations/
ibr locations.html.
(1) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 07 pro-
mulgated and effective as of Marcli 1,
1989;
(2) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 01, pro-
mulgated and effective as of March 1,
198S;
(3) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 02, pro-
mulgated and effective as of March 1,
1989;
(4) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 03. pro-
mulgated and effective as of March 1,
1989;
(5) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 04, pro-
mulgated and effective as of March 1,
1989;
(6) Code of Maryland Regulations,
Title 26, Subtitle 13. Chapter 05, section
.19, promulgated and effective as of Au-
gust 1, 1989;
(7) Code of Maryland Regulations,
Title 26, Subtitle 01, Chapter 02, pro-
mulgated and effective as of March 1,
1989;
(8) Code of Maryland Regulations,
Title 26, Subtitle 01, Chapter 04, pro-
mulgated and effective as of March 1.
1989.
(b) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region III and the Maryland De-
partment of the Environment, as sub-
mitted on August 2, 1983, and revised
on February 16,1984.
(c) Statement of legal authority. State-
ment from the Maryland Attorney
General on the Underground Injection
Control Program, as submitted on Au-
gust 2, 1983. and revised on February 16,
1984.
(d) Program Description. The Program
Description and other materials sub-
mitted as part of the application or as
supplements thereto.
[56 FR 9416, Mar. 6, 1991]
§§ 147.1051-147,1052 [Reserved]
§147.1053 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Maryland is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146. 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Maryland is November 25, 1988.
[53 FR 43088, Oct. 25, 1988, as amended at 56
FR 9416. Mar. 6, 1991]
§§ 147.1054-147.1099 [Reserved]
Subpart W—Massachusetts
§ 147.1100 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of Massachusetts, ex-
cept those on Indian lands, is the pro-
gram administered by the Massachu-
setts Department of Environmental
Protection, approved by EPA pursuant
to section 1422 of the SDWA. Notice of
757
-------
§147.1101
40 CFR Ch. i (7-1-04 Edition)
this approval was published in the FED-
ERAL REGISTER on November 23, 1982 (47
PR 52705); the effective date of this pro-
gram is December 23, 1982, This pro-
gram consists of the following ele-
ments, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Massachusetts, This incor-
poration by reference was approved by
the Director of the Federal Register on
June 25, 1984.
(1) Massachusetts General Laws An-
notated chapter 21, sections 27, 43, and
44 (West 1981);
(2) Code of Massachusetts Regula-
tions, title 310, sections 23.01-23.11 as
amended April 26, 1982.
(b) The Memorandum of Agreement
between EPA Region I and the Massa-
chusetts Department of Environmental
Quality Engineering, signed by the
EPA Regional Administrator on Au-
gust 18, 1982.
(c) Statement of legal authority, "Un-
derground Injection Control Program—
Attorney General's Statement for
Class I, II, III, IV and V Injection
Wells," signed by Assistant Attorney
General for Attorney General of Massa-
chusetts, May 13, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43088, Oct. 25, 1988]
§147.1101 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Massachusetts is administered
by EPA. This program consists of the
UIC program requirements of 40 CFR
parts 124, 144, 146, 148, and any addi-
tional requirements set forth In the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Massachusetts is November 25, 1988.
[53 FR 43088, Oct. 25. 1988, as amended at 56
FR 9416, Mar. 6, 1991]
Subpart X—Michigan
§ 147.1150 State-administered
gram. [Reserved]
pro-
§ 147,1151 EPA-administered program.
(a) Contents. The UIC program for the
State of Michigan, including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CPR parts 124, 144.
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
for the UIC program for all lands in
Michigan, including Indian lands, is
June 25, 1984.
[52 FR 17681, May 11, 1987, as amended at 56
FR 9416, Mar, 6, 1991]
§ 147.1152 Aquifer exemptions, [Re-
served]
§147.1153 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of § 144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.800-0.433 Sg)d
where:
Pm=injection pressure at the well head in
pounds per square inch
Sg=8pecific gravity of injected fluid
(unitless)
d=injection depth In feet,
§147.1154 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§ 144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
758
-------
Environmental Protection Agency
§147.1201
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he Is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regonal Administrator that such injec-
tion pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124. subpart A
of this chapter.
(2) Prior to such time as the Regional
Administrator establishes field rules
for maximum injection pressure based
on data provided pursuant to para-
graph (a)(2)(ii) of this section the
owner or operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within 1 year following the effective
date of this program.
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage will may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone: and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone,
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section, as needed to protect
USDWs.
i 147.1155 Requirements for all wells.
(a) Area of review. Notwithstanding
the alternatives presented in §146,6 of
this chapter, the area of review for
Class II wells shall be a fixed radius as
described in §146.6(b) of this chapter.
(b) Tubing and packer. The owner or
operator of an injection well injecting
salt water for disposal shall inject
through tubing and packer. The owner
of an existing well must comply with
this requirement within one year of the
effective date of this program.
Subpart Y—Minnesota
§ 147.1200 State-administered
gram. [Reserved]
pro-
§ 147.1201 EPA-administered program.
(a) Contents. The UIC program for the
State of Minnesota is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
759
203-160 D-25
-------
§147.1202
40 CFR Ch. I (7-1-04 Edition)
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Minnesota is:
June 11, 1984.
[49 FR 20197, May 11, 1984, as amended at 56
PB 9416. Mar. 6. 1991]
§ 147.1202 Aquifer exemptions. [Re-
served]
§147.1210 Requirements for Indian
lands.
(a) Purpose and scope. This section
sets forth additional requirements that
apply to injection activities on Indian
lands in Minnesota.
(b) Requirements. Notwithstanding
the other requirements of this subpart,
for Indian lands described in paragraph
(a) of this section, no owner or oper-
ator shall construct, operate, main-
tain, or convert any Class I, II, III, or
IV well. The UIC program for Class V
wells on such Indian Lands is adminis-
tered by EPA, and consists of the appli-
cable requirements of 40 CFR parts 124,
144, and 146, In addition, no owner or
operator shall abandon a well without
the approval of the Regional Adminis-
trator.
(c) Effective date. The effective date of
the UIC program requirements for In-
dian lands in Minnesota is December
30, 1984.
[49 FR 45307, Nov. 15, 1984]
Subpart Z—Mississippi
§ 147.1250 State-administered pro-
gram—Class I, III, IV, and V welts.
The UIC program for Class I, HI, IV
and V wells in the State of Mississippi,
except those on Indian lands, is the
program administered by the Mis-
sissippi Department of Natural Re-
sources approved by EPA pursuant to
section 1422 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on August 25, 1983 (48
FR 38641); the effective date of this pro-
gram is September 26, 1983. This pro-
gram consists of the following ele-
ments, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Mississippi. This incorpo-
ration by reference was approved by
the Director of the Federal Register on
June 25, 1984.
(1) Mississippi Air and Water Pollu-
tion Control Law, Mississippi Code An-
notated sections 49-17-1 through 49-17-
29 (1972) and Supp. 1983);
(2) Mississippi Department of Natural
Resources, Bureau of Pollution Con-
trol, Underground Injection Control
Program Regulations (adopted Feb-
ruary 11, 1982);
(3) Mississippi Department of Natural
Resources, Bureau of Pollution Con-
trol, State of Mississippi Wastewater
Permit Regulations for National Pol-
lutant Discharge Elimination System
(NPDES), Underground Injection Con-
trol (UIC), and State Operating Per-
mits (adopted May 1, 1974; amended
February 11, 1982).
(b) The Memorandum of Agreement
between EPA Region IV and the Mis-
sissippi Department of Natural Re-
sources, signed by the EPA Regional
Administrator on February 8,1983,
(c) Statement of legal authority. (1)
Letter from Attorney General of Mis-
sissippi (by Special Assistant Attorney
General) to Executive Director, Mis-
sissippi Department of Natural Re-
sources, "Re: Mississippi Department of
Natural Resources, Bureau of Pollution
Control, State Underground Injection
Control (UIC) Program; Statement of
the Attorney General of the State of
Mississippi," December 3, 1981;
(2) Letter from Attorney General of
Mississippi (by Special Assistant At-
torney General) to Executive Director,
Mississippi Department of Natural Re-
sources, "Re: Authority to Regulate
and Take Samples from Underground
Injection Systems," October 18, 1982;
(3) Letter from Attorney General of
Mississippi (by Special Assistant At-
torney General) to Regional Adminis-
trator, EPA Region IV, "Re: Public
Participation in State Enforcement
Actions, UIC Program," June 10, 1983.
(d) The Program Description and any
other materials submitted as part of
the application or supplements thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43088, Oct. 25, 1988]
760
-------
Environmental Protection Agency
§147.1300
§ 147.1251 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Mississippi, other than
those on Indian lands, is the program
administered by the State Oil and Gas
Board of Mississippi approved by EPA
pursuant to section 1425 of the SDWA,
Notice of this approval was published
in the FEDERAL REGISTER on March 2,
1989; the effective date of this program
is March 2, 1989. This prog'ram consists
of the following elements, as submitted
to EPA in the State's program applica-
tion:
(a) Incorporation by reference. The
requirements set forth in the State
statutes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Mississippi. This incorpo-
ration by reference was approved by
the Director of the Federal Register in
accordance with 5 U.S.C. 552(a).
(1) Mississippi Code Annotated, sec-
tion 5-9-9 (Supp. 1988).
(2) Mississippi Code Annotated, sec-
tions 53-1-1 through 53-1-47, inclusive
and sections 53-1-71 through 53-1-77, in-
clusive (1972 and Supp. 1988).
(3) Mississippi Code Annotated, sec-
tions 53-3-1 through 53-3-165, inclusive
(1972 and Supp. 1988).
(4) State Oil and Gas Board State-
wide Rules and Regulations, Rules 1
through 65, inclusive (Aug. 1, 1987, as
amended, Sept. 17, 1987),
(b) The Memorandum of Agreement
between EPA Region IV and the State
Oil and Gas Board of Mississippi signed
by the Regional Administrator on Oc-
tober 31, 1988.
(c) Statement of legal authority.
Statement from the Attorney General
signed on October 1, 1987 with amend-
ments to the Statement signed August
5, 1988 and September 15, 1988 by the
Special Assistant Attorney General,
(d) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[54 FR 8735, Mar. 2, 19891
§ 147.1252 EPA-administered pro-
gram—Indian lands.
(a) Contents, The UIC program for all
classes of wells on Indian lands in the
State of Mississippi is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program on Indian lands is
November 25. 1988.
[53 FR 8735, Mar. 2, 1989, as amended at 56 FR
9416, Mar. 6, 1991]
Subpart AA—Missouri
§ 147.1300 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of Missouri, except
those on Indian lands, is administered
by the Missouri Department of Natural
Resources, approved by EPA pursuant
to section 1422 and 1425 of the SDWA,
Notice of this approval was published
in the FEDERAL REGISTER on December
2. 1983 (48 PR 54349); the effective date
of this program is December 2, 1983).
This program consists of the following
elements, as submitted to EPA in the
State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Missouri. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Vernon's Annotated Missouri
Statutes sections 259.010 to 259.240
(Supp. 1984);
(2) Missouri Code of State Regula-
tions, title 10, division 50. chapters 1
and 2 (June 1984):
(3) Yernon's Annotated Missouri
Statutes chapter 204. §§204.006 through
204.470 (1983 and Cumm. Supp. 1990).
(b) The Memorandum of Agreement
between EPA Region VII and the Mis-
souri Department of Oil and Gas,
761
-------
§147.1301
40 CFR Ch. I (7-1-04 Edition)
signed by the EPA Regional Adminis-
trator on December 3, 1982.
(c) Statement of legal authority, (1)
Opinion Letter No, 63 and attached
Memorandum Opinion, signed by At-
torney General of Missouri, March 16,
1982;
(2) Addendum to Opinion Letter No,
63 (1982), signed by Attorney General of
Missouri, October 28, 1982,
(3) Opinion No. 127-83, signed by At-
torney General of Missouri, July 11,
1983.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FB 20197, May 11, 1984, as amended at 53
PR 43088, Oct. 25, 1988; 56 FB 9416, Mai', 6,
1991]
§ 147.1301 State-administered pro-
gram—Class I, ID, IV, and V wells,
The UIC program for Class I, III, IV,
and V wells in the State of Missouri,
other than those on Indian lands, is the
program administered by the Missouri
Department of Natural Resources, ap-
proved by EPA pursuant to section 1422
of the SDWA. Notice of this approval
was published in the FEDERAL REG-
ISTER on November 2, 1984; the effective
date of this program is July 31, 1985.
This program consists of the following'
elements, as submitted to EPA in the
State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited In this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Missouri. This incorpora-
tion by reference was approved by the
Director of the Federal Register effec-
tive July 31, 1985.
(1) Revised Statutes of the State of
Missouri, Volume 2, sections 204.016,
204.026, 204.051, 204.056 and Volume V,
section 577.155 (1978 and Cumm, Supp.
1984);
(2) Missouri Code of State Regula-
tions, title 10, division 20, Chapter 6,
sections 20-5.010, 20-6.020, 20-6,070, 20-
6.080, 20-6.090, and title 10, division 20,
Chapter 7, section 20-7.031 (1977, amend-
ed 1984).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for select
sections identified in paragraph (a) of
this section, are also part of the ap-
proved State-administered program.
(1) Revised Statutes of the State of
Missouri, chapters 204, 260, 536, 557, 558
and 560; sections 640.130,1 and 1.020 (1978
and Cumm. Supp. 1984);
(2) Rule 52.12 Vernon's Annotated
Missouri Rules (1978);
(3) Missouri Code of State Regula-
tions, title 10, division 20, Chapters 1
through 7 (1977, amended 1984).
(c) The Memorandum of Agreement
between EPA Region VII and the Mis-
souri Department of Natural Re-
sources, signed by the EPA Regional
Administrator on October 10,1984.
(d) Statement of Legal Authority. Opin-
ion No. 123-84, signed by Attorney Gen-
eral of Missouri, September 24, 1984.
Amended April 2, 1985.
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[50 FB 28942, July 17, 1985J
§147.1302 Aquifer exemptions. [Re-
served]
§ 147.1303 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Missouri is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 145, 146, 148, and any additional
requirements set forth in the remain-
der of this subpart. Injection well own-
ers and operators, and EPA shall com-
ply with these requirements.
(b) Effective date. The effective date
for the UIC program for Indian lands is
November 25,1988.
[53 PB 43088, Oct. 25, 1988, as amended at 56
PR 9417, Mar. 6, 1991]
Subpart BB—Montana
§ 147.1350 State-administered pro-
grams—Class II wells.
The UIC program for Class II injec-
tion wells in the State of Montana, ex-
cept for those in Indian Country, is the
program administered by the Montana
Board of Oil and Gas Conservation
762
-------
Environmental Protection Agency
§147.1352
(MBOGC) approved by the EPA pursu-
ant to Section 1425 of the SDWA. No-
tice of this approval was published in
the FEDEHAL REGISTER on November 19.
1996; the effective date of this program
is November 19, 1996, This program con-
sists of the following elements as sub-
mitted to EPA in the State's program
application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made part of the applicable
UIC program under the SDWA for the
State of Montana, This incorporation
by reference was approved by the Di-
rector of the FR in accordance with 5
U.S.C. 552(a) and 1 OPR part 51. Copies
may be obtained at the Montana Board
of Oil and Gas Conservation, 2535 St.
Johns Avenue, Billings, Montana,
59102. Copies may "be inspected at the
Environmental Protection Agency, Re-
gion VIII, 999 18th Street. Suite 500,
Denver, Colorado, 80202-2466, or at the
National Archives and Records Admin-
istration (NARA). For information on
the availability of this material at
NARA, call 202-741^6030, or go to: http://
www.archives.gov/federal register/
code of ^federal Regulations/
ibr iocalions.html.
(1) Montana Statutory Requirements
Applicable to the Underground Injec-
tion Control Program, August, 1996.
(2) Montana Regulatory Require-
ments Applicable to the Underground
Injection Control Program, August,
1996.
(b) Memorandum of Agreement (MOA).
(1) The MOA between EPA Region VIII
and the MBOGC signed by the Acting
EPA Regional Administrator on June
9, 1996.
(2) Letter dated May 24, 1996, from
the Administrator of the MBOGC and
the attached addendum (Addendum No.
1-96) to the MOA between MBOGC and
EPA Region VIII, signed by the Acting
EPA Regional Administrator on Au-
gust 14. 1996.
(c) Statement of legal authority. (Ti
Letter from the Montana Attorney
General to the Regional Administrator
dated August 1, 1995.
(2) MBOGC independent counsel's cer-
tification of Montana's UIC program
for Class II wells dated July 24, 1995.
(3) Letter dated March 8,1996, from
MBOGC independent counsel to
USEPA, Region VIII; "Re: EPA com-
ments of November 29, 1995, on Mon-
tana Class II primacy application."
(4) Letter dated March 8. 1996, from
the Administrator of the MBOGC and
the attached proposed replacement lan-
guage for the MOA; "Re: Responses to
EPA comments on Montana Class II
Primacy Application."
(d) Program Description. The Program
Description and any other materials
submitted as part of the application or
as supplemented thereto:
(1) Application and accompanying
materials for approval of Montana's
UIC program for Class II wells sub-
mitted by the Governor of Montana,
August 3, 1995.
(2) [Reserved]
[61 FE 58933, Nov. 19, 1996J
§ 147.1351 EPA-adtninistered program,
(a) Contents. The UIC program in the
State of Montana for Class I, III, IV.
and V wells, and for all Classes of wells
in Indian Country is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146. 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements,
{b) Effective dates. The effective date
for the UIC program on all lands in
Montana, including all Indian lands, is
June 25, 1984.
[52 FR 17681, May 11. 1987, as amended at 56
FR 9417. Mar. 6, 1991; 61 FR 58933, Nov. 19.
1996]
§ 147,1852 Aquifer exemptions.
Those portions of aquifers within
one-quarter mile of existing Class II
wells are exempted for the purpose of
Class II injection activities only.
NOTE: A complete listing of the exemptions
and their location is available for review in
the EPA Regional Office, 1860 Lincoln Street,
Denver, Colorado. An updated list of exemp-
tions will be maintained in the Regional
Office.
763
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§147.1353
40 CFR Ch. I (7-1-04 Edition)
§147.1363 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of § 144,28(f)(3)
(i) or (ii) as applicable or
(b) A value for well head pressure cal-
culated by using the following1 formula:
Pm=(Q.733 - 0.433 Sg)d
where:
Pm=injeetioxi pressure at the well head in
pounds per square inch
Sg=specific gravity of inject fluid (unitless)
d=injection depth in feet.
§147.1364 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter.
(2) Prior to such time as the Regional
Administrator established rules for
maximum injection pressure based on
data provided pursuant to paragraph
(ii) below the owner or operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within 1 year of the effective date of
this program.
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall when
required by the Regional Adminis-
trator:
(1) Isolate all USDWs by placing ce-
ment between the outermost casing
and the well bore as follows:
(i) If the injection well is east of the
108th meridian, cement the outermost
casing from a point 50 feet into a major
shale formation underlying the upper-
most USDW to the surface. For the
purpose of this paragraph, major shale
formations are defined as the Bearpaw,
Clagget, and Colorado formations,
(ii) If the injection well is west of the
108th meridian, cement the outermost
casing to a depth of 1,000 feet, or to the
base of the lowermost USDW in use as
a source of drinking water whichever is
deeper. The Regional Administrator
may allow an owner or operator to
cement to a lesser depth if he can
demonstrate to the satisfaction of the
Regional Administrator that no USDW
will be affected by the injection
facilities.
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
764
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Environmental Protection Agency
Pt. 147, Subpt, BB, App, A
(ii) Which is resistant to deteriortion
from formation and injection fluids;
and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section, as needed to protect
USDWs.
§ 147.1355 Requirements for all wells,
(a) Area of review. Notwithstanding
the alternatives presented in §146.6 of
this chapter, the area of review shall be
a fixed radius as described in §146.06(b)
of this chapter.
(b) The applicant must give separate
notice of intent to apply for a permit
to each owner or tenant of the land
within one-quarter mile of the site.
This requirement may be waived by the
Regional Administrator where indi-
vidual notice to all land owners and
tenants would be impractical. The ad-
dresses of those to whom notice is
given, and a description of how notice
was given, shall be submitted with the
permit application. The notice shall
include:
(1) Name and address of applicant;
(2) A brief description of the planned
injection activities, including well lo-
cation, name and depth of the injection
zone, maximum injection pressure and
volume, and fluid to be injected;
(3) EPA contact person; and
(4) A statement that opportunity to
comment will be announced after EPA
prepares a draft permit.
(c) Owners and operators on or within
one-half mile of Indian lands shall pro-
vide notice as specified in paragraph
(b) of this section, except that such no-
tice shall be provided within a one-half
mile radius of the site.
APPENDIX A TO SUBFART BB OP PART
147—STATE REQUIREMENTS INCOR-
PORATED BY REFERENCE IN SUBPART
BB OF PART 147 OF THE CODE OF
FEDERAL REGULATIONS
The following is an informational listing of
state requirements incorporated by reference
in Suopart BB of part 147 of the Code of Fed-
eraJ Regulations:
Subpart BB—Montana
(a) The statutory provisions include:
(1) Montana Code annotated, 1995, Title 2.
Chapter 15;
Section 2-15-121. Allocation for administra-
tive purposes only.
Section 3-15-124. Quasi-judicial boards.
Section 2-15-3303. Board of oil and gas con-
servation-composition—allocation—quasi-ju-
dicial.
(2) Montana Code annotated, 1995, Title 82,
Chapter 10:
Section 82-10-101. Action for accounting for
royalty.
Section 82-10-102. Remedy not exclusive.
Section 82-10-103. Obligation to pay royal-
ties as essence of contract-interest.
Section 82-10-104. Payment of royalties-
form of record required.
Section 82-10-105 through 82-10-109 re-
served.
Section 82-10-110. Division order-defini-
tion-effect.
Section 82-10-201. Authorization for lease
and terms-land not subject to leasing.
Section 82-10-202. Acreage pooling.
Section 82-10-203. Interference with normal
use of land prohibited.
Section 82-10-204. Lease of acquired oil and
gas interests.
Section 82-10-301. Definitions.
Section 82-10-302. Policy.
Section 82-10-303. Use of eminent domain
to acquire underground reservoirs.
Section 82-10-304. Certificate of board re-
quired prior to use of eminent domain.
Section 82-10-305. Proceedings.
Section 82-10-401. Notice required before
abandonment of well-owner's option,
Section 82-10-402. Inventory of abandoned
wells and seismic operations-reclamation
procedures.
Section 82-10-501. Purpose-legislative find-
ing's.
Section 82-10-502. Definitions.
Section 82-10-503. Notice of drilling oper-
ations,
Section 82-10-504. Surface damage and dis-
ruption payments-penalty for late payment.
Section 82-10-505. Liability for damages to
property.
Section 82-10-506. Notification of injury.
Section 82-10--0507. Agreement—offer of set-
tlement.
Section 82-10-508. Rejection—legal action.
Section 82-10-509 and 82-10-510. Reserved.
Section 82-10-511. Remedies cumulative.
(3) Montana Code annotated, 1995. Title 82.
Chapter 11:
Section 82-11-101. Definitions.
Section 82-11-102. Oil or g-as wells not pub-
lic utilities.
Section 82-11-103. Lands subject to law.
Section 82-11-104. Construction-no conflict
with board of land commissioners' authority.
Section 82-11-105 through 82-11-110 re-
served.
765
-------
Pf. 147, Subpt. BB, App. A
40 CFR Ch. I (7-1-04 Edition)
Section 82-11-111. Powers and duties of
board.
Section 82-11-112, Intergovernmental co-
operation.
Section 82-11-113, Role of board in imple-
mentation of national gas policy.
Section 82-11-114. Appointment of exam-
iners.
Section 82-11-115. Procedure to make de-
terminations.
Section 82-11-116. Public access.
Section 82-11-117. Confidentiality of
records.
Section 82-11-118. Pees for processing appli-
cations.
Section 82-11-119 through 82-11-120 re-
served.
Section 82-11-121. Oil and gas waste prohib-
ited.
Section 82-11-122. Notice of intention to
drill or conduct seismic operations-notice to
surface owner.
Section 82-11-123. Requirements for oil and
gas operations.
Section 82-11-124. Requirement relating- to
waste prevention.
Section 82-11-125. Availability of cores or
chips, cuttings, and bottom-hole tempera-
tures to board.
Section 82-11-126. Availability of facilities
to bureau of mines.
Section 82-11-127. Prohibited activity.
Section 82-11-128 through 82-11-130 re-
served.
Section 82-11-131. Privilege and license tax.
Section 82-11-132. Statements to treasurer
and payment of tax.
Section 82-11-133. Penalty for late pay-
ment.
Section 82-11-134. Permit fees.
Section 82-11-135. Money earmarked for
board expenses.
Section 82-11-136. Expenditure of funds
from bonds for plugging wells.
Section 82-11-137. Class II injection well
operating fee.
Section 82-11-138 through 82-11-140 re-
served.
Section 82-11-141. Administrative proce-
dure.
Section 82-11-142, Subpoena power-civil ac-
tions.
Section 82-11-143. Rehearing.
Section 82-11-144. Court review.
Section 82-11-145. Injunction or restraining
order.
Section 82-11-146. Appeal.
Section 82-11-147. Violations.
Section 82-11-148. Criminal penalties.
Section 82-11-149. Civil penalties.
Section 82-11-150. Legal assistance.
Section 82-11-151. Emergencies-notice and
hearing.
Section 82-11-152 through 82-11-160 re-
served.
Section 82-11-161. Oil and gas production
damage mitigation account-statutory appro-
priation.
Section 82-11-162. Release of producing oil
or gas well from drilling bond-fee.
Section 82-11-163. Landowner's bond on
noncommercial well.
Section 82-11-164. Lien created.
Section 82-11-165 through 82-11-170 re-
served.
Section 82-11-171, Terminated.
Section 82-11-201, Establishment of well
spacing units.
Section 82-11-202. Pooling of interest with-
in spacing unit.
Section 82-11-203, Pooling agreements not
in violation of antitrust laws.
Section 82-11-204. Hearing on operation of
pool as unit.
Section 82-11-205. Board order for unit op-
eration-criteria.
Section 82-11-206. Terms and conditions of
plan for unit operations.
Section 82-11-207. Approval of plan for unit
operations by persons paying costs.
Section 82-11-208. Board orders-amend-
ment.
Section 82-11-209. Units established by pre-
vious order.
Section 82-11-210. Unit operations-less than
whole of pool.
Section 82-11-211. Operations considered as
done by all owners in unit.
Section 82-11-212, Property rights and op-
erator's lien,
Section 82-11-213. Contract not terminated
by board order.
Section 82-11-214. Title to oil and gas
rights not affected by board order.
Section 82-11-215. Unit operation not re-
straint of trade.
Section 82-11-216. No creation of relation-
ship between parties in unit.
Section 82-11-301. Authorization to join
interstate compact for conservation of oil
and gas,
Section 82-11-302. Interstate oil and gas
compact.
Section 82-11-303. Extension of expiration
date.
Section 82-11-304. Governor as member of
Interstate Oil Compact Commission,
Section 82-11-305. Limitation on power of
representative.
Section 82-11-306. Expenses of representa-
tive,
(b) The regulatory provisions include: Ad-
ministrative Rules of Montana Board of Oil
and Gas Conservation, Chapter 22, revised
March 1996:
Rule 36.22.101. Organizational Rule.
Rule 36.22.201. Procedural Rules.
Rule 36.22.202. Environmental Policy Act
Procedural Rules.
Rule 36.22.301. Effective Scope of Rules.
Rule 36.22.302. Definitions.
766
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Environmental Protection Agency
Pt. 147, Subpt. BB, App. A
Rule 36.22.303. Classification of Wildcat or
Exploratory Wells.
Rule 36 22.304, Inspection of Record, Prop-
erties, and Wells.
Rule 36.22.305. Naming of Pools.
Rule 36.22,306. Organization of Reports.
Rule 36.22,307, Adoption of Forms.
Rule 36,22,308. Seal of Board.
Rule 36.22.309. Referral of Administrative
Decisions.
Rule 36.22,401. Office and Duties of Petro-
leum Engineer.
Rule 36.22.402. Office and Duties of Admin-
istrator,
Rule 36.22,403. Office and Duties of Geolo-
gist.
Rule 36.22.501. Shot Location Limitations.
Rule 36,22.502, Plugging and Abandonment.
Rule 36.22.503, Notification.
Rule 36,22.504, Identification.
Rule 36.22.601. Notice of Intention and Per-
mit to Drill.
Rule 36.22.602. Notice of Intention to Drill
and Application for Permit to Drill.
Rule 36.22.603. Permit Fees.
Rule 36.22.604. Permit Issuance - Expiration
- Extension.
Rule 36.22,605. Transfer of Permits.
Rule 36.22.606. Notice and Eligibility State-
ment for Drilling or Recompletion in Unit
Operations.
Rule 36.22.607. Drilling Permits Pending
Special Field Rules.
Rule 36.22.701. Spacing Units - General.
Rule 36.22.702. Spacing of Wells,
Rule 36.22.703. Horizontal Wells.
Rule 36.22.1001. Rotary Drilling- Procedure.
Rule 36.22.1002. Cable Drilling Procedure.
Rule 36.22.1003. Vertical Drilling Required
Deviation.
Rule 36.22.1004. Dual Completion of Wells.
Rale 36.22.1005. Drilling Waste Disposal and
Surface Restoration.
Rules 36.22.1006 through 36.22.1010, Re-
served.
Rule 36.22.1011. Well Completion and Re-
completion Reports.
Rule 36,22.1012. Samples of Cores and
Cuttings.
Rule 36.22.1013. Piling of Completion Re-
ports, Well Logs, Analyses, Reports, and Sur-
veys.
Rule 86.22.1014. Blowout Prevention and
Well Control Equipment.
Rule 36,22.1101. Fire Hazard Prevention.
Rule 36.22.1102. Fire Walls Required.
Rule 36.22.1103. Notification and Report of
Emergencies and Undesirable Incidents.
Rule 36,22.1104. Control and Cleanup.
Rule 36,22.1105, Solid Waste.
Rule 36,22,1201. Surface Equipment.
Rule 36.22.1202. Identification.
Rule 36.22.1203. Chokes Required.
Rule 36.22.1204. Separators Required.
Rule 36.22.1205. Vacuum Pumps Prohibited.
Rule 36.22.1206. Tubing Required.
Rule 36.22.1207. Earthen Pits and Open Ves-
sels.
Rule 36.22.1208. Producing from Different
Pools Through the Same Casing.
Rules 36.22.1209 through 36.22,1212. Re-
served.
Rule 36.22.1213. Reservoir or Pool Surveys.
Rule 36.22.1214. Subsurface Pressure Tests,
Rule 36.22.1215. Stabilized Production Test.
Rule 36.22.1216. Gas Oil Ratio Tests.
Rule 36.22.1217. Water Production Report.
Rule 36.22.1218. Gas to be Metered.
Rule 36.22.1219. Gas Waste Prohibited.
Rule 36,22.1220. Associated Gas Flaring
Limitation—Application to exceed—Board
Review and Action.
Rule 36.22.1221. Burning of Waste Gas Re-
quired,
Rule 36,22.1222. Hydrogen Sulfide Gas.
Rule 36.22.1223. Fencing, Screening, and
Netting of Pits.
Rules 36.22.1224 and 36.22.1425. Pveserved.
Rule 36.22.1226. Disposal of Water.
Rule 36.22.1227. Earthen Pits and Ponds.
Rule 36.22.1228. Disposal by Injection.
Rule 36,22.1229. Water Injection and Gas
Repressuring.
Rule 36.22,1230, Application Contents and
Requirements.
Rule 36.22.1231. Notice of Application Ob-
jections.
Rule 36.22.1232. Board Authorization.
Rule 36.22.1233, Notice of Commencement
or Discontinuance—Plugging of Abandoned
Wells.
Rule 36.22.1234. Record Required.
Rules 36.22.1235 through 36.22.1239. Re-
served.
Rule 36.22.1240. Report of Well Status
Change.
Rule 36.22.1241. Service Company Reports.
Rule 36.22.1242. Reports by Producers.
Rule 36.22.1243. Reports from Transporters.
Refiners, and Gasoline or Extraction Plants.
Rule 36.22.1244. Producer's Certificate of
Compliance.
Rule 36.22.1245. Illegal Production.
Rule 36.22.1301. Notice and Approval of In-
tention to Abandon Report.
Rule 36.22.1302. Notice of Abandonment.
Rule 36,22.1303. Well Plugging- Require-
ment.
Rule 36.22.1304. Plugging Methods and Pro-
cedure.
Rule 36.22,1305. Exception for Fresh Water
Wells.
Rule 36.22.1306. Approval for Pulling Casing
and Reentering Wells.
Rule 36.22.1307. Restoration of Surface.
Rule 36.22.1308. Plugging and Restoration
Bond,
Rule 36.22.1309. Subsequent Report of Aban-
donment.
Rule 36.22.1401. Definitions.
Rule 36.22,1402. Underground Injection.
Rule 36.22.1403. Application Contents and
Requirements Rules.
767
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§147.1400
40 CFR Ch. I (7-1-04 Edition)
Rule 36.22.1404 and 36.22.1405. Reserved.
Rule 36.22.1406. Corrective Action.
Rule 36.22.1407. Signing the Application.
Rule 36.22.1408. Financial Responsibility.
Rule 36.22.1409. Hearings.
Rule 36.22.1410. Notice of Application.
Rule 36.22.1411. Board Authorization,
Rules 36.22.1412 and 36.22.1413. Reserved.
Rule 36.22.1414. Notice of Commencement
or Discontinuance—Plugging of Abandoned
Wells.
Rule 36.22.1415. Records Required.
Rule 36.22.1416. Mechanical Integrity.
Rule 36.22.1417. Notification of Tests—Re-
porting Results.
Rule 36.22.1418. Exempt Aquifers.
Rule 36.22.1419. Tublngless Completions.
Rules 36.22.1420 and 36.22.1421. Reserved.
Rule 36.22.1422. Permit Conditions.
Rule 36.22.1423. Injection Fee—Well Classi-
fication.
Rule 36.22.1601. Who May Apply for Deter-
mination.
Rule 36.22.1602. Application Requirements
and Contents.
Rule 36.22.1603. Documents and Technical
Data Supporting Application.
Rule 36.22.1604. Docket Number.
Rule 36.22.1605. List of Applications—Pub-
lic Access.
Rule 36.22.1606. Objections to Applications.
Rule 36.22.1607. Deadlines for Action Deter-
minations.
Rule 36.22.1608. Deficient Applications.
Rule 36.22.1609. Board Action on Applica-
tions.
Rule 36.22.1610. Special Findings and Deter-
minations New Onshore Production Wells
Under Section 103.
Rule 36,22.1611. Special Finding's and Deter-
minations Stripper Well Production.
[61 PR 58934, Nov. 19, 1996]
Subpart CC—Nebraska
§ 147.1400 State-administered pro-
gram—Class II wells.
The UIC program for Class U wells in
the State of Nebraska, except those on
Indian lands, is the program adminis-
tered "by the Nebraska Oil and Gas Con-
servation Commission, approved by
EPA pursuant to section 1425 of the
SOW A.
(a) Incorporation by reference. The
requirements set forth in the State
statutes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Nebraska. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Rules and Regulations of the Ne-
braska Oil and Gas Conservation Com-
mission, Rules 1 through 6 (as pub-
lished by the Commission, May 1981);
(2) Revised Statutes of Nebraska, sec-
tions 57-903 and 57-906 (Reissue 1988).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for select
sections identified in paragraph (a) of
this section, are also part of the ap-
proved state-administered program:
(1) Chapter 57, Oil and Gas Conserva-
tion, Revised Statutes of Nebraska sec-
tions 57-901 through 57-922 (Reissue
1985).
(c) The Memorandum of Agreement
between EPA Region VII and the Ne-
braska Oil and Gas Conservation Com-
mission, signed by the EPA Regional
Administrator on July 12, 1982.
(d) Statement of legal authority. (1)
"Nebraska Underground Injection Con-
trol Program, Attorney General's
Statement for Class II Wells," signed
by Assistant Attorney General for At-
torney General of Nebraska, as sub-
mitted with "State of Nebraska Re-
quest for Administration of UIC Pro-
gram," January 23, 1982;
(2) "Re: Nebraska Underground Injec-
tion Control Program, Addendum to
Attorney General's Statement for
Class II Wells," signed by Assistant At-
torney General for Attorney General of
Nebraska," undated.
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 52
FR 17681, May 11, 1987; 56 FR 9417, Mar. 6.
1991]
§147.1401 State administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I, III, IV,
and V wells in the State of Nebraska,
except those on Indian lands, is the
program administered by the Nebraska
Department of Environmental Control,
approved by EPA pursuant to section
1422 of the SDWA.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
768
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Environmental Protection Agency
§147.1450
the State of Nebraska. This incorpora-
tion by reference was approved toy the
Director of the Federal Register effec-
tive June 26, 1984.
(1) Nebraska Environmental Protec-
tion Act, Revised Statutes of Nebraska
sections 81-1502, 81-1506, 81-1519, and 81-
1520 (Reissue 1987);
(2) Nebraska Department of Environ-
mental Control, Title 122—Rules and
Regulations for Underground Injection
and Mineral Production Wells, Effec-
tive Date: February 16, 1982, Amended
Dates: November 12. 1983, March 22,
1984; as amended by amendment ap-
proved by the Governor on January 2,
1989.
(b) Other laws. The following statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Nebraska Environmental Protec-
tion Act, Nebraska Revised Statutes
sections 81-1502, 81-1506, 81-1519. and 81-
1520 (Reissue 1987 and Cumm. Supp.
1988);
(c)(l) The Memorandum of Agree-
ment between EPA Region VII and the
Nebraska Department of Environ-
mental Control, signed by the EPA Re-
gional Administrator on July 12, 1982.
(2) Addendum to Underground Injec-
tion Control Memorandum of Agree-
ment signed by the EPA Regional Ad-
ministrator on July 12, 1982.
(3) Amendments to the Memorandum
of Agreement signed by the EPA Re-
gional Administrator on November 22,
1983.
(d) Statement of legal authority. (1)
"Nebraska Underground Injection Con-
trol Program, Attorney General's
Statement for Class I. Ill, IV, and V
Wells", signed by Assistant Attorney
General for Attorney General of Ne-
braska, as submitted with "State of Ne-
braska Request for Administration of
UIC Program, January 28, 1982;
(2) Letter from Attorney General (of
Nebraska), by Assistant Attorney Gen-
eral, to Director. (Nebraska) Depart-
ment of Environmental Control, Au-
gust 7. 1981;
(3) Letter from Attorney General (of
Nebraska), by Assistant Attorney Gen-
eral, to Director, (Nebraska) Depart-
ment of Environmental Control. April
20. 1982;
(4) Letter from Attorney General (of
Nebraska), by Assistant Attorney Gen-
eral, to Legal Counsel, (Nebraska) De-
partment of Environmental Control,
October 18, 1983.
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
(42 U.S.C. 1422)
[49 PR 24134. June 12. 1984, as amended at 52
PR 17681, May 11, 1987: 56 PR 9417. Mar- 6,
1991]
§147.1402 Aquifer exemptions. [Re-
served]
§ 147.1403 EPA-administered pro-
gram—Indian lands.
(a) Contents, The UIC program for all
classes of wells on Indian lands in the
State of Nebraska is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian Lands in
Nebraska is June 25, 1984.
[52 PR 17681, May 11, 1987, as amended at 56
FR 9417, Mar. 6, 1991]
Subpart DD—Nevada
§ 147.1450 State-administered pro-
gram.
The UIC program for all classes of
underground injection wells in the
State of Nevada, other than those on
Indian lands, is the program adminis-
tered by the Nevada Division of Envi-
ronmental Protection approved by EPA
pursuant to section 1422 of the SDWA.
Notice of this approval was published
in the FEDERAL REGISTER on February
18, 1988; the effective date of this pro-
gram is October 5, 1988. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application.
(a) Incorporation by reference. The
requirements set forth in the State
statutes and regulations cited in this
paragraph are hereby incorporated by
769
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§147.1451
40 CFR Ch. 1 (7-1-04 Edition)
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Nevada, This Incorpora-
tion by reference was approved by the
Director of the Federal Register in ac-
cordance with 5 U.S.C. 552(a) and 1 CFR
part 51. Copies may be obtained at the
Nevada Department of Conservation
and Natural Resources, Division of En-
vironmental Protection, 201 South Pall
Street, Carson City, Nevada 89710.
Copies may be inspected at the Envi-
ronmental Protection Agency, Region
IX, 215 Fremont Street, San Francisco,
California 99105, or at the National Ar-
chives and Records Administration
(NARA). For information on the avail-
ability of this material at NARA, call
202-741-6030, or go to: http://
www.archives.gov/federal register/
code of^federal regulations/
ibr locations.html.
(1) Nevada Revised Statutes [NRS],
Volume 25, Chapters 445.131 through
445,354, Inclusive. 1987.
(2) Nevada Revised Statutes [NRS],
Volume 29, Chapters 534A.010 through
534A.090, Inclusive. 1987.
(3) Nevada Revised Statutes [NRS],
Volume 28, Chapters 522.010 through
522.190, Inclusive. 1987.
(4) Nevada Administrative Code
[NAC], Underground Injection Control
Regulations, Sections 1 through 96.1,
Inclusive. July 22, 1987, revised Sep-
tember 3, 1987 (amending NAC Chapter
445).
(5) Nevada Administrative Code
[NAC], Regulations and Rules of Prac-
tice and Procedure adopted Pursuant
to NRS 534A, Sections 1 through 69, In-
clusive. November 12, 1985 (amending
NAC Chapter 534A).
(6) Nevada Administrative Code
[NAC], Regulations and Rules of Prac-
tice and Procedure adopted Pursuant
to NRS 522.010 through 522.625, Inclu-
sive. July 22, 1987 (amending NAC
Chapter 522).
(b) The Memorandum of Agreement
between EPA Region 9 and the Nevada
Department of Conservation and Nat-
ural Resources signed by the EPA Re-
gional Administrator on April 6, 1988.
(c) Statement of Legal Authority,
Statement and Amendment to the
Statement from the Attorney General
of the State of Nevada, signed on July
22, 1987 and November 6, 1987 respec-
tively, by the Deputy Attorney Gen-
eral.
(d) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[53 PR 39089, Oct. 5, 1988]
§147.1451 EPA administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Nevada is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this snbpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective dates. The effective date
of the UIC program for Indian lands in
Nevada is June 25, 1984.
[53 PR 43088, Oct. 25, 1988, as amended at 56
FR 9417, Mar. 6, 1991]
8147.1452 Aquifer exemptions. [Re-
served]
1147.1453 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of § 144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the formula:
Pm=(0.733-O.433 Sg)d
where:
Pm=injection pressure at the wellhead in
pounds per square inch
Sg=speciflc gravity of injected fluid
(unitless)
d=injection depth in feet.
1147.1454 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
770
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Environmental Protection Agency
§147.1500
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(il) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of § 144.28(f)(3)(ii) (A) and
(B), The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for public hearing, according to
the provisions of part 124, subpart A of
this chapter.
(21 Prior to such time as the Regional
Administrator establishes field rules
for maximum injection pressure based
on data provided pursuant to para-
graph (a)(2)(ii) of this section the
owner or operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within one year following the effective
date of this program.
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating' all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section, as needed to protect
USDWs.
Subpart EE—New Hampshire
§ 147.1500 State-administered pro-
gram.
The UIO program for all classes of
wells in the State of New Hampshire,
except those wells on Indian lands, is
the program administered by the New
Hampshire Department of Environ-
mental Services, approved by the EPA
pursuant to section 1422 of the SDWA.
Notice of this approval was published
in the FR on September 21. 1982 (47 FR
41561); the effective date of this pro-
gram is October 21, 1982. This program
consists of the following elements;
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of New Hampshire. This in-
corporation by reference was approved
by the Director of the Federal Register
on June 25, 1984.
(1) New Hampshire Revised Statutes
Annotated section 149:8 IH(a) (1978);
(2) New Hampshire Code of Adminis-
trative Rules, Part We 410 (Protection
771
-------
§147.1501
40 CFR Ch. I (7-1-04 Edition)
of Groundwaters of the State, sections
Ws 410.1 through Ws 410.16) (Issue Ws 3-
82).
(b)(l) The Memorandum of Agree-
ment between EPA Region I and the
New Hampshire Water Supply and Pol-
lution Control Commission, signed by
the EPA Regional Administrator on
August 23, 1982;
(2) Amendment No. 1 to the Memo-
randum of Agreement, signed by the
EPA Regional Administrator on July
16,1982.
(c) Statement of legal authority. (1)
Letter from Attorney General of New
Hampshire to Regional Administrator,
EPA Region I, "Re: Attorney General's
Statement—Underground Injection
Control Program," March 23, 1982;
(2) Letter from Attorney General of
New Hampshire to Regional Adminis-
trator, EPA Region I, "Re: Attorney
General's Statement—Underground In-
jection Control Program," July 1, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 53
PR 43088, Oct. 25, 1988; 56 PR 9417, Mar. 8,
1991]
§ 147.1501 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of New Hampshire is adminis-
tered by EPA. This program consists of
the UIC program requirements of 40
CPR parts 124, 144, 146, 148, and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements,
(b) Effective date. The effective date
of the UIC program for Indian lands in
New Hampshire is November 25, 1988.
[53 FR 43088, Oct. 25, 1988, as amended at 56
PR 9417, Mar. 6, 1991]
Subpart FF—New Jersey
§ 147.1550 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of New Jersey, ex-
cept those on Indian lands, is the pro-
gram administered by the New Jersey
Department of Environmental Protec-
tion, approved by EPA pursuant to sec-
tion 1422 of the SDWA. Notice of this
approval was published in the Federal
Register on July 15, 1983 (48 PR 32343);
the effective date of this program is
August 15, 1983. This program consists
of the following elements, as submitted
to EPA in the State's program applica-
tion.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of New Jersey. This incorpo-
ration by reference was approved by
the Director of the Federal Register on
June 25, 1984.
(1) Water Pollution Control Act, New
Jersey Statutes Annotated sections
58:10A~1 through 58:10A~-20 (West 1982
and Supp. 1990);
(2) New Jersey Administrative Code,
sections 7:14A-1.1 through 1.9 (sub-
chapter 1), 7:14A-2.1 through 2.15 (sub-
chapter 2), 7:14A-5.1 through 5.17, (sub-
chapter 5) (amended March 1988).
(b)(l) The Memorandum Agreement
between EPA Region II and the New
Jersey Department of Environmental
Protection, signed by the EPA Re-
gional Administrator on September 9.
1982;
(2) Letter from Commissioner, New
Jersey Department of Environmental
Protection, to Regional Administrator,
EPA Region II, March 21, 1983.
(c) Statement of legal authority. (1)
Letter from Attorney General of New
Jersey (by Deputy Attorney General)
to Commissioner, Department of Envi-
ronmental Protection, "Re: New Jersey
Pollutant Discharge Elimination Sys-
tem—Underground Injection Control,"
February 9,1982;
(2) Letter from Attorney General of
New Jersey (by Deputy Attorney Gen-
eral) to Commissioner. Department of
Environmental Protection, "Re: New
Jersey Pollutant Discharge Elimi-
nation System—Underground Injection
Control," April 15, 1983 (six pages);
(3) Letter from Attorney General of
New Jersey (by Assistant Attorney
General) to Commissioner, Department
of Environmental Protection, "Re: New
772
-------
Environmental Protection Agency
§147.1601
Jersey Pollutant Discharge Elimi-
nation System—Underground Injection
Control," April 15, 1983 (two pages).
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11. 1984, as amended at 53
FR 43089, Oct. 25, 1988; 56 PR 9417, Mar. 6,
1991]
§ 147.1551 EPA-administered pro-
gram—Indian lands.
(a) Contents, The UIC program for all
classes of wells on Indian lands in the
State of New Jersey is administered "by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
New Jersey is November 25, 1988.
[53 FR 43089, Oct. 25, 1988, as amended at 56
FR 9417, Mar. 6, 1991]
Subpart QG—New Mexico
§ 147.1600 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of New Mexico, except for
those on Indian lands, is the program
administered by the New Mexico En-
ergy and Minerals Department, Oil
Conservation Division, approved by
EPA pursuant to section 1425 of the
SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
February 5, 1982 (47 FR 5412); the effec-
tive date of this program is March 7,
1982. This program consists of the fol-
lowing elements as submitted to EPA
in the State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of New Mexico. This incorpo-
ration by reference was approved by
the Director of the Federal Register on
June 25, 1984.
(1) Oil and Gas Act, New Mexico Stat-
utes Annotated sections 70-2-1 through
-36 (1978):
(2) State of New Mexico Energy and
Mineral Department, Oil Conservation Di-
vision—Rules and Regulations (dated 10-
1-78), sections B-3, 1-701 through 1-708,
M-1100 through M-1121.
(b)(l) The Memorandum of Agree-
ment between EPA Region VI and the
New Mexico Energy and Minerals De-
partment, Oil Conservation Division,
signed by the EPA Regional Adminis-
trator on December 10, 1981;
(2) Addendum No. 1 to the Memo-
randum of Agreement, signed by the
EPA Regional Administrator on June
28, 1982;
(3) Addendum No. 2 to the Memo-
randum of Agreement, signed by the
EPA Regional Administrator on No-
vember 18, 1982;
(4) Letter from Director, Oil Con-
servation Division, New Mexico Energy
and Minerals Department, and Assist-
ant Attorney General of New Mexico,
to Regional Administrator, EPA Re-
gion VI, November 6, 1981.
(c) Statement of legal authority.
"Statement of Legal Authority of the
State of New Mexico by and through
its Oil Conservation Division of the En-
ergy and Mines Department to conduct
an Underground Injection Control Pro-
gram," signed by Assistant Attorney
General and General Counsel to the Oil
Conservation Division.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43089, Oct. 25, 1988]
1147.1601 State-administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I, III, IV
and V injection wells in the State of
New Mexico, except for those on Indian
lands, is the program administered by
the New Mexico Water Quality Control
Commission, the Environmental Im-
provement Division, and the Oil Con-
servation Division, approved by EPA
pursuant to section 1422 of the SDWA.
Notice of this approval was published
in the FEDERAL REGISTER on July 11.
1983 (48 FR 31840): the effective date of
this program is August 10, 1983. This
773
-------
§147.1603
40 CFR Ch. I (7-1-04 Edition)
program consists of the following ele-
ments, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of New Mexico. This incorpo-
ration by reference was approved by
the Director of the Federal Register on
June 25,1984.
(1) New Mexico Water Quality Con-
trol Commission Regulations (WQCC
82-1) sections 1-100 through 5-300 (Sep-
tember 20, 1982).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, are also part of
the approved State-administered UIC
program:
(1) Water Quality Act, New Mexico
Statutes Annotated sections 74-6-1
through 74-6-13 (1978 and Supp. 1982);
(2) Geothermal Resources Conserva-
tion Act, New Mexico Statutes Anno-
tated sections 71-5-1 through 71-5-24
(1978 and Supp. 1982);
(3) Surface Mining Act, New Mexico
Statutes Annotated sections 69-25A-1
through 69-25A-35 (1978 and Supp. 1980).
(c)(l) The Memorandum of Agree-
ment between EPA Region VI and the
New Mexico Water Quality Control
Commission, the Environmental Im-
provement Division, and the Oil Con-
servation Division, signed by the EPA
Regional Administrator on April 13,
1983;
(2) Letter from the Director, Envi-
ronmental Improvement Division and
the Director, Oil Conservation Divi-
sion, to Regional Administrator, EPA
Region IV, "Re: New Mexico Under-
ground Injection Control Program—
Clarification," February 10,1983.
(d) Statement of legal authority. "At-
torney General's Statement," signed by
the Assistant Attorney General for the
Environmental Improvement Division,
the Assistant Attorney General for Oil
Conservation Division, and the Deputy
Attorney General, Civil Division, Coun-
sel for the Mining and Minerals Divi-
sion, undated, submitted December 8,
1982,
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
PR 43089, Oct. 25, 1988]
§ 147,1603 EPA-administered pro-
gram—Indian lands,
(a) Contents. The UIC program for all
classes of wells on Indian lands in New
Mexico is administered by EPA. The
program consists of the requirements
set forth at Subpart HHH of this part.
Injection well owners and operators
and EPA shall comply with these re-
quirements.
(b) Effective date. The effective date
for the UIC program on Indian lands in
New Mexico is November 25, 1988.
[53 PR 43089, Oct. 25, 1988]
Subpart HH—New York
§ 147.1650 State-administered
gram, [Reserved]
pro-
§ 147,1651 EPA-administered program.
(a) Contents. The UIC program for the
State of New York, including all Indian
lands, is administered by EPA. The
program consists of the UIC program
requirements of 40 CPR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
of the UIC program for New York for
all injection activities except those on
lands of the Seneca Indian Tribe is
June 25, 1984. The effective date for the
UIC program for the lands of the Sen-
eca Indian Tribe is November 25, 1988.
[53 PR 43089, Oct. 25, 1988; 54 PR 10618, Mar.
14, 1989, as amended at 56 PR 9417, Mar. 6.
1991]
§ 147.1652 Aquifer exemptions.
(a) This section identifies any aquifer
or their portions exempted in accord-
ance with §§144.7(b) and 146.4 of this
chapter at the time of program promul-
gation. EPA may in the future exempt
other aquifers or portions, according to
applicable procedures, without codi-
fying such exemptions in this section.
An updated list of exemptions will be
maintained in the Regional office.
774
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Environmental Protection Agency
§147.1654
(b) The following portions of aquifers
are exempted in accordance with the
provisions of §§ 144.7(b) and 146,4 of this
chapter for Class II injection activities
only:
(1) The Bradford First, Second, and
Third Sand Members and the Kane
Sand Member in the Bradford Field in
Cattaraugus County.
(2) The Chipmunk Oil field in
Cattaraugus County.
§147.1653 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144.28(f)(3)
(i) or (ii) as applicable; or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0,733- 0.433 Sg)d
where:
Pm=mjection pressure at the well head in
pounds per square inch
Sg=specific gravity of inject fluid (nnitless)
d=injeetion depth in feet.
§147.1654 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure, or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(lMi) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of § 144.28(f)(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter,
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(ii) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place, A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within one year of the effective date of
this program.
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(iii) For wells as described in
§146.8(b)(3)(ii), installing a smaller di-
ameter pipe inside the existing injec-
tion tubing and setting it on an appro-
priate packer; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 50 feet
above the injection zone; and
(3) Use cement:
775
-------
§147.1655
40 CFR Ch. I (7-1-04 Edition)
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iil) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may-
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section as needed to protect
USDWs.
§ 147,1655 Requirements for wells au-
thorized by permit,
(a) The owner or operator of a Class
I well authorized by permit shall in-
stall or shall ensure that the well has:
(1) Surface casing present;
(i) Extending from the surface to a
depth at least 50 feet below the base of
the lowermost USDW; and
(ii) Cemented back to the surface by
recirculating the cement; and
(2) Long string casing and tubing;
(i) Extending to the injection zone;
and
(ii) Cemented back to 50 feet above
the base of the next largest casing
string.
(b) The owner or operator of a new
Class II well authorized by permit
shall:
(1) Install surface casing from the
surface to at least 50 feet below the
base of the lowermost USDW.
(2) Cement the casing by recircu-
lating to the surface or by using no less
than 120% of the calculated annular
volume.
(3) For new enhanced recovery wells,
install tubing or long string casing ex-
tending to the injection zone.
(4) For new salt water disposal wells,
install long string casing and tubing
extending to the injection zone.
(5) Isolate any injection zone by plac-
ing sufficient cement to fill the cal-
culated volume to a point 50 feet above
the injection zone.
(c) The Regional Administrator may
specify casing and cementing require-
ments other than those listed in para-
graphs (a) and (b) of this section on a
case by case basis as conditions of the
permit.
Subpart II—North Carolina
§ 147,1700 State-administered pro-
gram,
The UIC program for all classes of
wells in the State of North Carolina,
except those wells on Indian lands, is
the program administered by the North
Carolina Department of Environment,
Health and Natural Resources approved
by EPA pursuant to section 1422 of the
SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
April 19, 1984 (49 FR 15553); the effective
date of this program is April 19, 1984.
This program consists of the following
elements, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of North Carolina. This in-
corporation by reference was approved
by the Director of the OPR in accord-
ance with 5 U.S.C. 552(a) and 1 CFR
part 51. Copies may be obtained at the
North Carolina Department of Environ-
ment, Health and Natural Resources,
P.O. Box 27687, Raleigh, North Carolina
27611. Copies may be inspected at the
Environmental Protection Agency, Re-
gion IV, 345 Courtland Street, NE., At-
lanta, Georgia 30365, or at the National
Archives and Records Administration
(NARA). For information on the avail-
ability of this material at NARA, call
202-741-6030, or go to: http://
www.archives.gov/federal register/
code of federal_ regulations/
ibr_Jocations.html.
(1) Administrative Procedure Act,
N.C. GEN. STAT. 150B-1 through 150B-
64 (1987 and Cumm. Supp. 1989);
(2) North Carolina Well Construction
Act, N.C. GEN. STAT. §§87-83 through
87-99 (1989 and Cumm. Supp. 1989);
(3) Water and Air Resources, N.C.
GEN. STAT. §§143-211 through 143-
215.10 (1987 and Cumm. Supp. 1989);
(4) Solid Waste Management. N.C.
GEN. STAT. §§130A-290 through 130A-
309.03(1989);
(5) North Carolina Drinking Water
Act, N.C, GEN. STAT. §§130A-311
through 130A-332 (1989);
776
-------
Environmental Protection Agency
§147.1750
(6) Sanitary Sewage Systems, N.C,
GEN. STAT. |§13QA-333 through 130A-
335 (1989).
(b) Other laws. The following rules
and regulations, although not incor-
porated by reference, are also part of
the approved State-administered
program:
(!) N.C. ADMIN. CODE, Title 15, r.
02L.01QQ et seq. Groundwater Classifica-
tion and Standards: General Consider-
ations (September 22, 1988);
(2) N.C. ADMIN. CODE. Title 15, r.
02L.0100 et seq. Criteria and Standards
Applicable to Injection Wells (Sep-
tember 22, 1988).
(c) Memorandum of Agreement. The
Memorandum of Agreement between
the State of North Carolina and EPA
Region IV, signed March 1, 1984.
(d) Statement of legal authority. (1) Un-
derground Injection Control Program,
Attorney General's Statement (June
15, 1982);
(2) Amendment to Underground In-
jection Control Program, Attorney
General's Statement (February 9, 1984).
(e) Program Description. The Program
Description and other materials sub-
mitted as part of the application or as
supplements thereto.
[56 FR 9417, Mar. 6. 1991]
§§ 147,1701-147.1702 [Reserved]
§ 147.1703 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of North Carolina is adminis-
tered by EPA. This program consists of
the UIC program requirements of 40
CPR parts 124, 144, 146, 148, and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements,
(b) Effective date. The effective date
of the UIC program for Indian lands in
North Carolina is November 25, 1988.
[53 FR 43089, Oct. 25, 1988, as amended at 56
FB 9418, Mar. 6, 1991]
§§147.1704-147,1749 [Reserved]
Subpart JJ—North Dakota
§ 147.1750 State-administered pro-
gram—Class II wells,
The UIC program for Class II wells in
the State of North Dakota, except
those on Indian lands, is the program
administered by the North Dakota In-
dustrial Commission, approved by EPA
pursuant to section 1425 of the SDWA.
Notice of this approval was published
in the FEDERAL REGISTER on August 23.
1983 (48 FR 38237); the effective date of
this program is September 24. 1983.
This program consists of the following
elements, as submitted to EPA in the
State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by
reference and made a part of the ap-
plicable UIC program under the SDWA
for the State of North Dakota. This in-
corporation by reference was approved
by the Director of the Federal Register
on June 25, 1984.
(1) North Dakota Century Code,
Chapter 38-08 (Control of Gas and Oil
Resources, 1987 and Supp. 1989);
(2) North Dakota Administrative
Code, Chapter 43-02-05 (Underground
Injection Control, as published in Stat-
utes and Rules for the Conservation of Oil
and Gas, North Dakota Industrial Com-
mission, revised effective November 1,
1987);
(3) North Dakota Administrative
Code, Chapter 43-02-03 (General Rules,
as published in Statutes and Rules for
the Conservation of Oil and Gas, North
Dakota Industrial Commission, revised
effective November 1, 1987).
(b) The Memorandum of Agreement
between EPA Region VIII and the
North Dakota Industrial Commission,
Oil and Gas Division, signed by the
EPA Regional Administrator on June
16, 1983, as amended September 7. 1989.
(e) Statement of legal authority. "Un-
derground Injection Control Program
Attorney General's Statement," as sub-
mitted with the North Dakota Under-
ground Injection Control Program Pri-
macy Application for Class II Injection
Wells, transmitted by the Governor on
July 15, 1982 (16 pages).
777
-------
§147.1751
40 CFR Ch. I (7-1-04 Edition)
(d) The Program Description and
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 53
FB 43089, Oct. 26, 1988; 56 FB 9418, Mar. 6.
1991]
§ 147.1751 State-administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I, III, IV,
and V wells in the State of North Da-
kota, except those on Indian lands, is
the program administered by the North
Dakota Department of Health, ap-
proved by EPA pursuant to section 1422
of the SDWA. Notice of this approval
was published In the FEDERAL REO-
TSTEE on September 21, 1984; the effec-
tive date of this program is October 5,
1984. This program consists of the fol-
lowing- elements, as submitted to EPA
in the State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of North Dakota. This incor-
poration by reference was approved by
the Director of the Federal Register ef-
fective October 5, 1984.
(1) North Dakota Century Code Sec-
tions 38-12-01, 38-12-03 (1980);
(2) North Dakota Century Code, Sec-
tions 61-28-02 and 61-28-06 (1989);
(3) North Dakota Administrative
Code Sections 33-25-01-01 through 33-
25-01-18 (North Dakota State Health
Department Underground Control Pro-
gram) (1983);
(4) North Dakota Administrative
Code. Chapter 43-02-02 (Subsurface
Mineral Exploration and Development)
(August 1986), and Chapter 43-02-02.1
(Underground Injection Control Pro-
gram) (March 1. 1984);
(5) North Dakota Administrative
Code Sections 43-02-02-1-01 through 43-
02-02-4-18 (North Dakota Geological
Survey—Undergound Injection Control
Program) (1984);
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, also are part of
the approved State-administered
program;
(1) North Dakota Environmental Law
Enforcement Act of 1975, North Dakota
Century Code Sections 32-40-01 to 32-
40-11 (1976);
(2) North Dakota Century Code, Ch,
38-12 (Regulation, Development, and
Production of Subsurface Minerals)
(1979);
(3) North Dakota Century Code Chap-
ter 61-28 (Control, Prevention and
Abatement of Pollution of Surface Wa-
ters) (1989);
(4) North Dakota Administrative
Code Article 33-22 (Practice and Proce-
dure) (1983).
(c) The Memorandum of Agreement
between EPA Region VIII and the
North Dakota Department of Health,
signed by the EPA Regional Adminis-
trator on May 18, 1984.
(d) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FB 37066, Sept. 21, 1984, as amended at 56
FB 9418, Mar. 6, 1991]
§ 147.1752 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of North Dakota is administered
by EPA. This program consists of the
UIC program requirements of 40 CPR
parts 124, 144, 146. 148, and any addi-
tional requirements set forth in the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements,
(b) Effective date. The effective date
of the UIC program for Indian lands in
North Dakota is November 25, 1988.
[53 PR 43089, Oct. 25, 1988. as amended at 56
PR 9418. Mar. 6, 1991]
Subpart KK—Ohio
§147,1800 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Ohio, except for those on
Indian lands, is the program adminis-
tered by the Ohio Department of Nat-
ural Resources, approved by EPA pur-
suant to section 1425 of the SDWA. No-
tice of this approval was published in
the FEDERAL REGISTER on August 23,
1983 (48 FR 38238); the effective date of
778
-------
Environmental Protection Agency
§147.1801
this program is September 22, 1983,
This program consists of the following:
elements, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Ohio, This incorporation
by reference was approved by the Di-
rector of the Federal Register on June
25,1984.
(1) Ohio Revised Code Annotated, sec-
tions 1509.01 through 1509.22 (Page 1978
and Supp. 1982);
(2) Rules of the Division of Oil and
Gas, Ohio Administrative Code sections
1501:91-01, through 1501: 9-11-13 (1983).
(b) The Memorandum of Agreement
between EPA Region V and the Ohio
Department of Natural Resources.
(c) Statement of legal authority. "Un-
derground Injection Control Program—
Attorney General's Statement," signed
by the Assistant Attorney General,
Chief, Environmental Law Section, for
the Attorney General of Ohio, Sep-
tember 30, 1982.
(d) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FE 20197, May 11, 1984, as amended at 53
FR 43089, Oct. 25, 1988]
§ 147.1801 State-administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I, III, IV,
and V wells in the State of Ohio, other
than those on Indian lands, is the pro-
gram administered by the Ohio Depart-
ment of Natural Resources and the
Ohio Environmental Protection Agen-
cy, approved by EPA pursuant to sec-
tion 1422 of the SDWA. Notice of this
approval was published in the FEDERAL
REGISTER on November 29, 1984; the ef-
fective date of this program is January
14. 1985. This program consists of the
following elements, as submitted to
EPA in the State's program applica-
tion.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Ohio. This incorporation
by reference was approved by the Di-
rector of the Federal Register effective
January 14, 1985,
(1) Ohio Revised Code Annotated, sec-
tions 1509.01, 1509.03, 1509.221 (Supp.
1983);
(2) Rules of the Division of Oil and
Gas, Ohio Administrative Code, sec-
tions 1501:9-7-01 through 7-14 (1984);
(3) Ohio Revised Code Annotated, sec-
tions 6111.04, 6111.043, 6111.044 (Supp.
1983);
(4) Rules of the Ohio Environmental
Protection Agency, Ohio Administra-
tive Code, sections 3745-34-01 through
34-41; 3745-9-01 through 9-11 (Director
Ohio EPA Order, June 18, 1984).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, also are part of
the approved State-administered
program:
(1) Ohio Revised Code, Chapter 119
(1978 Replacement Part);
(2) Ohio Code Supplement, sections
6111.041, 6111.042, 6111.045 (Supp. 1982).
(c) (1) The Memorandum of Agree-
ment between EPA Region V a.nd the
Ohio Department of Natural Resources,
signed by the EPA Regional Adminis-
trator on March 30, 1984;
(2) Memorandum of Agreement be-
tween the Ohio Department of Natural
Resources and the Ohio Environmental
Protection Agency, Related to the
Underground Injection Control Pro-
gram for the State of Ohio, signed Au-
gust 1, 1984.
(d) Statement of legal authority. State-
ment from Attorney General of the
State of Ohio, by Senior Assistant At-
torney General, "Underground Injec-
tion Control Program—Attorney Gen-
eral's Statement," July 25, 1984.
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FR 46897, Nov. 29, 19841
779
-------
§147.1802
40 CFR Ch. I (7-1-04 Edition)
§147.1802 Aquifer
served]
exemptions. [Be-
§147.1803 Existing Class I and III
wells authorized by rule—maximum
injection pressure.
The owner or operator shall limit In-
jection pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of
§144.28(f)(3)(i); or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm = (0.8^0.433 Sg) d
where:
Pm = injection pressure at the well head in
pounds per square inch
Sg = specific gravity of injected fluid
(unitless)
d = injection depth in feet.
[49 FE 45308, Nov. 15, 1984]
§ 147.1805 EPA-administered pro-
gram—Indian lands.
(a) Contents, The UIC program for all
classes of wells on Indian lands in the
State of Ohio is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CFE parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements,
(b) Effective date. The effective date
of the UIC program for Indian lands in
Ohio is November 25, 1988.
[53 FB 43089, Oct. 25. 1988, as amended at 56
FR 9418, Mar. 6, 1991]
Subpart LL—Oklahoma
§ 147.1850 State-administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I. Ill, IV,
and V wells in the State of Oklahoma,
except those on Indian lands, is the
program administered by the Okla-
homa State Department of Health, ap-
proved by EPA pursuant to SDWA sec-
tion 1422. Notice of this approval was
published in the FEDERAL REGISTER on
June 24, 1982 (47 FE 27273). The effec-
tive date of this program is July 24.
1982. This program consists of the fol-
lowing- elements, as submitted to EPA
in the State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Oklahoma. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Oklahoma Statutes title 63 sec-
tions 1-901, 1-903 (1981);
(2) Oklahoma Controlled Industrial
Waste Disposal Act, Oklahoma Statute
Annotated title 63 sections 1-2002, 1-
2014 (West Supp. 1983-1984);
(3) Regulations. [Reserved]
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for select
sections identified in paragraph (a) of
this section, are also part of the ap-
proved State-administered UIC pro-
gram:
(1) Oklahoma Open Meeting Act,
Oklahoma Statutes title 25 sections 301
through 314 (Supp. 1978);
(2) Oklahoma Statutes Annotated
title 63 sections 1-101 to 1-114, 1-901 to
1-911, 1-1601 et seq., 1-1701, 1-2001 to 1-
2014 (West 1973 and Supp. 1982);
(3) Oklahoma Statutes Annotated
title 75 sections 301 to 327 (West 1976
and Supp. 1982).
(c) (1) The Memorandum of Agree-
ment between EPA Region VI and the
Oklahoma State Department of Health,
signed by the EPA Regional Adminis-
trator on April 13, 1982;
(2) Memorandum of Understanding
between the Oklahoma State Depart-
ment of Health and the Oklahoma Cor-
poration Commission (OCC), signed by
members of the OCC on February 12,
1982;
(3) Memorandum of Understanding
between the Oklahoma State Depart-
ment of Health and the Oklahoma De-
partment of Mines (ODM), signed by
the Deputy Chief Mine Inspector, ODM,
on February 15, 1982.
(d) Statement of legal authority. Letter
from Attorney General of Oklahoma to
Commissioner of Health, Oklahoma
State Department of Health, "Re:
Statement and Memorandum of Law
Concerning the Authority for the Okla-
homa State Department of Health's
780
-------
Environmental Protection Agency
§147.1900
Underground Injection Control Pro-
gram," February 12, 1982.
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43090, Oct. 25, 1988]
§ 147.1851 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Oklahoma, including the
lands of the Five Civilized Tribes, but
not including those on other Indian
lands, is the program, administered by
the Oklahoma Corporation Commission
approved by EPA pursuant to SDWA
section 1425. Notice of this approval
was published in the FEDERAL REG-
ISTER on December 2, 1981 (46 FR 58588).
This program consists of the following
elements, as submitted to EPA in the
State's program application;
(a) Incorporation by reference. [Re-
served]
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, are also part of
the approved State-administered UIC
program:
(1) Oklahoma Statutes, title 17 sec-
tions 51-53; title 52 sections 86.1-86.5,
139-153, 243, 307-318.1 (1971).
(2) OCOOGE Rules No. 1-101-3-303.
(c) (1) The Memorandum of Agree-
ment between EPA Region VI and the
Oklahoma Corporation Commission,
signed by the EPA Regional Adminis-
trator on April 13, 1981;
(2) Letter from the Manager, Under-
ground Injection Control, Oklahoma
Corporation Commission, to EPA, June
18, 1981.
(d) Statement of legal authority.
"Statement of Legal Authority of the
Oklahoma Corporation Commission to
Conduct an Underground Injection
Control Program," (Part IV, pages 30-41
of "State of Oklahoma Primacy Appli-
cation for Authority to Regulate Class
II Injection Wells," submitted April 14,
1981), signed by the Conservation At-
torney, Counsel to the Director and the
Oklahoma Corporation Commission.
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PE 20.197, May 11, 1984, as amended at 53
FR 43090, Oct. 25, 1988]
§ 147.1852 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
wells on Indian lands in Oklahoma, ex-
cept Class II wells on the lands of the
Five Civilized Tribes, is administered
by EPA. The UIC program for Class II
wells on the Osage Mineral Reserve
consists of the requirements set forth
in subpart GGG of this part. The UIC
program for all other wells on Indian
lands consists of the requirements set
forth in subpart III of this part. Injec-
tion well owners and operators and
EPA shall comply with these require-
ments.
(b) Effective date. The effective date
for UIC program for Class II wells on
the Osage Mineral Reserve is December
30, 1984. The effective date for the UIC
program for all other wells on Indian
lands is November 25, 1988.
[53 PR 43090, Oct. 25, 1988]
Subpart MM—Oregon
§ 147.1900 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of Oregon, except
those on Indian lands, is administered
by the Oregon Department of Environ-
mental Quality, approved by EPA pur-
suant to section 1422 and section 1425 of
the SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
September 25, 1984; the effective date of
this program is October 9, 1984. This
program consists of the following ele-
ments, as submitted to EPA in the
State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Oregon. This incorporation
by reference was approved by the Di-
rector of the Federal Register effective
October 9, 1984.
(1) Oregon Revised Statutes, Title 16,
chapter 184, section 164,785; Title 36,
781
-------
§147.1901
40 CFR Ch. I (7-1-04 Edition)
chapter 468, sections 468.005, 468,065 to
468.070, 468.700 to 468.815; Title 43, chap-
ter 520 sections 520.005, 520.095, 520,155—
520.330 (1983);
(2) Oregon Administrative Rules,
Chapter 340, Division 44, sections 340-
44-005 through 340-44-055 (October 1983);
Chapter 340, Division 45, sections 340-
45--005 through 340-45-075 (January
1990); Chapter 632, Division 10, sections
632-10-002 through 632-10-235 (May 1986);
Chapter 632, Division 20, sections 632-
20-005 through 632-20-180 (May 1984).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Oregon Revised Statutes, Chapter
183 (1987); 192.420, 192.500, 459,460(3),
468.005 through 468.605, and 468.780
through 468.997; Chapters 516 and 522
(1983);
(2) Oregon Administrative Rules,
chapter 137, Div. 3 (July 1982); chapter
340, Div. 11 (April 1988): chapter 340,
Div. 12 (March 1989); chapter 340, Div. 14
(November 1983); chapter 340, Div. 52
(November 1983); chapter 632, Div. 1
(June 1980); chapter 632. Div. 20 (Janu-
ary 1981).
(c)(l) The Memorandum of Agree-
ment between EPA Region X and the
Oregon Department of Environmental
Quality, signed by the EPA Regional
Administrator on May 3, 1984.
(d) Statement of legal authority, (1)
"Underground Injection Control Pro-
gram Legal Counsel's Statement," Oc-
tober 1983, signed by the Assistant At-
torney General, Oregon;
(2) Opinion of the Attorney General,
Oregon. 35 Op. Attorney General 1042
(1972).
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 PR 37594. Sept. 25, 1984, as amended at 53
FR 43090. Oct. 25, 1988; 56 FR 9418, Mar. 6,
1991]
§ 147.1901 EPA-administered pro-
gram—Indian lands.
(a) Contents, The UIC program for all
classes of wells on Indian lands in the
State of Oregon is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Oregon is November 25, 1988.
[53 FR 43090, Oct. 25, 1888, as amended at 56
FR 9419, Mar. 6, 1991]
Subpart NN—Pennsylvania
§ 147.1950 State-administered pro-
gram. [Reserved]
§ 147.1951 EPA-administered program.
(a) Contents. The UIC program for the
State of Pennsylvania, including all In-
dian lands, is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CFR parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
for the UIC program on Indian lands is
November 25, 1988. The effective date
for the UIC program for the rest of
Pennsylvania is June 25, 1984.
[53 FR 43090, Oct. 25, 1988, as amended at 56
FR 9419, Mar. 6, 1991]
§ 147.1852 Aquifer exemptions.
(a) This section identifies any
aquifers or their portions exempted in
accordance with §§144.7(b) and 146.4 of
this chapter at the time of program
promulgation. EPA may in the future
exempt other aquifers or portions, ac-
cording to applicable procedures, with-
out codifying such exemptions in this
section. An updated list of exemptions
will be maintained in the Regional
office.
(b) Those portions of the following oil
bearing aquifers, which would other-
wise meet the definition of a USDW,
are exempted in accordance with the
provisions of §§144.7(b) and 146.4 of this
chapter for Class II enhanced recovery
injection activities only.
(1) The Sugar Run and Bradford se-
ries of oil producing sands of the Brad-
ford Field, in McKean County; includ-
ing the Bradford, West Branch, Stack,
782
-------
Environmental Protection Agency
§147.1954
Bennett Brook, Manila Brook, Brooder
Hollow, Cyclone, Minard Bun, Minard
Bun School, and Sugar Bun (or
Watsonville) Pools.
(2) The Bradford Third oil producing
sand of the Guffey Field in McKean
County,
(3) The Bradford series of oil pro-
ducing sands of the Lewis Bun Field in
McKean County.
(4) The Bradford series of oil pro-
ducing sands of the Windfall Field and
Kings Bun Pool in McKean County.
(5) The Bed Valley member of the
Second Sand formation of the Venango
Group of oil producing sands in the
Foster-Beno Field in Venango County;
including the Foster, Bully Hill, Vic-
tory, Bredinsburg, Egypt Corners,
Beno, Monarch Park and Seneca Pools.
(6) The Glade and Clarendon oil pro-
ducing sands of the Morrison Bun Field
and Elk Bun Pool in Warren County.
(7) The Clarendon and Glade oil pro-
ducing sands of the Clarendon Field in
Warren County.
(8) The Bradford Third oil producing
sand in the Shinglehouse Field, includ-
ing the Kings Bun, Janders Bun and
Ceres Pools in Potter and McKean
Counties.
§147.1953 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144.28(f)(3)
(i) or (ii) as applicable or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.733— 0.433
where:
Pm=mjection pressure at the well head in
pounds per square inch
Sg=specific gravity of injection fluid
(unitless)
d=injeetioB depth in feet.
§147.1954 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating- requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Begional Administrator for the
field or formation in which the well is
located. The Begional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided he submits a request in writing
to the Begional Administrator, and
demonstrates to the satisfaction of the
Begional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii) (A) and
(B). The Begional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a public hearing, according
to the provisions of part 124, subpart A
of this chapter.
(2) Prior to such time as the Begional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(ii) of tip? section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of il44.28(f)(3)(ii):
and
(ii) Submit data acceptable to the
Begional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Begional Administrator approves
such submission. The information shall
be submitted to the Begional Adminis-
trator within one year of the effective
date of this regulation.
(b) Casing and cementing. Where the
Begional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§ 144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
783
-------
§147.1955
40 CFR Ch. I (7-1-04 Edition)
of this section, when required by the
Regional Administrator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most TJSDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(iii) For wells as described in
§146.8(b)(3)(ii), installing a smaller di-
ameter pipe inside the existing injec-
tion tubing and setting it on an appro-
priate packer; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 50 feet
ataoye the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section as needed to protect
USDWs.
§ 147.1955 Requirements for wells au-
thorized by permit,
(a) The owner or operator of a Class
I well authorized by permit shall in-
stall or shall ensure that the well has:
(1) Surface casing present;
(i) Extending from the surface to a
depth at least 50 feet below the base of
the lowermost USDW; and
(ii) Cemented back to the surface by
recirculating the cement; and
(2) Long string casing and tubing:
(i) Extending to the injection zone;
and
(ii) Cemented back to 50 feet above
the base of the next largest casing
string.
(b) The owner or operator of a new
Class II well authorized by permit
shall:
(1) Install surface casing from the
surface to at least 50 feet below the
base of the lowermost USDW.
(2) Cement the casing by recircu-
lating to the surface or by using no less
than 120% of the calculated annular
volume.
(3) For new enhanced recovery wells.
install tubing or long string casing ex-
tending to the injection zone.
(4) For new salt water disposal wells,
install long string casing and tubing
extending to the injection zone.
(5) Isolate any injection zone by plac-
ing sufficient cement to fill the cal-
culated yolume to a point 50 feet above
the injection zone.
(c) The Regional Administrator may
specify casing and cementing require-
ments other than those listed in para-
graphs (a) and (b) of this section on a
case by case basis as conditions of the
permit.
Subpart OO—Rhode Island
§ 147.2000 State-administered pro-
gram—Class I, II, III, IV, and V
wells.
The UIC program for all classes of
wells in Rhode Island, except those on
Indian lands, is the program adminis-
tered by the Rhode Island Department
of Environmental Management, ap-
proved by EPA pursuant to section 1422
of the SDWA. Notice of this approval
was published in the FEDERAL REG-
ISTER on August 1, 1984; the effective
date of this program is August 15, 1984.
This program consists of the following
elements, as submitted to EPA in the
State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Rhode Island. This incor-
poration by reference was approved by
the Director of the Federal Register ef-
fective August 15, 1984.
(1) Rhode Island Gen. Laws sections
46-12-1. 46-12-5, and 46^12-28 (Supp.
1983);
(2) "Underground Injection Control
Program Rules and Regulations." State
of Rhode Island-and Providence Planta-
tions Department of Environmental
784
-------
Environmental Protection Agency
§147.2050
Management. Division of Water Re-
sources (as received by the Secretary of
State, May 21, 1984).
(b) Other laws. The following statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Rhode Island General Laws, Sec-
tion 10-20-1 et seq., entitled "State En-
vironmental Rights";
(2) Rhode Island General Laws, Sec-
tion 23-19.1-1 et seq., entitled "Haz-
ardous Waste Management";
(3) Rhode Island General Laws, Sec-
tion 42-17.1 et seq., entitled "Depart-
ment of Environmental Management";
(4) Rhode Island General Laws, Sec-
tion 42-35-1 et seq., entitled "Adminis-
trative Procedures";
(5) Rhode Island General Laws, Sec-
tion 46-12-1 et seq., entitled "Water
Pollution";
(6) Hazardous Waste Management
Facility Operating Permit Rules and
Regulations—Landfills, at last amend-
ed November 2, 1981 (hereinafter re-
ferred to as the "Hazardous Waste Reg-
ulation");
(7) Water Quality Regulations for
Water Pollution Control, effective No-
vember 19,1981; and
(8) Administrative Rules of Practices
and Procedure for Department of Envi-
ronmental Management, effective No-
vember 12, 1980.
(c) (1) The Memorandum of Agree-
ment between EPA Region I and the
Rhode Island Department of Environ-
mental Management, signed by the
EPA Regional Administrator on March
29, 1984;
(2) Letter from Director, Rhode Is-
land Department of Environmental
Management, to Regional Adminis-
trator, EPA Region I, amending Sec-
tion III, C of the Memorandum of
Agreement, April 25, 1984.
(d) Statement of legal authority. Letter
fr'om Attorney General, State of Rhode
Island and Providence Plantations, to
Regional Administrator, EPA Region 1.
"Re: Attorney General's Statement,
Underground Injection Control Pro-
gram," January 17, 1984,
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FR 30699, Aug. 1, 1984, as amended at 53
PE 43090, Oct. 25, 1988]
§ 147.2001 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Rhode Island is administered
by EPA, This program consists of the
UIC program requirements of 40 CPR
parts 124, 144, 146, 148, and any addi-
tional requirements set forth in the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Rhode Island is November 25, 1988.
[53 FR 43090, Oct. 25.
FE 9419, Mar. 6, 1991]
8, as amended at 56
Subpart PP—South Carolina
1147.2050 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of South Carolina,
except for those on Indian lands, is the
program administered by the South
Carolina Department of Health and En-
vironmental Control, approved by EPA
pursuant to section 1422 of the SDWA.
Notice of this approval was published
in the FEDERAL REGISTER on July 10,
1984; the effective date of this program
is July 24, 1984. This program consists
of the following elements, as submitted
to EPA in the State's program
application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of South Carolina. This in-
corporation by reference was approved
by the Director of the Federal Register
effective July 24, 1984.
(1) Pollution Control Act, S.C. Code
Ann. Sections 48-1-10, 48-1-90. 48-1-100.
48-1-110 (Law. Co-op. 1976 and Supp.
1983).
(2) South Carolina Department of
Health and Environmental Control,
785
-------
§147.2051
40 CFR Ch. I (7-1-04 Edition)
Ground-Water Protection Division, Un-
derground Injection Control Regula-
tions, B-61-87, Effective Date: June 24,
1983 Published in South Carolina State
Register, Volume 7, Issue 6; Amended
Date: March 23, 1984, as amended by no-
tice in South Carolina State Register,
Volume 8, Issue 3.
(b) Other laws. The following' statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-Administered pro-
gram:
(1) Pollution Control Act, B.C. Code
Ann. Sections 48-1-10 to 48-1-360 {Law.
Co-op. 1976 and Supp. 1983).
(2) State Safe Drinking Water Act,
S.C. Code Ann. Sections 44-55-10 to 44-
55-100 (Law. Co-op. 1976 and Supp. 1983).
(3) Administrative Procedures Act,
S.C. Code Ann. Sections 1-23-10 et seq.,
and 1-23-310 to 1-23-400 (Law. Co-op.
1976 and Supp. 1983).
(4) S.C. Code Ann. Sections 15-5-20,
15-5-200 (Law. Co-op. 1976 and Supp.
1983).
(c)(l) The Memorandum of Agree-
ment between EPA Region IV and the
South Carolina Department of Health
and Environmental Control signed by
the EPA Regional Administrator on
May 29, 1984.
(d) Statement of legal authority. (1)
"Underground Injection Control Pro-
gram, Attorney General's Statement
for Class I, II, III, IV and VA and VB
Wells," signed by the Attorney General
of South Carolina on April 27, 1984.
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FB 28058, July 10. 1984, as amended at 53
PR 43090, Oct. 25, 1988]
§ 147.2051 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Rhode Island is administered
by EPA. This program consists of the
UIC program requirements of 40 CPR
parts 124, 144, 146, 148, and any addi-
tional requirements set forth in the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
South Carolina is November 25,1988.
[53 PR 43090, Oct. 25, 1988, as amended at 56
PR 9419, Mar. 6, 1991]
Subpart QQ—South Dakota
§ 147.2100 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of South Dakota, except
those on Indian lands, is the program
administered by the South Dakota De-
partment of Water and Natural Re-
sources, approved by EPA pursuant to
section 1425 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on October 24, 1984; the
effective date of this program is De-
cember 7, 1984. This program consists
of the following elements, as submitted
to EPA in the State's program
application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of South Dakota. This incor-
poration by reference was approved by
the Director of the Federal Register ef-
fective December 7, 1984.
(1) South Dakota Codified Laws, sec-
tions 45-9-2. 45-9-4, 45-9-11, 45-9-13, 45-
9-14, 45-9-15 (1983).
(2) Administrative Rules of South
Dakota, sections 74:10:02 through
74:10:07, 74:10:09, and 74:10:11 published
by the South Dakota Code Commis-
sion, as revised through October 4, 1987.
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, also are part of
the approved State-administered
program:
(1) South Dakota Codified Laws,
Chapter 45-9 (sections not cited above)
(1983): 1-26 (1981).
(c)(l) The Memorandum of Agree-
ment between EPA Region VIII and the
South Dakota Department of Water
and Natural Resources, signed by the
EPA Regional Administrator on July
18, 1984.
786
-------
Environmental Protection Agency
§147.2103
(d) Statement of legal authority. (1)
"Underground Injection Control Pro-
gram for Class II Wells: Attorney Gen-
eral's Statement," signed by Mark V.
Meierhery, Attorney General, South
Dakota, on January 16, 1984.
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[50 FR 7061, Feb. 20. 1985. as amended at 56
FR 9419. Mar, 6.1991]
§ 147.2101 EPA-administered pro-
gram—Class I, III, IV and V wells
and all wells on Indian lands.
(a) Contents. The UIC program for all
Class I, III, IV, and V wells, including-
those on Indian lands, and for Class II
wells on Indian lands in the state of
South Dakota is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CPU parts 124,
144, 146. 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective date. The effective date
of the UIC program for Class I, III, IV
and V wells on all lands in South Da-
kota, including Indian lands, and for
Class II wells on Indian lands only, is
December 30, 1984.
[52 PR 17682, May 11, 1987. as amended at 56
FR 9419, Mar. 6, 1991]
§ 147.2102 Aquifer exemptions.
(a) This section identifies any
aquifers or their portions exempted in
accordance with §§144.7(b) and 146.4 of
this chapter at the time of program
promulgation. EPA may in the future
exempt other aquifers or their por-
tions, according to applicable proce-
dures, without codifying such exemp-
tions in this section. An updated list of
exemptions will be maintained in the
Regional office.
(b) Those portions of all aquifers lo-
cated on Indian Lands, which meet the
definition of USDW and into which ex-
isting Class II wells are injecting, are
exempted within a 14 mile radius of the
well for the purpose of Class II injec-
tion activities only.
[49 FR 45308, Nov. 15, 1984]
§147.2103 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum injection pressure. (1) To
meet the operating requirements of
|144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(1) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ments, and opportunity for a public
hearings, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at a pressure greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating pro-
vided lie submits a request in writing
to the Regional Administrator, and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of §144.28(f)(3)(ii)(A) and (B).
The Regional Administrator may grant
such a request after notice, oppor-
tunity for comment, and opportunity
for a public hearing, according to the
provisions of part 124, subpart A of this
chapter.
(2) Prior to such time as the Regional
Administrator establishes field rules
for maximum injection pressure based
on data provided pursuant to para-
graph (a)(2)(ii) of this section the
owner or operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit to the Regional Adminis-
trator data acceptable to the Regional
administrator which defines the frac-
ture pressure of the formation in which
injection is taking place. A single test
may be submitted on behalf of two or
more operators conducting operations
in the same formation, if the Regional
Administrator approves such submis-
sion.
(b) Casing and, cementing. Where the
Regional Administrator determines
787
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§147.2104
40 CFR Ch. I (7-1-04 Edition)
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirement of §§ 144.28(e) and
146.22, the owner or operator shall when
required by the Regional Adminis-
trator:
(1) Protect USDWs by:
(i) Cementing surface casing by recir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operation
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(ill) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone; and/or
(4) Comply with other requirements
which the Regional Administrator may
specify in addition to or in lieu of the
requirements set forth in paragraphs
(b) (1) through (3) of this section as
needed to protect USDWs.
[49 PR 45308, Nov. 15, 1984]
§ 147.2104 Requirements for all wells.
(a) The owner or operator converting
an existing well to an injection well
shall check the condition of the casing
with one of the following logging tools:
(1) A pipe analysis log; or
(2) A caliper log.
(b) The owner or operator of a new
injection well cased with plastic (PVC,
ABS, or others) casings shall:
(1) Not construct a well deeper than
500 feet:
(2) Use cement and additives compat-
ible with such casing material; and
(3) Cement the annular space above
the injection intermal from the bottom
of the blank casing to the surface.
(c) The owner or operator of a newly
drilled well shall install centralizers a-s
directed by the Regional Adminis-
trator.
(d) The owner or operator shall as re-
quired by the Regional Administrator;
(1) Protect USDWs by:
(i) Setting surface casing 50 feet
below the lowermost USDW:
(ii) Cementing surface casing by re-
circulating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ill) Isolating all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement:
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure; and
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
approve alternate casing and cement-
ing practices provided that the owner
or operator demonstrates that such
practices will adequately protect
USDWs.
(e) Area of review. Notwithstanding
the alternatives presented in §146.6 of
this chapter, the area of review shall be
a fixed radius as described in §146.6(b)
of this chapter.
(f) The applicant must give separate
notice of intent to apply for a permit
to each owner of record of the land
within one-quarter mile of the site.
The addresses of those to whom notice
is given and the description of how no-
tice was given shall be submitted with
the permit application. The notice
shall include:
(1) The name and address of appli-
cant:
(2) A brief description of the planned
injection activities, including well lo-
cation, name and depth of the injection
zone, maximum injection pressure and
volume, and fluid to be injected;
(3) The EPA contact person; and
(4) A statement that opportunity to
comment will be announced after EPA
prepares a draft permit.
788
-------
Environmental Protection Agency
§147.2154
This requirement may be waived by the
Regional Administrator if he deter-
mines that individual notice to all land
owners of record would be impractical.
[49 PR 45308, No¥. 15, 1984]
Subpart RR—Tennessee
§ 147.2150 State-administered
gram. [Reserved]
pro-
§ 147.2151 EPA-administered program.
(a) Contents, The UIC program for the
State of Tennessee, including all In-
dian lands, is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CPR parts 124,
144, 146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. Effective date for
the UIC program on Indian lands is No-
vember 25, 1988. The effective date for
the UIC program for the rest of Ten-
nessee is June 25, 1984.
[53 PE 43090, Oct. 25, 1988, as amended at 56
FE 9419, Mar, 6, 1991]
§147.2152 Aquifer exemptions. [Re-
served]
§147.2153 Existing Class I, II (except
enhanced recovery and hydro-
carbon storage) and III wells au-
thorized by rule.
Maximum injection pressure. The
owner or operator shall limit injection
pressure to the lesser of:
(a) A value which will not exceed the
operating requirements of §144,28(f)(3)
(i) or (ii) as applicable or
(b) A value for well head pressure cal-
culated by using the following formula:
Pm=(0.600-0.433 Sg)d
where:
Pm=ijijection pressure at the well head in
pounds per square inch
Sgr=specific gravity of inject fluid (unltless)
d=injectlon depth in feet.
S 147.2154 Existing Class II enhanced
recovery and hydrocarbon storage
wells authorized by rule.
(a) Maximum- injection pressure. (1) To
meet the operating requirements of
§144.28(f)(3)(ii) (A) and (B) of this chap-
ter, the owner or operator:
(i) Shall use an injection pressure no
greater than the pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing, according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure; or
(ii) May inject at pressures greater
than those specified in paragraph
(a)(l)(i) of this section for the field or
formation in which he is operating,
provided he submits a request in writ-
ing to the Regional Administrator and
demonstrates to the satisfaction of the
Regional Administrator that such in-
jection pressure will not violate the re-
quirement of § 144.28(f>(3)(ii) (A) and
(B). The Regional Administrator may
grant such a request after notice, op-
portunity for comment, and oppor-
tunity for a puhlic hearing, according
to the provisions of part 124, subpart A
of this chapter.
(2) Prior to such time as the Regional
Administrator establishes rules for
maximum injection pressure based on
data provided pursuant to paragraph
(a)(2)(ii) of this section the owner or
operator shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of §144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within one year of the effective date of
this regulation,
(b) Casing and cementing. Where the
Regional Administrator determines
that the owner or operator of an exist-
ing enhanced recovery or hydrocarbon
storage well may not be in compliance
with the requirements of §§144.28(e) and
146.22, the owner or operator shall com-
ply with paragraphs (b) (1) through (4)
789
-------
§147.2155
40 CFR Ch. I (7-1-04 Edition)
of this section, when required by the
Regional Administrator:
(1) Protect TJSDWs by:
(i) Cementing surface casing by reeir-
culating the cement to the surface
from a point 50 feet below the lower-
most USDW; or
(ii) Isolating- all USDWs by placing
cement between the outermost casing
and the well bore; and
(2) Isolate any injection zones by
placing sufficient cement to fill the
calculated space between the casing
and the well bore to a point 250 feet
above the injection zone; and
(3) Use cement;
(i) Of sufficient quantity and quality
to withstand the maximum operating
pressure;
(ii) Which is resistant to deteriora-
tion from formation and injection
fluids; and
(iii) In a quantity no less than 120%
of the calculated volume necessary to
cement off a zone.
(4) The Regional Administrator may
specify other requirements in addition
to or in lieu of the requirements set
forth in paragraphs (b) (1) through (3)
of this section, as needed to protect
USDWs.
§ 147.2155 Requirements for all wells—
area of review.
Notwithstanding the alternatives
presented in § 146.6 of this chapter, the
area of review shall be a minimum
fixed radius as described in §146.6(b) of
this chapter.
Subpart SS—Texas
§ 147.2200 State-administered pro-
gram—Class I, III, IV, and V wells.
The UIC program for Class I, in, IV,
and V wells in the State of Texas, ex-
cept for those wells on Indian lands,
Class III brine mining wells, and cer-
tain Class V wells, is the program ad-
ministered by the Texas Commission
on Environmental Quality approved by
EPA pursuant to section 1422 of the
Safe Drinking Water Act (SDWA). No-
tice of the original approval for Class I.
Ill, IV, and V wells was published in
the FEDERAL REGISTER on January 6,
1982 and became effective February 7,
1982. Class V geothermal wells and
wells for the in situ combustion of coal
are regulated by the Bail Road Com-
mission of Texas under a separate UIC
program approved by EPA and pub-
lished in the FEDERAL REGISTER on
April 23, 1982. A subsequent program re-
vision application for Class I, III, IV,
and V wells, not including Class III
brine mining wells, was approved by
the EPA pursuant to section 1422 of
SDWA. Notice of this approval was
published in the FEDERAL REGISTER on
February 25, 2004; the effective date of
these programs is March 26, 2004, The
program for Class I, III. IV, and V
wells, not including Class III brine
mining wells, consists of the following
elements as submitted to the EPA in
the State's revised program applica-
tions. The UIC program for Class III
brine mining wells in the State of
Texas, except for those wells on Indian
lands, is the program administered by
the Railroad Commission of Texas. A
program revision application for Class
III brine mining wells was submitted
by Texas and approved by EPA. Notice
of that approval was published in the
FEDERAL REGISTER on February 26,
2004; the effective date of this program
is March 29, 2004,
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made part of the applicable
UIC program under SDWA for the
State of Texas. This incorporation by
reference was approved by the Director
of the Federal Register in accordance
with 5 U.S.C. 552(a) and 1 CFR part 51.
Copies of the materials that are incor-
porated by reference in this paragraph
are available at EPA Region VI, 1445
Ross Avenue, Dallas, TX 75202 or from
the National Archives and Records Ad-
ministration (NARA), For information
on the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archives.gov/fe.d-eral register/
code_of_federal_ regulations/
ibr locations. html..
(1) Texas Statutory and Regulatory
Requirements Applicable to the Under-
ground Injection Control Program for
Class I, III, IV, and V Wells, except for
Class III Brine Mining Wells, March
2002.
790
-------
Environmental Protection Agency
§147,2201
(2) Texas Statutory and Regulatory
Requirements Applicable to the Under-
ground Injection Control Program for
Class III Brine Mining Wells, March
2002.
(b) Other laws. The following statutes
and regulations, as effective on March
31, 2002, although not incorporated by
reference except for any provisions
identified in paragraph (a) of this sec-
tion, are also part of the approved
State-administered UIC program.
(1) Class I, III, IV, and V wells, (i)
Title 30 of the Texas Administrative
Code Chapters 39, 50, 55, 80, and 281.
(ii) Vernon's Texas Codes Annotated,
Water Code, Chapters 5, 7, 26, and 32,
Health and Safety Code Section 361,
Government Code (DBA) Chapter 552
and Government Code (APA) Chapter
2001.
(2) Class III brine mining wells, (i)
Vernon's Texas Codes Annotated, Nat-
ural Resources Code, Chapters 91, 2001,
and 331;
(ii) Vernon's Texas Codes Annotated,
Government Code Title 10, Chapters
2001, 552, and 311.
(iii) General Rules of Practice and
Procedure before the Railroad Commis-
sion of Texas.
(c) Memorandum of Agreement—(1)
Class /, III, IV, and V wells. The Memo-
randum of Agreement between EPA
Region VI and the Texas Natural Re-
source Conservation Commission a
predecessor to the Texas Commission
on Environmental Quality (TCEQ), re-
vised March 23, 1999, and signed by the
EPA Regional Administrator on Octo-
ber 23, 2001.
(2) Class III brine mining wells. The
Memorandum of Agreement between
EPA Region VI and the Railroad Com-
mission of Texas signed by the EPA
Regional Administrator on October 23,
2001.
(d) Statement of legal authority—(1)
Class I, III, IV, and V wells. "State of
Texas Office of Attorney General
Statement for Class I, III, IV, and V
Underground Injections Wells," signed
by the Attorney General of Texas, June
30, 1998.
(2) Class III brine mining wells. State
of Texas "Attorney General's State-
ment" for Class III Brine Mining Injec-
tion Wells, signed by the Attorney
General of Texas, February 2, 1992 and
the "Supplement to Attorney General's
Statement of February 19, 1992," signed
by the Attorney General of Texas, June
2, 1998.
(e) Program Description—(1) Class /,
///, IV, and V wells. The Program De-
scription and any other materials sub-
mitted as part of the revision applica-
tion or as supplements thereto.
(2) Ctoss III brine mining wells. The
Program Description and any other
materials submitted as part of the revi-
sion application or as supplements
thereto.
[69 FK 8568, Feb. 25, 2004, as amended at 69
PR 8828, Feb. 26, 2004]
§ 147.2201 State-administered pro-
gram—Class II wells
The UIC program for Class II wells in
the State of Texas, except for those
wells on Indian lands, is the program
administered by the Railroad Commis-
sion of Texas, approved by EPA pursu-
ant to section 1425 of the SDWA. Notice
of this approval was published in the
FEDERAL REGISTER on April 23, 1982 (47
PR 17488). The effective date of this
program was May 23, 1982. This pro-
gram consists of the following ele-
ments, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Texas. This incorporation
by reference was approved by the Di-
rector of the Federal Register on June
25, 1984.
(1) Injection Well Act, Texas Water
Code Annotated sections 27.031 and
27.033 (Vernon Supp. 1984);
(2) Texas Natural Resources Code An-
notated sections 85.041, 85.045, 85.046
and 85.052 (Vernon 1978 and Supp. 1982);
(3) Rules Having Statewide General
Application to Oil, Gas, and Geo-
thermal Resource Operations, sections
.051.02.02.000 to .051.02.02.080 (Railroad
Commission of Texas, Oil and Gas Divi-
sion, Revised 12-22-81), amended as fol-
lows:
(i) Amendment to 16 TAG section 3.9
(section .051.02.02.009) issued December
21,1981, effective April 1, 1982;
791
203-160 D-26
-------
§147,2205
40 CFR Ch. I (7-1-04 Edition)
(li) Amendment to 16 TAO section
3.46 (section .051,02.02.046) issued De-
cember 21, 1981, effective April 1, 1982.
(ill) Amendment to 16 TAC section
3.71 (section .051.02.02.074) issued De-
cember 21,1981, effective April 1,1982.
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference, are also part of
the approved State-administered UIC
program:
(1) Texas Water Code, Chapters 26, 27
and 29 (Yernon 1972 and Supp. 1982);
(2) Texas Natural Resources Code,
Chapters 81. 85-89, 91 and 141 (Vernon
1978 and Supp. 1982);
(3) General Rules of Practice and
Procedure, Subchapters A-J (Railroad
Commission of Texas, adopted Novem-
ber 24, 1975, revised December 1980).
(c)(l) The Memorandum of Agree-
ment between EPA Region VI and the
Railroad Commission of Texas, signed
by the EPA Regional Administrator on
March 24, 1982.
(2) Letter from Director of Under-
ground Injection Control, Railroad
Commission of Texas, to Chief, Ground
Water Protection Section, EPA Region
VI, "Re: Letter of Clarification—UIC
Program Application," March 21, 1982.
(d) Statement of legal authority.
"Statement of Legal Authority of the
Railroad Commission of Texas to con-
duct the Underground Injection Con-
trol Program," signed by Special Coun-
sel, Railroad Commission of Texas, as
submitted with "State of Texas Under-
ground Injection Control Program Ap-
plication for Primacy Enforcement Au-
thority," prepared by the Railroad
Commission of Texas, January 15, 1982.
(e) The Program Description and any
other materials submitted as part of
the application or as supplements
thereto.
[49 PR 20197, May 11, 1984, as amended at 53
PB 43091, Oct. 25, 1988]
§ 147.2205 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Texas is administered by EPA.
This program consists of the UIC pro-
gram requirements of 40 CPR parts 124,
144,146,148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective date. The effective date
for the Indian lands program for the
State of Texas is November 25,1988.
[53 FR 43091, Oct. 25, 1988, as amended at 56
PR 9419, Mar. 6, 1991]
Subpart TT—Utah
§ 147.2250 State-administered pro-
gram—Class I, III, IV, and V wells.
The UIC program for Class I, III, IV,
and V wells in the State of Utah, ex-
cept those on Indian lands, is adminis-
tered by the Utah Department of
Health, Division of Environmental
Health, approved by EPA pursuant to
Section 1422 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on January 9, 1983 (47
PR 2321). The effective date of this pro-
gram is February 10, 1983. Changes to
Utah's regulations for Class I wells
were made on May 15, 1990, in response
to modification of national rules as
promulgated by 53 PR 28188, July 26,
1988. Utah's rules were effective July
20, 1990. The revised rules, Program De-
scription, Attorney General's state-
ment, and Memorandum, of Agreement
were approved as a minor program
modification on October 3, 1990. This
program consists of the following ele-
ments as submitted to EPA:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Utah. This incorporation
by reference was approved by the Di-
rector of the Federal Register on June
25,1984.
(1) Utah Water Pollution Control
Act, Utah Code Annotated, Title 26,
Chapter 11, Sections 2, 8, and 10 (1989);
(2) Underground Injection Control
Regulations; Utah Administrative
Code, Section R448-7 (effective as of
January 2,1990);
(3) Underground Injection Control
Program (adopted January 20, 1982 and
revised effective July 20, 1990) (Offi-
cially submitted to EPA by the Execu-
tive Secretary of Utah Water Pollution
Control Committee on August 16, 1990).
792
-------
Environmental Protection Agency
§147.2251
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for se-
lected sections identified in paragraph
(a) of this section, are also part of the
approved State-administered program:
(1) Utah Pollution Control Act, Utah
Code Annotated, Sections 26-11-1
through -20 (Supp. 1990);
(c)(l) The revised Memorandum of
Agreement between EPA, Region VIII
and the Utah Department of Health,
Division of Environmental Health,
signed by the Regional Administrator
on October 3, 1990.
(2) Letter from Director, Utah De-
partment of Health, Division of Envi-
ronmental Health, Bureau of Water
Pollution Control, to EPA Region VIII,
Re: Underground Injection Control
Program—Utah, March 15, 1982;
(3) Letter from the Executive Sec-
retary of the Utah Water Pollution
Control Committee to EPA Region
VIII, "Re: Utah UIC Class I Well Pro-
gram Changes," August 16, 1990;
(d) Statement of legal authority. (1)
"Underground Injection Control Pro-
gram—Attorney General's statement,"
signed by Attorney General, State of
Utah, January, 1982;
(2) Letter from Assistant Attorney
General of Utah to Chief, Drinking
Water Branch, EPA Region VIII, June
18, 1982;
(3) Addendum to Underground Injec-
tion Control Program, Attorney Gen-
eral's Statement signed by Attorney
General of Utah, August 10, 1990.
(e) The Program Description (revised
June 19, 1990) and any other materials
submitted as part of the application or
supplements thereto.
[56 PR 9419, Mar. 6,1991]
§ 147.2251 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Utah, except those on In-
dian lands, is the program adminis-
tered by the Utah Department of Nat-
ural Resources, Division of Oil, Gas,
and Mining, approved by EPA pursuant
to section 1425 of the SDWA. Notice of
this approval was published in the FED-
ERAL REGISTER on October 8, 1982 (47
PR 44561); the effective date of this pro-
gram is November 7, 1982. This program
consists of the following elements, as
submitted to EPA in the State's pro-
gram application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Utah. This incorporation
by reference was approved by the Di-
rector of the Federal Register on June
25, 1984.
(1) Utah Code Annotated, 1953, sec-
tion 40-6-1 through 40-6-18, as amended
1988 and Cumm. Supp. 1990;
(2) The Oil and Gas Conservation
General Rules, adopted under the au-
thority of the Oil and Gas Conservation
Act, 40-6-1 et seq., Utah Code Anno-
tated, as amended 1988 (revised March
1989), rules R615-1 through R615-4, and
R615-8 through R615-10.
(b) Other laws. [Reserved]
(c)(l) The Memorandum of Agree-
ment between EPA, Region VIII and
the Utah Department of Natural Re-
sources, Division of Oil, Gas, and Min-
ing and the Board of Oil, Gas and Min-
ing, signed by the EPA Regional
Administrator on July 19,1983;
(2) Letter from Director, Division of
Oil, Gas and Mining, Utah Department
of Natural Resources and Energy, to
Regional Administrator, EPA Region
VIII, "Re: Aquifer Exemption Process,"
June 16,1982;
(3) "Memorandum of Understanding"
between Utah Department of Health
and Utah Department of Natural Re-
sources, dated March 5,1981;
(4) "Second Addition to Agreement
between the Department of Health and
the Department of Natural Resources
and Energy," dated December 15, 1981.
(d) Statement of legal authority. (1)
Part III of "Primacy Application—Class
II Underground Injection Wells," con-
sisting of "Synopsis of Pertinent Stat-
utes and Regulations," "Statement of
Legal Authority," and "Certification by
the Attorney General," by Assistant
Attorney General, Department of Nat-
ural Resources and Energy, dated De-
cember 18, 1981;
(2) Letter from Assistant Attorney
General, State of Utah, to EPA Region
VIII, undated, received in the EPA Of-
fice of Regional Counsel June 10, 1982.
793
-------
§147.2253
40 CFR Ch, I (7-1-04 Edition)
(3) Memorandum to Director, Divi-
sion of Oil, Gas and Mining from As-
sistant Attorney General regarding Un-
derground Injection Control Program,
January 8, 1985.
(e) The Program Description and any-
other materials submitted as part of
the application or amendments there-
to.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43091, Oct. 25, 1988; 56 PR 9420, Mar. 6,
1991]
§ 147.2253 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Utah is administered by EPA.
The program for wells on the lands of
the Navajo and Ute Mountain Ute con-
sists of the requirements set forth at
subpart HHH of this part. The program
for all other wells on Indian lands con-
sists of the TJIO program requirements
of 40 CFR parts 124, 144, 146, 148, and
any additional requirements set forth
in the remainder of this subpart. Injec-
tion well owners and operators, and
EPA shall comply with these require-
ments.
(b) Effective date. The effective date
for this program for all other Indian
lands in Utah (as well ae for the pro-
gram of the Navajo and Ute Mountain
Ute) is November 25, 1988.
[53 FR 40391, Oct. 25, 1988, as amended at 56
PR 9420, Mar. 6, 1991] h
Subpart UU—Vermont
§ 147.2300 State-administered pro-
gram.
The UIC program for all classes of
wells in the State of Vermont, except
those wells on Indian lands, is the
program administered by the Vermont
Department of Environmental Con-
servation, approved by EPA pursuant
to section 1422 of the SDWA. Notice of
this approval was published in the FR
on June 22, 1984; the effective date of
this program is July 6, 1984. This pro-
gram consists of the following ele-
ments:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Vermont. This incorpora-
tion by reference was approved by the
Director of the Federal Register July 6,
1984.
(1) Vt. Stat. Ann. tit. 10, sections
1251, 1259, 1263 (1973 and Supp. 1981), Ef-
fective date: July 1,1982.
(2) Vermont Department of Water Re-
sources and Environmental Engineer-
ing, Chapter 13 Water Pollution Con-
trol Regulations, Subchapter 13.UIC—
Underground Injection Control, Dis-
charges to Injection Wells, Effective
Date: June 21, 1984.
(b) Other laws. The following statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Vt. Stat. Ann. tit. 10, sections 1251
through 1283 (1973 and Supp. 1981).
(2) Vt. Stat. Ann. tit. 10, sections 901
through 911 (1973 and Supp. 1981).
(3) Vt. Stat. Ann. tit. 3, sections 801
through 847 (1973 and Supp. 1981).
(c)(l) The Memorandum of Agree-
ment between EPA Region I and the
Vermont Agency of Environmental
Conservation signed by the EPA Re-
gional Administrator on January 16,
1984.
(d) Statement of legal authority. (1)
"Vermont Attorney General's State-
ment for Classes I, II, III, IV and V In-
jection Wells," signed by Attorney Gen-
eral John J. Easton, Jr., as submitted
with Vermont Application for Primary
Enforcement Responsibility to Admin-
ister the Underground Water Source
Protection Program Pursuant to the
Safe Drinking Water Act and 40 CFR
145.21 through 145.24 (December 20,
1983).
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
(42 U.S.C. 300)
[49 FR 25634, June 22, 1984, as amended at 53
FR 43091, Oct. 25, 1988; 56 FR 9420, Mar. 6,
1991]
794
-------
Environmental Protection Agency
§ 147.2400
§§ 147.2OT1-147.2302 [Reserved]
§ 147.2303 EPA-administered pro-
gram—Indian lands,
(a) Contents. The UIC program for all
classes of wells on Indian lands In the
State of Vermont is administered by
EPA. This program consists of the UIC
program requirements of 40 CPR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands in
Vermont is November 25,1988.
[53 FR 43091, Oct. 25, 1988, as amended at 56
PR 9420, Mar. 6, 1991]
§§ 147.2304-147.2349 [Reserved]
Subpart W—Virginia
§ 147.2850 State-administered pro-
gram. [Reserved]
§ 147.23S1 EPA-administered program.
(a) Contents. The UIC program for the
State of Virginia, including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CPR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
for the UIC program on Indian lands is
November 25, 1988. The effective date
for the UIC program for the remainder
of Virginia is June 25, 1984. (53 PR
43091, October 25, 1988).
[56 FR 9420, Mar. 6, 1991]
§ 147.23S2 Aquifer exemptions. [Re-
served]
Subpart WW—Washington
§ 147.2400 State-administered pro-
gram—Class I, II, III, IV, and V
wells.
The UIC program for Class I, II, III,
TV, and V wells in the State of Wash-
ington other than those on Indian
lands, Is the program administered by
the Washington Department of Ecol-
ogy, approved by EPA pursuant to sec-
tion 1422 of the SDWA. Notice of this
approval was published in the FEDERAL
REGISTER on August 9, 1984; the effec-
tive date of this program is September
24, 1984. This program consists of the
following elements, as submitted to
EPA in the State's program
application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the State of Washington. This incorpo-
ration by reference was approved by
the Director of the Federal Register ef-
fective September 24, 1984.
(1) Revised Code of Washington sec-
tion 90.48.020, 90.48.080, 90.48.160, and
90.48.162 (Bureau of National Affairs,
1983 Laws);
(2) Washington Administrative Code
sections 173-218-010 to 173-218-110 (Bu-
reau of National Affairs, 2/29/84):
(3) Washington Administrative Code
sections 344-12-001 to 344-12-262 (1983
Ed.)
(4) Washington Administrative Code
Chapter 173-160 (reprinted May 1988).
(b) Other laws. The following statutes
and regulations although not incor-
porated by reference, also are part of
the approved State-administered pro-
gram:
(1) Revised Code of Washington, chap-
ter 34.04 (Bureau of National Affairs,
1981 Laws), entitled "Administrative
Procedure act";
(2) Revised Code of Washington, chap-
ter 43.21A (Bureau of National Affairs,
1980 Laws), entitled "Department of
Ecology," as amended by 1983 Wash-
ington Laws, Chapter 270;
(3) Revised Code of Washington, chap-
ter 70.105 (Bureau of National Affairs.
1983 Laws), entitled "Hazardous Waste
Disposal";
(4) Revised Code of Washington, chap-
ter 78.52 (Bureau of National Affairs,
1983 Laws), entitled "Oil and Gas Con-
servation";
(5) Revised Code of Washington, chap-
ter 90.48 (Bureau of National Affairs,
1986 Laws), entitled "Water Pollution
Control."
(c)(l) The Memorandum of Agree-
ment between EPA Region X and the
795
-------
§147.2403
40 CFR Ch. I (7-1-04 Edition)
Washington Department of Ecology,
signed by the EPA Regional Adminis-
trator on May 14,1984;
(2) Memorandum of Agreement be-
tween the Washington Department of
Ecology and Oil and Gas Conservation
Committee, Belated to the Under-
ground Injection Control Program for
the State of Washington, signed March
23, 1984;
(3) Memorandum of Agreement be-
tween the Washington Department of
Ecology and Washington Department
of Natural Resources, Related to the
Underground Injection Control Pro-
gram for the State of Washington,
signed March 23,1984;
(4) Memorandum of Agreement be-
tween the Washington Department of
Ecology and Department of Social and
Health Services, Related to the Under-
ground Injection Control Program for
the State of Washington, signed March
23, 1984;
(d) Statement of legal authority. Letter
from Attorney General of the State of
Washington, by Senior Assistant At-
torney General, to Director, Wash-
ington State Department of Ecology,
"Re: Underground Injection Control
Regulatory Program—Attorney Gen-
eral's Statement," February 28,1984.
(e) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[49 FB 31876, Aug. 9, 1984, as amended at 56
FR 9420, Mar. 6,1991]
§ 147.2403 EPA-admuustered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Washington is administered by
EPA. This program, for all Indian lands
except those of the Colville Tribe, con-
sists of the UIC program requirements
of 40 CFR parts 124, 144, 146, 148, and
any additional requirements set forth
in the remainder of this subpart. Injec-
tion well owners and operators, and
EPA shall comply with these require-
ments.
(b) Effective date. The effective date
for the UIC program for Indian lands in
Washington is November 25,1988.
[53 PR 43091, Oct. 25, 1988, as amended at 56
PR 9420, Mar. 6, 1991]
§ 147,2404 EPA-administered pro-
gram—Colville Reservation.
(a) The UIC program for the Colville
Indian Reservation consists of a prohi-
bition of all Class I, II, III and IV injec-
tion wells and of a program adminis-
tered by EPA for Class V wells. This
program consists of the UIC program
requirements of 40 CFR part 124, 144
and 146 and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
EPA shall comply with these require-
ments. The prohibition on Class I-IV
wells is effective November 25, 1988. No
owner or operator shall construct, op-
erate, maintain, convert, or conduct
any other injection activity thereafter
using Class I-IV wells.
(b) Owners and operators of Class I,
II, III or IV wells in existence on the ef-
fective date of the program shall cease
injection immediately. Within 60 days
of the effective date of the program,
the owner or operator shall submit a
plan and schedule for plugging and
abandoning the well for the Director's
approval. The owner or operator shall
plug and abandon the well according to
the approved plan and schedule.
[53 FB 43091, Oct. 25, 1988]
Subpart XX—West Virginia
§§ 147.2450-147.2452 [Reserved]
§ 147.2453 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of West Virginia is administered
by EPA. This program consists of the
UIC program requirements of 40 CFR
parts 124, 144, 146, 148, and any addi-
tional requirements set forth in the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements.
(b) Effective date. The effective date
for the UIC program on Indian lands in
West Virginia is November 25,1988.
[53 FR 43092, Oct. 25, 1988, as amended at 56
PR 9420, Mar. 6, 1991]
796
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Environmental Protection Agency
§§ 147.2454-147.2499 [Reserved]
Subpart YY—Wisconsin
1147.2500 State-administered pro-
gram.
The UIC program for Class I, II, III,
IV, and V wells in the State of Wis-
consin, other than those on Indian
lands as described in §147.2510, is the
program administered by the Wis-
consin Department of Natural Re-
sources, approved by EPA pursuant to
SDWA section 1422. Notice of this ap-
proval was published in the FEDERAL
REGISTER on September 30, 1983 (48 FR
44783); the effective date of this pro-
gram is November 30, 1983. This pro-
gram consists of a prohibition of all in-
jection wells except heat pump return
flow injection wells and may be found
in the following elements, as submitted
to EPA in the State's program applica-
tion.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Wisconsin. This incorpora-
tion by reference was approved by the
Director of the OFR in accordance with
5 U.S.C. 552(a) and 1 CFR part 51. Cop-
ies may be obtained at the Wisconsin
Department of Natural Resources, Box
7921, Madison, Wisconsin, 53707. Copies
may be inspected at the Environmental
Protection Agency, Region V, 77 West
Jackson Boulevard, Chicago, Illinois,
60604, or at the National Archives and
Records Administration (NARA). For
information on the availability of this
material at NARA, call 202-741-6030, or
go to: http://www.archives.gov/
federal register/
code of federal regulations/
ibr locations.html.
(1) Wisconsin Statutes Annotated
§§147.015, 147.02 and 147.04 (West 1974
and Supp. 1983);
(2) Chapter NR 112, Well Construction
and Pump Installation, Wisconsin Ad-
ministrative Code §§NR 112.03 and
112.20 (October 1981), as amended by
Natural Resources Board Order No.
WQ-25-82, approved by the Natural Re-
sources Board on August 25, 1982;
§147.2500
(3) Chapter NR 113, Servicing Septic
Tanks, Seepage Pits, Grease Traps or
Privies, Wisconsin Administrative
Code |§NR 113.07-113.08 (1979), as
amended by Natural Resources Board
Order No. WQ-25-82, approved by the
Wisconsin Natural Resources Board on
August 25, 1982;
(4) Chapter NR 181, Hazardous Waste
Management, Wisconsin Administra-
tive Code §§NR 181.04-181.415 (1981), as
amended June 1985;
(5) Chapter NR 210, Sewage Treat-
ment Works, Wisconsin Administrative
Code §210.05 Natural Resources Board
Order No. WQ-25-82, approved by the
Wisconsin Natural Resources Board on
August 25, 1982;
(6) Chapter NR 214, Land Application
and Disposal of Liquid Industrial
Wastes and By-Products, Wisconsin Ad-
ministrative Code §§214.03 and 214.08
(1983).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for select
sections identified in paragraph (a) of
this section, are also part of the ap-
proved State-administered program:
(1) Chapter 144, Water, Sewage,
Refuse, Mining and Air Pollution, Wis-
consin Statutes Annotated (West 1974
and Supp. 1983);
(2) Chapter 147, Pollution Discharge
Elimination, Wisconsin Statutes Anno-
tated (West 1974 and Supp. 1983);
(3) Chapter 162, Pure Drinking Water,
Wisconsin Statutes Annotated (West
1974 and Supp. 1983);
(4) Laws of 1981, Chapter 20, §2038 (Re:
heat pump injection);
(5) Wisconsin Statutes 803.09(1) (West
1977) (intervention as of right in civil
actions).
(c) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region V and the Wisconsin De-
partment of Natural Resources, signed
by the Regional Administrator on De-
cember 6, 1983.
(d) Statement of legal authority. (1)
"Attorney General's Statement," signed
by Attorney General, State of Wis-
consin;
(2) Letter from Assistant Attorney
General, State of Wisconsin, to EPA
Region, "Re: Amendments to Attorney
General's Statement-UIC," June 30,
1983.
797
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§147.2510
40 CFR Ch. I (7-1-04 Edition)
(e) Program Description. The Program
Description and other materials sub-
mitted as part of the application or as
supplements thereto.
[49 FR 45309, Nov. 15, 1984, as amended at 56
FR 9420, Mar. 6, 1991; 56 FR 14150, Apr. 5, 1991;
62 FR 1834, Jan. 14, 1997]
§ 147.2510 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for In-
dian lands in the State of Wisconsin is
administered by EPA. This program
consists of 40 CFR parts 144 and 146 and
additional requirements set forth in
this section. Injection well owners and
operators, and EPA, shall comply with
these requirements.
(b) Requirements. Notwithstanding
the requirements of paragraph (a) of
this section for Indian lands in Wis-
consin no owner or operator shall con-
struct, operate, maintain, or convert
any Class I, II, III, IV or V injection
well.
(c) Effective date. The effective date of
the UIC program requirements for In-
dian lands in Wisconsin is December 30,
1984.
[49 FR 45309, Nov. 15, 1984]
Subpart ZZ—Wyoming
§ 147.2550 State-administered pro-
gram—Class I, III, IV and V wells.
The UIC program for Class I, III, IV
and V wells in the State of Wyoming,
except those on Indian lands is the pro-
gram administered by the Wyoming
Department of Environmental Quality
approved by EPA pursuant to section
1422 of the SDWA. Notice of this ap-
proval was published in the FEDERAL
REGISTER on July 15, 1983 (48 FR 32344);
the effective date of this program is
August 17, 1983. The program consists
of the following elements as submitted
to EPA in the State's program applica-
tion:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Wyoming. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Wyoming Environmental Quality
Act, Wyoming Statutes sections 35-11-
101 through 35-11-115, and 35-11-301
through 35-11-305 (1977 Republished
Edition and 1989 Cumm. Supp.);
(2) Water Quality Rules and Regula-
tions, Wyoming Department of Envi-
ronmental Quality, Chapter III: Regu-
lations for Permit to Construct, Install
or Modify Public Facilities Capable or,
(sic) Causing or Contributing to Pollu-
tion (certified copy, signed December
21, 1983);
(3) Water Quality Rules and Regula-
tions, Wyoming Department of Envi-
ronmental Quality, Chapter VIII: Qual-
ity Standards for Groundwaters of Wy-
oming (certified copy, signed April 9,
1980);
(4) Water Quality Rules and Regula-
tions, Wyoming Department of Envi-
ronmental Quality, Chapter IX: Wyo-
ming Groundwater Pollution Control
Permit (certified copy, signed April 9,
1980);
(5) Water Quality Rules and Regula-
tions, Wyoming Department of Envi-
ronmental Quality, Chapter XIII: Pro-
hibitions of Permits for New Hazardous
Waste Injection Wells (certified copy,
signed August 25, 1989);
(6) Land Quality Rules and Regula-
tions, Wyoming Department of Envi-
ronmental Quality, Chapter XXI: In
Situ Mining (effective March 26, 1981).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for select
sections identified in paragraph (a) of
this section, are also part of the ap-
proved State-administered program:
(1) Article 9, Underground Water, Wy-
oming Statutes sections 41-3-901
through 41-3-938 (September 1982);
(2) Wyoming Administrative Proce-
dure Act, Wyoming Statutes sections
9-4-101 through 9-4-115 (1988);
(3) Department of Environmental
Quality Rules of Practice and Proce-
dure (1982).
(c)(l) The Memorandum of Agree-
ment between EPA, Region VIII and
the Wyoming Department of Environ-
mental Quality, signed by the EPA Re-
gional Administrator on April 26, 1983.
(2) Letter from Regional Adminis-
trator, EPA Region VIII, to Governor
798
-------
Environmental Protection Agency
§147.2551
of Wyoming-, May 21, 1982, with Attach-
ment (regarding aquifer exemptions);
(3) Letter from Governor of Wyoming-
to Regional Administrator, EPA Re-
g-ion VIII, "Re: Underground Injection
Control (UIC) Program—Aquifer Ex-
emption Issues," June 7, 1982;
(4) Letter from Regional Adminis-
trator, EPA Region VIII to Governor of
Wyoming, "Re: Underground Injection
Control (UIC) Program—Aquifer Ex-
emption Issues," June 25, 1982;
(5) Letter from Director, Wyoming
Department of Environmental Quality,
to Acting Director, Water Management
Division, EPA Region VIII, December
1, 1982.
(d) Statement of legal authority. (1)
"Attorney General's Statement—Wyo-
ming Statutory and Regulatory Au-
thority for Assumption of the Under-
ground Injection Control Program Pur-
suant to the Federal Safe Drinking
Water Act," signed by Attorney Gen-
eral and Assistant Attorney General
for the State of Wyoming, September
22, 1982;
(2) Letter from Attorney General for
the State of Wyoming to Acting Re-
gional Counsel, EPA Region VIII, "Re:
Wyoming Assumption of the UIC Pro-
gram—$36, Chapter IX, Wyoming Water
Quality Rules and Regulations," No-
vember 24, 1982.
(e) The Program Description and any
other materials submitted as part of
the application or amendment thereto.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43092, Oct. 25, 1988; 56 FR 9421, Mar. 6,
1991]
§ 147.2551 State-administered pro-
gram—Class II wells.
The UIC program for Class II wells in
the State of Wyoming, except those on
Indian lands, is the program adminis-
tered by the Wyoming Oil and Gas Con-
servation Commission approved by
EPA pursuant to section 1425 of the
SDWA. Notice of this approval was
published in the FR on November 23,
1982 (47 FR 52434); the effective date of
this program is December 23, 1982. This
program consists of the following ele-
ments as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the State of Wyoming-. This incorpora-
tion by reference was approved by the
Director of the OFR in accordance with
5 U.S.C. 552(a) and 1 CFR Part 51. Cop-
ies may be obtained at the Wyoming
Oil and Gas Conservation Commission,
Office of the State Oil and Gas Super-
visor, P.O. Box 2640, 77 West First
Street, Casper, Wyoming, 82602. Copies
may be inspected at the Environmental
Protection Agency, Region VIII, 999
18th Street, Suite 500, Denver, Colo-
rado, 80202-2405, or at the National Ar-
chives and Records Administration
(NARA). For information on the avail-
ability of this material at NARA, call
202-741-6030, or go to: http://
www.archives.gov/federal register/
code of_federal regulations/
ibr locations.html.
(1) Rules and Regulations of the Wyo-
ming Oil and Gas Conservation Com-
mission, including Rules of Practice
and Procedure, as published by the Wy-
oming Oil and Gas Conservation Com-
mission, August 7, 1990;
(2) Title 30, Chapter 5, Wyoming Stat-
utes, sections 30-5-101 through 30-5-126
(June 1983 and Wyoming Statutes An-
notated, July 1990 Supp.).
(b) Memorandum of Agreement. (1) The
initial Memorandum of Agreement be-
tween EPA, Region VIII and Wyoming
Oil and Gas Conservation Commission,
signed by the EPA Regional Adminis-
trator and the Oil Field Supervisor of
the Commission on June 2, 1982;
(2) Amendment No. 1 to the Memo-
randum of Agreement, dated December
22, 1982;
(3) Amendment No. 2 to the Memo-
randum of Agreement, dated January
25, 1990;
(4) Letter from State Oil and Gas Su-
pervisor, Wyoming Oil and Gas Con-
servation Commission, to the Acting
Director, Water Management Division,
EPA Region VIII, "Re: Application for
Primacy in the Regulation of Class II
Injection Wells," March 8, 1982;
(5) Letter from State Oil and Gas Su-
pervisor, Wyoming Oil and Gas Con-
servation Commission, to EPA Region
VIII, "Re: Regulation of Liquid Hydro-
carbon Storage Wells Under the UIC
Program," July 1, 1982;
799
-------
§147.2553
40 CFR Ch. I (7-1-04 Edition)
(6) Memorandum of Agreement Be-
tween the Wyoming State Board of
Control, State Engineer, Oil and Gas
Conservation Commission, and the De-
partment of Environmental Quality,
dated October 14, 1981.
(c) Statement of legal authority. (1)
"Statement of Legal Authority" and
"State Review of Regulations and Stat-
utes Relevant to the UIC Program-
Class II Wells," signed by Special As-
sistant Attorney General for the State
of Wyoming, as submitted with "Wyo-
ming- Oil and Gas Conservation Com-
mission, Application for Primacy in
the Regulation of Class II Injection
Wells under Section 1425 of the Safe
Drinking Water Act," November 1981;
(2) Letter from special Assistant At-
torney General for the State of Wyo-
ming- to Assistant Regional Counsel,
EPA Region VIII, May 13, 1982;
(3) Letter from special Assistant At-
torney General for the State of Wyo-
ming to Assistant Regional Counsel,
EPA Region VIII, July 1, 1982.
(d) Program Description. The Program
Description and other material sub-
mitted as part of the application or
amendments thereto, including the
memorandum to the National UIC
Branch reporting on Improvement to
the Wyoming Oil and Gas 1425 program,
dated April 28, 1989.
[56 FR 9421, Mar. 6, 1991]
§ 147.2553 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
State of Wyoming is administered by
EPA. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and any additional re-
quirements set forth in the remainder
of this subpart. Injection well owners
and operators, and EPA shall comply
with these requirements.
(b) Effective date. The effective date
for the UIC program on Indian lands in
Wyoming is November 25, 1988.
[53 FR 43092, Oct. 25, 1988, as amended at 56
FR 9422, Mar. 6, 1991]
§ 147.2554 Aquifer exemptions.
In accordance with §§144.7(b) and
146.4 of this chapter, those portions of
aquifers currently being used for injec-
tion in connection with Class II (oil
and gas) injection operations on the
Wind River Reservation, which are de-
scribed below, are hereby exempted for
the purpose of Class II injection activ-
ity. This exemption applies only to the
aquifers tabulated below, and includes
those portions of the aquifers defined
on the surface by an outer boundary of
those quarter-quarter sections dis-
sected by a line drawn parallel to, but
one-quarter mile outside, the field
boundary, and is restricted to extend
no further than one-quarter mile out-
side the Reservation boundary. Maps
showing the exact boundaries of the
field may be consulted at the EPA's
Region 8 Office, and at the EPA Head-
quarters in Washington, DC.
AREAS To BE EXEMPTED FOR THE PURPOSE OF CLASS II INJECTION ON THE WIND RIVER
RESERVATION
Formation
Approximate
depth
Location
Steamboat Butte Field
Phosphoria
Tensleep
Winkleman Dome Field
Tensleep
6,500-7,100
6,900-7,500
2,800-3,300
Phosphoria
T3N, R1W—W/2 Sec. 4, Sec. 5, E/2 Sec. 6, NE/4
Sec. 8, W/2 Sec. 9.
T4N, R1W—W/2 Sec. 29, E/2 Sec. 30, E/2 Sec. 31,
Sec. 32.
T3N, R1W—W/2 Sec. 4, Sec. 5, E/2 Sec. 6, NE/4
Sec. 8, W/2 Sec. 9.
T4N, R1W—W/2 Sec. 29, E/2 Sec. 30, E/2 Sec. 31,
Sec. 32.
T2N, R1W—SW/4 Sec. 17, Sections 18, 19, 20, 29,
NE/4 Sec. 30.
T2N, R2W—E/2 Sec. 13, NE/4 Sec. 24.
T2N, R1W—SW/4 Sec. 17, Sections 18, 19, 20, 29,
NE/4 Sec. 30.
T2N, R2W—E/2 Sec. 13, NE/4 Sec. 24.
800
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Environmental Protection Agency
AREAS To BE EXEMPTED
§147.2555
FOR THE PURPOSE OF CLASS II INJECTION ON THE WIND RIVER
RESERVATION—Continued
Formation
Approximate
depth
Location
Nugget
Lander Field
Phosphoria
NW Sheldon Field
Crow Mountain and Cloverly
Circle Ridge Field
Tensleep
Phosphoria
Amsden
Rolff Lake Field
Crow Mountain
1,100-1,500
1,100-3,800
3,400-3,600
1,500-1,800
800-1,800
700-1,200
3,500-3,700
T2N, R1W—SW/4 Sec. 17, Sections 18, 19, 20, 29,
NE/4 Sec. 30.
T2N, R2W—E/2 Sec. 13, NE/4 Sec. 24.
T2S, R1E—Sections 12 and 13, E/2 Sec. 24, NE/4
Sec. 25.
T2S, R2E—W/2 Sec. 18, W/2 Sec. 19, Sec. 30.
T33N, R99W—Sec. 4.
T6N, R3W—SE/4 Sec. 35, SW/4 Sec. 36.
T5N, R3W—N/2Sec. 1.
T6N, R2W—Sec. 6, N/2 Sec. 7.
T7N, R3W—SE/4 Sec. 36.
T7N, R2W—SW/4 Sec. 31.
T6N, R3W— E/2 Sec. 1.
T7N, R3W—S/2 Sec. 36.
T6N, R3W—NE/4 Sec. 1.
T6N, R3W—Sec. 6.
T6N, R3W—SW/4 Sec. 26, NW/4 Sec. 27.
[53 FR 43092, Oct. 25, 1988]
§ 147.2555 Aquifer exemptions since
January 1, 1999.
In accordance with §144.7(b) and
§146.4 of this chapter, the aquifers de-
AQUIFER EXEMPTIONS SINCE JANUARY 1,1999
scribed in the following, table are here-
by exempted from the definition of an
underground source of drinking water,
as defined in 40 CFR 144.3:
Formation
Powder River Basin, only approximately 0.4
square miles of the Lance Formation which is
less than 0.005% of the Basin at indicated
depths and location..
Lance Formation at indicated depths and locations
Approximate depth (feet
below
ground surface)
3 800 — 6 800
3,800—6,500
Location
Two cylindrical volumes with centers in the wells
COGEMA DW No. 1 and 18-3 Christensen re-
spectively, and radius of 1 ,320 feet. Both wells
are located in the Christensen Ranch, in John-
son County, WY. The COGEMA DW No. 1
well is located at approximately 450 feet West
of N/S line and 100 feet North of E/W line of
SE/4, NW/4, Section 7, T44N, R76W. The 18-
3 Christensen well is located approximately
600 feet West of N/S line and 550 South of E/
W line of NE/4, NW/4, Section 18, T44N,
R76W.
Two cylindrical volumes with centers in the wells
COGEMA DW No. 2 and COGEMA DW No. 3
respectively, and radius of 1320 feet. Both
wells are located in the Christensen Ranch, in
Johnson County WY. The COGEMA DW No.
2 is located at approximately 2,290 feet from
the North line and 1130 feet from the East line
SW1/4 SE1/4 NE1/4 of Section 7, Township
44 North, Range 76 West. The COGEMA DW
No. 3 is located approximately 3300 feet from
the North line and 1340 feet from the West
line center of SW1/4 of Section 5, Township
44 North, Range 76 West.
[64 FR 14803, Mar. 26, 1999, as amended at 67 FR 47726, July 22, 2002]
801
-------
§147.2600
40 CFR Ch. I (7-1-04 Edition)
Subpart AAA—Guam
§ 147.2600 State-administered pro-
gram.
The UIC program for all classes of
wells in the territory of Guam, except
those on Indian lands, is the program
administered by the Guam Environ-
mental Protection Agency, approved
by EPA pursuant to SDWA section
1422. Notice of this approval was pub-
lished in the FEDERAL REGISTER on
May 2, 1983 (47 FR 19717); the effective
date of this program is June 1, 1983.
This program consists of the following
elements, as submitted to EPA in the
State's program application:
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the territory of Guam. This incorpora-
tion by reference was approved by the
Director of the Federal Register on
June 25, 1984.
(1) Water Resources Conservation
Act, Government Code of Guam sec-
tions 57021-57025, Public Law 9-31
(March 9, 1967), as amended by Public
Law 9-76 (July 29, 1967), as amended by
Public Law 12-191 (December 30, 1974);
(2) Water Pollution Control Act, Gov-
ernment Code of Guam sections 57042
and 57045, Public Law 9-76 (July 29,
1967), as amended by Public Law 9-212
(August 5, 1968), as amended by Public
Law 10-31 (March 10, 1969), as amended
by Public Law 12-191 (December 30,
1974);
(3) Guam Environmental Protection
Agency, Underground Injection Control
Regulations, Chapters 1-9, as revised
by amendments adopted September 24,
1982;
(4) Guam Environmental Protection
Agency, Water Quality Standards, Sec-
tion I-IV (approved September 25, 1981,
effective November 16, 1981).
(b) Other laws. The following statutes
and regulations, although not incor-
porated by reference except for specific
sections identified in paragraph (a) of
this section, are also part of the ap-
proved State-administered program:
(1) Government Code of Guam, Title
XXV, Chapters I-III (sections 24000-
24207);
(2) Government Code of Guam, Title
LXI, Chapters I-III (sections 57000-
57051);
(3) Government Code of Guam, Title
LXI, Chapters VI (sections 57120-57142);
(4) Government Code of Guam, Title
LXI, Chapters VIII (sections 57170-
57188);
(5) Government Code of Guam, Title
LXI, Chapters XII (sections 57285-
57299);
(c) The Memorandum of Agreement
between EPA, Region IX and the Guam
Environmental Protection Agency
signed by the Regional Administrator
on January 14, 1983.
(d) Statement of legal authority. (1)
Letter from Attorney General of Guam
to Regional Administrator, Region IX,
"Re: Attorney General's Statement for
Underground Injection Control Pro-
gram (UIC), Ground Water Program
Guidance #16" May 12, 1982;
(2) Letter from Attorney General of
Guam to Regional Administrator, Re-
gion IX, "Re: Additional comments to
be incorporated into the May 12, 1982,
Attorney General's Statement for Un-
derground Injection Control Program,"
September 2, 1982.
(e) The Program Description and any
other materials submitted as part of
the application or amendments there-
to.
[49 FR 20197, May 11, 1984, as amended at 53
FR 43092, Oct. 25, 1988]
§ 147.2601 EPA-administered pro-
gram—Indian lands.
(a) Contents. The UIC program for In-
dian lands in the territory of Guam is
administered by EPA. This program
consists of the UIC program require-
ments of 40 CFR parts 124, 144, 146, 148,
and any additional requirements set
forth in the remainder of this subpart.
Injection well owners and operators,
and EPA shall comply with these re-
quirements.
(b) Effective date. The effective date
for the UIC program on Indian lands in
the territory of Guam is November 25,
1988.
[53 FR 43093, Oct. 25, 1988, as amended at 56
FR 9422, Mar. 6, 1991]
802
-------
Environmental Protection Agency
§147.2701
Subpart BBB—Puerto Rico
§ 147.2650 State-administered pro-
gram—Class I, II, III, IV, and V
wells.
The Underground Injection Control
Program for all classes of wells in the
Commonwealth of Puerto Rico, other
than those on Indian lands, is the pro-
gram administered by Puerto Rico's
Environmental Quality Board (EQB),
approved by the EPA pursuant to the
Safe Drinking Water Act (SDWA) sec-
tion 1422. This program consists of the
following elements, as submitted to
EPA in the Commonwealth's program
application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this
paragraph are hereby incorporated by
reference and made a part of the appli-
cable UIC program under the SDWA for
the Commonwealth of Puerto Rico.
This incorporation by reference was ap-
proved by the Director of the Federal
Register in accordance with 5 U.S.C.
552(a) and 1 CFR part 51. Copies may be
obtained or inspected at the following
locations: EPA, Region II, 26 Federal
Plaza, room 845, New York, NY 10278;
EPA, Headquarters, 401 M St., SW.,
room E1101A, Washington, DC 20460; or
the National Archives and Records Ad-
ministration (NARA). For information
on the availability of this material at
NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal register/
code of_federal regulations/
ibr locations.html.
(1) Underground Injection Control
Regulations of the Commonwealth of
Puerto Rico, Parts I through V and ap-
pendices A and B, adopted September
14, 1983 (Amended July 20, 1988).
(2) Puerto Rico Public Policy Envi-
ronmental Act (PRPPE), Title 12 Laws
of Puerto Rico Annotated (LPRA)
Chapters 121 and 131, 1977 edition, as
amended 1988 edition, and Chapter 122,
1988 edition.
(b) Memorandum of Agreement. The
Memorandum of Agreement between
EPA Region II and the Commonwealth
of Puerto Rico's EQB signed by the Re-
gional Administrator on August 23,
1991.
(c) Statement of legal authority. (1)
Attorney General's statement on the
Commonwealth of Puerto Rico's Au-
thority to apply for, assume and carry
out the UIC Program, dated June 26,
1987. (2) Letter from the Governor of
the Commonwealth of Puerto Rico re-
questing the program, dated July 16,
1987.
(d) Program description. The Descrip-
tion of the Commonwealth of Puerto
Rico's Underground Injection Control
Program, dated with the effective date
October 30, 1986.
[57 FR 33446, July 29, 1992]
§ 147.2651 EPA-administered pro-
gram— Indian lands.
(a) Contents. The UIC program for all
classes of wells on Indian lands in the
Commonwealth of Puerto Rico is ad-
ministered by EPA. This program con-
sists of the UIC program requirements
of 40 CFR parts 124, 144, 146, 148 and any
additional requirements set forth in
the remainder of this subpart. Injec-
tion well owners and operators and
EPA shall comply with the require-
ments.
(b) Effective date. The effective date
for the UIC program on Indian Lands in
the Commonwealth of Puerto Rico is
November 25, 1988.
[57 FR 33446, July 29, 1992]
Subpart CCC—Virgin Islands
§ 147.2700 State-administered pro-
gram. [Reserved]
§ 147.2701 EPA-administered program.
(a) Contents. The UIC program for the
Virgin Islands, including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CFR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
of the UIC program for non-Indian
lands in the Virgin Islands is December
30, 1984. The effective date for Indian
lands in the Virgin Islands is November
25, 1988.
[53 FR 43093, Oct. 25, 1988, as amended at 56
FR 9422, Mar. 6, 1991]
803
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§147.2750
40 CFR Ch. I (7-1-04 Edition)
Subpart ODD—American Samoa
§ 147.2750 State-administered
gram. [Reserved]
pro-
§ 147.2751 EPA-administered program.
(a) Contents. The UIC program for
American Samoa, including all Indian
lands, is administered by EPA. This
program consists of the UIC program
requirements of 40 CFR parts 124, 144,
146, 148, and any additional require-
ments set forth in the remainder of
this subpart. Injection well owners and
operators, and EPA shall comply with
these requirements.
(b) Effective dates. The effective date
for the UIC program on non-Indian
lands is June 25, 1984. The effective
date of the UIC program on Indian
lands is November 25, 1988.
[53 FR 43093, Oct. 25, 1988, as amended at 56
FR 9422, Mar. 6, 1991]
§ 147.2752 Aquifer exemptions. [Re-
served]
Subpart EEE—Commonwealth of
the Northern Mariana Islands
§ 147.2800 State-administered pro-
gram—Class I, II, III, TV, and V
wells.
The UIC program for Class I, II, III,
IV, and V wells in the Commonwealth
of the Northern Mariana Islands, other
than those on Indian lands, is the pro-
gram administered by the Common-
wealth of the Northern Mariana Islands
Division of Environmental Quality ap-
proved by EPA pursuant to Section
1422 of the SDWA. Notice of this ap-
proval was published in the FEDERAL
REGISTER on January 18, 1985; the effec-
tive date of this program is August 30,
1985. This program consists of the fol-
lowing elements, as submitted to EPA
in the State's program application.
(a) Incorporation by reference. The re-
quirements set forth in the State stat-
utes and regulations cited in this para-
graph are hereby incorporated by ref-
erence and made a part of the applica-
ble UIC program under the SDWA for
the Commonwealth of the Northern
Mariana Islands. This incorporation by
reference was approved by the Director
of the Federal Register effective July
31, 1985.
(1) CNMI Environmental Protection
Act, 2 CMC sections 3101, et seq. (1984);
(2) CNMI Coastal Resources Manage-
ment Act, 2 CMC sections 1501, et seq.
(1984);
(3) CNMI Drinking Water Regula-
tions, Commonwealth Register, Vol-
ume 4, Number 4 (August 15, 1982);
(4) CNMI Underground Injection Con-
trol Regulations, Commonwealth Reg-
ister, Volume 6, Number 5 (May 15,
1984, amended November 15, 1984, Janu-
ary 15, 1985);
(5) CNMI Coastal Resources Manage-
ment Regulations, Commonwealth
Register, Volume 6, Number 12, Decem-
ber 17, 1984.
(b)(l) The Memorandum of Agree-
ment between EPA Region IX and the
Commonwealth of the Northern Mar-
iana Islands Division of Environmental
Quality, signed by the EPA Regional
Administrator on May 3, 1985;
(c) Statement of legal authority. State-
ment from Attorney General Common-
wealth of the Northern Mariana Is-
lands, "Underground Injection Control
Program—Attorney General's State-
ment," signed on October 10, 1984.
(d) The Program Description and any
other materials submitted as part of
the original application or as supple-
ments thereto.
[50 FR 28943, July 17, 1985]
§ 147.2801 EPA-administered program.
(a) Contents. The UIC program for In-
dian lands in the Commonwealth of the
Northern Mariana Islands is adminis-
tered by EPA. This program consists of
the UIC program requirements of 40
CFR parts 124, 144, 146, 148, and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements.
(b) Effective date. The effective date
of the UIC program for Indian lands is
November 25, 1988.
[53 FR 43093, Oct. 25, 1988, as amended at 56
FR 9422, Mar. 6, 1991]
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Environmental Protection Agency
§147.2902
§147.2802 Aquifer exemptions. [Re-
served]
Subpart FFF—Trust Territory of the
Pacific Islands
§ 147.2850 State-administered
gram. [Reserved]
pro-
§ 147.2851 EPA-administered program.
(a) Contents. The UIC program for
Trust Territory of the Pacific Islands,
including all Indian lands, is adminis-
tered by EPA. This program consists of
the UIC program requirements of 40
CFR parts 124, 144, 146, 148, and any ad-
ditional requirements set forth in the
remainder of this subpart. Injection
well owners and operators, and EPA
shall comply with these requirements.
(b) Effective dates. The effective date
of the UIC program for non-Indian
lands of the Trust Territory of the Pa-
cific Islands is June 25, 1984. The effec-
tive date for the Indian lands is No-
vember 25, 1988.
[53 PR 43093, Oct. 25, 1988, as amended at 56
PR 9422, Mar. 6, 1991]
§147.2852 Aquifer exemptions. [Re-
served]
Subpart GGG—Osage Mineral
Reserve—Class \\ Wells
AUTHORITY: Safe Drinking Water Act, 42
U.S.C. 300h.
SOURCE: 49 FR 45309, Nov. 15, 1984, unless
otherwise noted.
§ 147.2901 Applicability and scope.
This subpart sets forth the rules and
permitting requirements for the Osage
Mineral Reserve, Osage County, Okla-
homa, Underground Injection Control
Program. The regulations apply to
owners and operators of Class II injec-
tion wells located on the Reserve, and
to EPA.
§147.2902 Definitions.
Most of the following terms are de-
fined in §144.3, and have simply been
reproduced here for the convenience of
the reader. This section also includes
definitions of some terms unique to the
Osage program. Terms used in this sub-
part are defined as follows:
Administrator—the Administrator of
the United States Environmental Pro-
tection Agency, or an authorized rep-
resentative.
Aquifer—a geologic formation, group
of formations, or part of a formation
that is capable of yielding a significant
amount of water to a well or spring.
BIA—The "Bureau of Indian Affairs,"
United States Department of Interior.
Casing—a pipe or tubing of varying
diameter and weight, lowered into a
borehole during or after drilling in
order to support the sides of the hole
and, thus, prevent the walls from cav-
ing, to prevent loss of drilling mud into
porous ground, or to prevent water,
gas, or other fluid from entering the
hole.
Cementing—the operation whereby a
cement slurry is pumped into a drilled
hole and/or forced behind the casing.
Class II Wells—wells which inject
fluids:
(a) Which are brought to the surface
in connection with conventional oil or
natural gas production and may be
commingled with waste waters from
gas plants which are an integral part of
production operations, unless those wa-
ters would be classified as a hazardous
waste at the time of injection;
(b) For enhanced recovery of oil or
natural gas; and
(c) For storage of hydrocarbons
which are liquid at standard tempera-
ture and pressure.
Existing Class II Wells—wells that
were authorized by BIA and con-
structed and completed before the ef-
fective date of this program.
New Class II Wells—wells constructed
or converted after the effective date of
this program, or which are under con-
struction on the effective date of this
program.
Confining bed—a body of impermeable
or distinctly less permeable material
stratigraphically adjacent to one or
more aquifers.
Confining zone—a geologic formation,
group of formations, or part of a forma-
tion that is capable of limiting fluid
movement above an injection zone.
Contaminant—any physical, chemical,
biological, or radiological substance or
matter in water.
805
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§147.2903
40 CFR Ch. I (7-1-04 Edition)
Disposal well—a well used for the dis-
posal of waste into a subsurface stra-
tum.
EPA—The United States Environ-
mental Protection Agency.
Fault—a surface or zone of rock frac-
ture along which there has been dis-
placement.
Fluid—material or substance which
moves or flows whether in a semisolid,
liquid, sludge, gas or any other form or
state.
Formation—a body of rock character-
ized by a degree of lithologic homo-
geneity which is prevailingly, but not
necessarily, tabular and is mappable on
the earth's surface or traceable in the
subsurface.
Freshwater—"Underground source of
drinking water."
Ground water—water below the land
surface in a zone of saturation.
Injection well—a well into which
fluids are being injected.
Injection zone—a geological forma-
tion, group of formations, or part of a
formation receiving fluids through a
well.
Lithology—the description of rocks on
the basis of their physical and chem-
ical characteristics.
Owner/operator—the owner or oper-
ator of any facility or activity subject
to regulation under the Osage UIC
program.
Packer—a device lowered into a well
to produce a fluid-tight seal within the
casing.
Permit—an authorization issued by
EPA to implement UIC program re-
quirements. Permit does not include
the UIC authorization by rule or any
permit which has not yet been the sub-
ject of final Agency action.
Plugging—the act or process of stop-
ping the flow of water, oil or gas into
or out of a formation through a
borehole or well penetrating that for-
mation.
Pressure—the total load or force per
unit area acting on a surface.
Regional Administrator—the Regional
Administrator of Region 6 of the
United States Environmental Protec-
tion Agency, or an authorized rep-
resentative.
Subsidence— the lowering of the nat-
ural land surface in response to: Earth
movements; lowering of fluid pressure;
removal of underlying supporting ma-
terial by mining or solution solids, ei-
ther artificially or from natural
causes; compaction due to wetting
(hydrocompaction); oxidation of or-
ganic matter in soils; or added load on
the land surface.
Underground source of drinking
water— an aquifer or its portion:
(a)(l) Which supplies any public
water system; or
(2) Which contains a sufficient quan-
tity of ground water to supply a public
water system; and
(i) Currently supplies drinking water
for human consumption; or
(ii) Contains fewer than 10,000 mg/1
total dissolved solids; and
(b) Which is not an exempted aquifer.
USDW—underground source of drink-
ing water.
Well—a bored, drilled, or driven shaft,
or a dug hole whose depth is greater
than the largest surface dimension.
Well injection—the subsurfac emplace-
ment of fluids through a bored, drilled,
or driven well; or through a dug well,
where the depth of the dug well is
greater than the largest surface dimen-
sion.
Well workover—any reentry of an in-
jection well; including, but not limited
to, the pulling of tubular goods, ce-
menting or casing repairs; and exclud-
ing any routine maintenance (e.g. re-
seating the packer at the same depth,
or repairs to surface equipment).
§ 147.2903 Prohibition of unauthorized
injection.
(a) Any underground injection, ex-
cept as authorized by permit or rule
issued under the UIC program, is pro-
hibited. The construction or operation
of any well required to have a permit is
prohibited until the permit has been
issued.
(b) No owner or operator shall con-
struct, operate, maintain, convert,
plug, or abandon any injection well, or
conduct any other injection activity,
in a manner that allows the movement
of fluid containing any contaminant
into underground sources of drinking
water, if the presence of that contami-
nant may cause the violation of any
primary drinking water regulation
under 40 CFR part 142 or may otherwise
adversely affect the health of persons.
806
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Environmental Protection Agency
§147.2905
The applicant for a permit shall have
the burden of showing that the require-
ments of this paragraph are met.
(c) Injection between the outermost
casing protecting underground sources
of drinking water and the well bore is
prohibited.
§ 147.2904 Area of review.
(a) The area of review for an injec-
tion well or project will be a fixed ra-
dius of one-forth of a mile from the
well, field or project.
(b) The zone of endangering influence
is the lateral area around the injection
well or project in which the injection
zone pressures may cause movement of
fluid into an underground source of
drinking water (USDW) if there are im-
properly sealed, completed or aban-
doned wells present. A zone of endan-
gering influence may be determined by
EPA through the use of an appropriate
formula that addresses the relevant
geologic, hydrologic, engineering and
operational features of the well, field,
or project.
§ 147.2905 Plugging and abandonment.
The owner/operator shall notify the
Osage UIC office within 30 days of the
date injection has terminated. The well
must be plugged within 1 year after
termination of injection. The Regional
Administrator may extend the time to
plug, but only if no fluid movement
into a USDW will occur, and the oper-
ator has presented a viable plan for uti-
lizing the well within a reasonable
time.
(a) Until an injection well has been
properly plugged and abandoned, an-
nual reports to the Regional Adminis-
trator on well status, and mechanical
integrity tests as outlined in §§147.2912
and 147.2920 will be required, whether
or not injection has ceased.
(b) All wells shall be plugged to pre-
vent movement of fluid into an USDW.
(c) The owner/operator shall notify
the Osage UIC office by certified mail
at least 5 days prior to the commence-
ment of plugging operations. The Osage
UIC office may waive or reduce the 5-
day notice requirement when a quali-
fied EPA representative is available to
witness the plugging operation. The
following information must be sub-
mitted as part of the notification:
(1) Type and number of plugs to be
used;
(2) Elevation of top and bottom of
each plug;
(3) Method of plug placement; and
(4) Type, grade and quantity of ce-
ment to be used.
(d) The well shall be kept full of mud
as casing is removed. No surface casing
shall be removed without written ap-
proval from the Regional Adminis-
trator.
(e)(l) If surface casing is adequately
set and cemented through all fresh-
water zones (set to at least 50 feet
below the base of freshwater), a plug
shall be set at least 50 feet below the
shoe of the casing and extending at
least 50 feet above the shoe of the
casing, or
(2) If the surface casing and cement-
ing is inadequate, the well bore shall be
filled with cement from a point 50 feet
below the base of fresh water to a point
50 feet above the shoe of the surface
casing, and any additional plugs as re-
quired by the Osage UIC office and/or
the Osage Agency.
(3) In all cases, the top 20 feet of the
well bore below 3 feet of ground surface
shall be filled with cement. Surface
casing shall be cut off 3 feet below
ground surface and covered with a se-
cure steel cap on top of the surface
pipe. The remaining 3 feet shall be
filled with dirt.
(f)(l) Except as provided in paragraph
(f)(2) of this section, each producing or
receiving formation shall be sealed off
with a 50-foot cement plug placed at
the base of the formation and a 50-foot
cement plug placed at the top of the
formation.
(2) The requirement in paragraph
(f)(l) of this section does not apply if
the producing/receiving formation is
already sealed off from the well bore
with adequate casing and cementing
behind casing, and casing is not to be
removed, or the only openings from the
producing/receiving formation into the
well bore are perforations in the cas-
ing, and the annulus between the cas-
ing and the outer walls of the well is
filled with cement for a distance of 50
feet below the base of the formation
and 50 feet above the top of the forma-
tion. When such conditions exist, a
807
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§147.2906
40 CFR Ch. I (7-1-04 Edition)
bridge plug capped with 10 feet of ce-
ment set at the top of the producing
formation may be used.
(g) When specified by the Osage UIO
office, any uncased hole below the shoe
of any casing to be left in the well shall
be filled with cement to a depth of at
least 50 feet below the casing shoe, or
the "bottom of the hole, and the casing
above the shoe shall be filled with ce-
ment to at least 50 feet above the shoe
of the casing. If the well has a screen
or liner which is not to be removed, the
well bore shall be filled with cement
from the base of the screen or liner to
at least 50 feet above the top of the
screen or liner.
(h) All intervals between cement
plugs in the well bore shall be filled
with mud.
(i) A report containing copies of the
cementing tickets shall be submitted
to BIA within 10 days of plugging com-
pletion.
(j) A surety bond must be on file with
the Bureau of Indian Affairs (BIA), and
shall not be released until the well has
been properly plugged and the Regional
Administrator has agreed to the re-
lease of the bond.
§ 147.2906 Emergency permits.
(a) An emergency permit may be
issued if:
(1) There will he an imminent health
hazard unless an emergency permit is
issued; or
(2) There will be a substantial and ir-
retrievable loss of oil and gas re-
sources, timely application for a per-
mit could not practicably have been
made, and injection will not result in
movement of fluid into an USDW; or
(3) There will he a substantial delay
in oil or gas production, and injection
will not result in movement of fluid
into an USDW.
(b) Requirements—(1) Permit duration.
(i) Emergency permits issued to avoid
an imminent health threat may last no
longer than the time necessary to pre-
vent the hazard.
(ii) Emergency permits issued to pre-
vent a substantial and irretrievable
loss of oil or gas resources shall be for
no longer than 90 days, unless a com-
plete permit application has been sub-
mitted during that time; in which case
the emergency permit may be extended
until a final decision on the permit ap-
plication has been made.
(iii) Emergency permits to avoid a
substantial delay in oil or gas produc-
tion shall be issued only after a com-
plete permit application has been sub-
mitted and shall be effective until a
final decision on the permit applica-
tion is made.
(2) Notice of the emergency permit
will be given by the Regional Adminis-
trator according to the notice proce-
dure for a draft permit within 10 days
after issuance.
(3) An emergency permit may be oral
or written. If oral, a written emergency
permit must be issued within five cal-
endar days.
§147.2907 Confidentiality of informa-
tion.
(a) The following information cannot
be claimed confidential by the sub-
mitter:
(1) Name and address of permit appli-
cant or permittee.
(2) Information concerning the exist-
ence, absence or level of contaminants
in drinking water.
(b) Other information claimed as con-
fidential will be processed in accord-
ance with 40 CFR part 2.
§ 147.2906 Aquifer exemptions.
(a) After notice and opportunity for a
public hearing, the Administrator may
designate any aquifer or part of an aq-
uifer as an exempted aquifer.
(b) An aquifer or its portion that
meets the definition of a USDW may be
exempted by EPA from USDW status if
the following conditions are met:
(1) It does not currently serve as a
source of drinking water, and
(2) It cannot now and will not in the
future serve as a source of drinking
water because:
(i) It is hydrocarbon producing, or
can be demonstrated by a permit appli-
cant as a part of a permit application
for a Class II operation to contain hy-
drocarbons that are expected to be
commercially producible (based on his-
torical production or geologic informa-
tion); or
(ii) It is situated at a depth or loca-
tion which makes recovery of water for
drinking water purposes economically
or technologically impractical; or
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Environmental Protection Agency
(ill) It is so contaminated that it
would "be economically or techno-
logically impractical to render that
water fit for human consumption; or
(3) The Total Dissolved Solids con-
tent of the groundwater is more than
3,000 and less than 10,000 mg/1 and it is
not reasonably expected to supply a
public water system.
§147.2909 Authorization of existing
wells by rule.
All existing Class II injection wells
(wells authorized by BIA and con-
structed or completed on or before the
effective date of the Osage UIO pro-
gram) are hereby authorized. Owners or
operators of wells authorized by rule
must comply with the provisions of
§§147.2903, 147.2905, 147.2907, and 147.2910
through 147.2915.
§ 147.2910 Duration of authorization
by rule.
Existing Class II induction wells are
authorized for the life of the well, sub-
ject to the obligation to obtain a per-
mit if specifically required by the Re-
gional Administrator pursuant to
§147.2915.
§ 147.2911 Construction requirements
for wells authorized by rule.
All Class II wells shall be cased and
cemented to prevent movement of
fluids into USDWs. The Regional Ad-
ministrator shall review inventory in-
formation, data submitted in permit
applications, and other records, to de-
termine the adequacy of construction
(completion) or existing1 injection
wells. At the Regional Administrator's
discretion, well casing and cementing
may be considered adequate if it meets
the BIA requirements that were in ef-
fect at the time of construction (com-
pletion) and will not result in move-
ment of fluid into an USDW. If the Re-
gional Administrator determines that
the construction of a well authorized
by rule is inadequate, he shall require
a permit, or he shall notify the owner/
operator and the owner/operator shall
correct the problem according to in-
structions from the Regional Adminis-
trator. All corrections must be com-
pleted within one year of owner/oper-
ator notification of inadequacies.
§147.2912
§147,2912 Operating requirements for
wells authorized by rule.
(a) Bach well authorized by rule must
have mechanical integrity. Mechanical
integrity must be demonstrated within
five years of program adoption. The
Regional Administrator will notify the
well owner/operator three months be-
fore proof of mechanical integrity
must be submitted to EPA. The owner/
operator must contact the Osage UIC
office at least five days prior to test-
ing. The owner/operator may perform
the mechanical integrity test prior to
receiving notice from the Regional Ad-
ministrator, provided the Osage UIC of-
fice is notified at least five days in ad-
vance. Conditions of both paragraphs
(a)(l) and (a)(2) of this section must be
met,
(1) There is no significant leak in the
casing, tubing or packer. This may be
shown by the following:
(i) Performance of a pressure test of
the casing/tubing annulus to at least
200 psi, or the pressure specified by the
Regional Administrator, to be repeated
thereafter, at five year intervals, for
the life of the well (pressure tests con-
ducted during well operation shall
maintain an injection/annulus pressure
differential of at least 100 psi through
the tubing length); or
(ii) Maintaining a positive gauge
pressure on the casing/tubing annulus
(filled with liquid) and monitoring the
pressure monthly and reporting of the
pressure information annually; or
(iii) Radioactive tracer survey; or
(iv) For enhanced recovery wells,
records of monitoring showing the ab-
sence of significant changes in the re-
lationship between injection pressure
and injection flow rate at the well
head, following an initial pressure test
as described by paragraph (a)(l)(i) or
(v) of this section; or
(v) Testing or monitoring programs
approved by the Regional Adminis-
trator on a case-by-case basis, and
(2) There is no significant fluid move-
ment into a USDW through vertical
channels adjacent to the well bore.
This may be shown by any of the fol-
lowing;
(i) Cementing records (need not be re-
viewed every five years);
(ii) Tracer survey (in appropriate
hydrogeologic settings; must be used in
809
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§147.2913
40 CFR Ch. I (7-1-04 Edition)
conjunction with at least one of the
other alternatives);
(iii) Temperature log;
(iv) Noise log; or
(v) Other tests deemed acceptable by
the Regional Administrator.
(b) Injection pressure at the wellhead
shall be limited so that it does not ini-
tiate new fractures or propagate exist-
ing fractures in the confining zone ad-
jacent to any UDSW.
(1) For existing Class II salt water
disposal wells, The owner/operator
shall, except during well stimulation,
use an injection pressure at the well-
head no greater than the pressure cal-
culated by using the following formula:
Pm=(0.75-0.433Sg)d
where:
Pm=injection pressure at the wellhead in
pounds per square inch
Sg=specific gravity of injected fluid
(unitless)
d=injection depth in feet.
Owner/operator of wells shall comply
with the above injection pressure lim-
its no later than one year after the ef-
fective date of this regulation.
(2) For existing Class II enhanced re-
covery wells, the owner or operator:
(i) Shall use an injection pressure no
greater than trie pressure established
by the Regional Administrator for the
field or formation in which the well is
located. The Regional Administrator
shall establish such a maximum pres-
sure after notice, opportunity for com-
ment, and opportunity for a public
hearing according to the provisions of
part 124, subpart A of this chapter, and
will inform owners and operators in
writing of the applicable maximum
pressure.
(ii) Prior to such time as the Re-
gional Administrator establishes rules
for maximum injection pressures based
on data provided pursuant to para-
graph (b)(2)(ii)(B) of this section the
owner/operator shall:
(A) Limit injection pressure at the
wellhead to a value which will not ini-
tiate new fractures or propagate exist-
ing fractures in the confining zone ad-
jacent to any USDW; and
(B) Submit data acceptable to the
Regional Administrator which defines
the fracture pressure of the formation
in which injection is taking place. A
single test may be submitted on behalf
of two or more operators conducting
operations in the same formation, if
the Regional Administrator approves
such submission. The data shall be sub-
mitted to the Regional Administrator
within one year of the effective date of
this program.
(c) Injection wells or projects which
have exhibited failure to confine in-
jected fluids to the authorized injec-
tion zone or zones may be subject to re-
striction of injection volume and pres-
sure, or shut-down, until the failure
has been identified and corrected.
(The information collection requirements
contained in paragraphs (a)(l) (ii) through
(v) and (a)(2) (i) through (v) were approved by
the Office of Management and Budget under
control number 2040-0042)
§147.2913 Monitoring and reporting
requirements for wells authorized
by rule.
(a) The owner/operator has the duty
to submit inventory information to the
Regional Administrator upon request.
Such request may be a general request
to all operators in the County (e.g.,
public notice, or mailout requesting
verification of information).
(b) The operator shall monitor the in-
jection pressure (psi) and rate (bbl/day)
at least monthly, with the results re-
ported annually. The annual report
shall specify the types of methods used
to generate the monitoring data.
(c) The owner/operator shall notify
the Osage UIC office within 30 days of
any mechanical failure or down-hole
problems involving well integrity, well
workovers, or any noncompliance. As
required, operators must apply for and
obtain a workover permit from the Bu-
reau of Indian Affairs Osage Agency be-
fore reentering an injection well. If the
condition may endanger an USDW, the
owner/operator shall notify the Osage
UIC office orally within 24 hours, with
written notice including plans for test-
ing and/or repair to be submitted with-
in five days. If all the information is
not available within five days, a fol-
lowup report must be submitted within
30 days.
(d) The owner/operator shall deter-
mine the nature of injected fluids ini-
tially, when the nature of injected
810
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Environmental Protection Agency
§147.2918
fluids is changed or when new constitu-
ents are added. The records should re-
flect the source of character of the new
fluid and the date changes were made.
(e) The owner/operator shall retain
all monitoring records for three years,
unless an enforcement action is pend-
ing, and then until three years after
the enforcement action has been re-
solved.
(Approved by the Office of Management and
Budget under control number 2040-0042)
§147.2914 Corrective action for wells
authorized by rule.
Based on the Regional Administra-
tor's discretion, corrective action to
prevent movement of fluid into an
USDW may be required for improperly
sealed, completed or abandoned wells
(i.e., wells or well bores which may pro-
vide and avenue for fluid migration
into a USDW) within the zone of endan-
gering influence (as defined in
§147.2904, Area of Review) of an injec-
tion well authorized by rule.
(a) EPA will notify the operator
when corrective action is required. Cor-
rective action may include:
(1) Well modifications:
(i) Recementing;
(ii) Workover;
(ill) Reconditioning;
(iv) Plugging or replugging;
(2) Limitations on injection pressure
to prevent movement of fluid into an
USDW;
(3) A more stringent monitoring pro-
gram; and/or
(4) Periodic testing of other wells to
determine if significant movement of
fluid has occurred.
(b) If the monitoring discussed in
paragraph (a) (3) or (4) of this section
indicate the potential endangerment of
an USDW, then action as described in
paragraph (a) (1) or (2) of this section
must be taken.
§ 147.2915 Requiring a permit for wells
authorized by rule.
(a) The Regional Administrator may
require the owner or operator of any
well authorized by rule to apply for an
individual or area permit. The Re-
gional Administrator shall notify the
owner/operator in writing that a per-
mit application is required. The notice
shall contain:
(1) Explanation of need for applica-
tion;
(2) Application form and, if appro-
priate, a list of additional information
to be submitted; and
(3) Deadline for application submis-
sion.
(b) Cases in which the Regional Ad-
ministrator may require a permit in-
clude:
(I) The owner or operator is not in
compliance with provisions of the rule;
(2) Injection well is no longer within
the category of wells authorized by
rule;
(3) Protection of USDWs requires
that the injection operation be regu-
lated by requirements which are not
contained in the rule; or
(4) Discretion of Regional Adminis-
trator.
(c) Injection is no longer authorized
by rule upon the effective date of a per-
mit or permit denial, or upon failure of
the owner/operator to submit an appli-
cation in a timely manner as specified
in the notice described in paragraph (a)
of this section.
(d) Any owner/operator authorized by
rule may request to be excluded from
the coverage of the rules by applying
for an individual or area UIC permit,
§147.2916 Coverage of permitting re-
quirements.
The owner or operator of a new Class
II injection well or any other Class II
well required to have a permit in the
Osage Mineral Reserve shall comply
with the requirements of §§147.2903.
147.2907, 147.2918, through 147.2928.
§ 147.2917 Duration of permits.
Unless otherwise specified in the per-
mit, the permits will be in effect until
the well is plugged and abandoned or
the permit terminated. The Regional
Administrator will review each issued
permit at least once every five years to
determine whether it should be modi-
fied or terminated.
§ 147.2918 Permit application informa-
tion.
(a) The owner/operator must submit
the original and three copies of the per-
mit application, with two complete
sets of attachments, to the Osage UIC
office. The application should be signed
811
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§147.2919
40 CFR Ch. I (7-1-04 Edition)
by the owner/operator or a duly au-
thorized representative. The applica-
tion should also include appropriate
forms (i.e., BIA's Application for Oper-
ation or Report on Wells and EPA's
permit application). The applicant has
the burden of proof to show that the
proposed injection activities will not
endanger USDWs.
(b) The application shall include the
information listed below. Information
required by paragraphs (b) (5), (7), or (9)
of this section that is contained in
EPA or BIA files may be included in
the application by reference.
(1) Map using township-range sec-
tions showing the area of review and
identifying all wells of public record
penetrating the injection interval.
(2) Tabulation of data on the wells
identified in paragraph (b)(l) of this
section, including location, depth, date
drilled, and record of plugging and/or
completion.
(3) Operating data:
(i) Maximum and average injection
rate;
(ii) Maximum and average injection
pressure;
(iii) Whether operation is on cyclic or
continuous operation basis; and
(iv) Source and appropriate analysis
of injected fluids, including total dis-
solved solids, chlorides, and additives.
(4) Geologic data on the injection and
confining zones, including faults, geo-
logical name, thickness permeability,
depth and lithologic description.
(5) Depth to base of fresh water.
(6) Schematic drawings of the surface
and subsurface details of the well,
showing:
(i) Total depth or plug-back depth;
(ii) Depth to top and bottom of injec-
tion interval;
(iii) Depths to tops and bottoms of
casing and cemented intervals, and
amount of cement to be used;
(iv) Size of casing and tubing, and
depth of packer; and
(v) Hole diameter.
(7) Proof that surety bond has been
filed with the BIA Superintendent in
accordance with 25 CFR 226,6. A surety
bond must be maintained until the well
has been properly plugged.
(8) Verification of public notice, con-
sisting of a list showing the names, ad-
dresses, and date that notice of permit
application was given or sent to:
(i) The surface land owner;
(ii) Tenants on land where injection
well is located or proposed to be lo-
cated; and
(iii) Each operator of a producing
lease within one-half mile of the well
location.
(9) All available logging and testing
data on the well (for existing wells, i.e.,
wells to be converted or wells pre-
viously authorized by rule).
(Approved by the Office of Management and
Budget under control number 2040-0042)
§ 147.2919 Construction requirements
for wells authorized by permit.
(a) All Class II wells shall be sited so
that they inject into a formation that
is separated from any TJSDW by a con-
fining zone free of known open faults or
fractures within the area of review.
(b) All Class II wells shall be cased
and cemented to prevent movement of
fluids into or between USDWs. Require-
ments shall be based on the depth to
base of fresh water, and the depth to
the injection zone. Newly drilled Class
II wells must have surface casing set
and cemented to at least 50 feet below
the base of fresh water, or the equiva-
lent (e.g., long string cemented to sur-
face). At the Regional Administrator's
discretion, the casing and cementing of
wells to be converted may be consid-
ered adequate if they meet the BIA re-
quirements that were in effect at the
time of construction (completion), and
will not result in movement of fluid
into a USDW.
(c) Owner/operators shall provide a
standard female fitting with cut-off
valves, connected to the tubing and the
tubing/casing annulus so that the in-
jection pressure and annulus pressure
may be measured by an EPA represent-
ative by attaching a gauge having a
standard male fitting.
(d) No owner or operator may begin
construction of a new well until a per-
mit authorizing such construction has
been issued, unless such construction is
otherwise authorized by an area per-
mit.
812
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Environmental Protection Agency
§147.2921
§ 147.2920 Operating requirements
wells authorized by permit.
for
(a) For new Class II wells, injection
shall be through adequate tubing and
packer. Packer shall be run on the tub-
ing and set inside the casing within 75
feet of the top of the injection interval.
For existing Class II, wells, injection
shall be through adequate tubing and
packer, or according to alternative op-
erating requirements approved by the
Regional Administrator, as necessary
to prevent the movement of fluid into
a USDW.
(b) Each well must have mechanical
integrity. Mechanical integrity of the
injection well must be shown prior to
operation. The owner/operator must
notify the Osage UIC office at least five
days prior to mechanical integrity
testing. Conditions of both paragraphs
(b) (1) and (2) of this section must be
met.
(1) There is no significant leak in the
casing, tubing or packer. This may be
shown by the following:
(i) Performance of a pressure test of
the casing/tubing annulus to at least
200 psi, or the pressure specified by the
Regional Administrator, to be repeated
thereafter, at five year intervals, for
the life of the well (Pressure tests con-
ducted during well operation shall
maintain an injection/annulus pressure
differential of at least 100 psi through-
out the tubing length); or
(ii) Maintaining a positive gauge
pressure on the casing/tubing annulus
(filled with liquid) and monitoring the
pressure monthly and reporting of the
pressure information annually; or
(iii) Radioactive tracer survey; or
(iv) For enhanced recovery wells,
record of monitoring showing the ab-
sence of significant changes in the re-
lationship between injection pressure
and injection flow rate at the wellhead,
following an initial pressure test as de-
scribed by paragraph (b)(l) (i) or (v) of
this section; or
(v) Testing or monitoring programs
approved by the Administrator on a
case-by-case basis, and
(2) There is no significant fluid move-
ment into a USDW through vertical
channels adjacent to the well bore.
This may be shown by any of the fol-
lowing:
(i) Cementing records (need not be re-
viewed every five years);
(ii) Tracer survey (in appropriate
hydrogelogic settings; must be used in
conjunction with at least one of the
other alternatives);
(iii) Temperature log;
(iv) Noise log; or
(v) Other tests deemed acceptable by
the Administrator.
(c) Injection pressure at the wellhead
shall be limited so that it does not ini-
tiate new fractures or propagate exist-
ing fractures in the confining zone ad-
jacent to any UDSW.
(d) Injection wells or projects which
have exhibited failure to confine in-
jected fluids to the authorized injec-
tion zone or zones may be subject to re-
striction of injected volume and pres-
sure or shut-in, until the failure has
been identified and corrected.
(e) Operation shall not commence
until proof has been submitted to the
Regional Administrator, or an EPA
representative has witnessed that any
corrective action specified in the per-
mit has been completed.
§ 147.2921 Schedule of compliance.
The permit may, when appropriate.
specify a schedule of compliance lead-
ing to compliance with the Safe Drink-
ing Water Act and the Osage UIC regu-
lations.
(a) Any schedule of compliance shall
require compliance as soon as possible.
and in no case later than three years
after the effective date of the permit.
(b) If a permit establishes a schedule
of compliance which exceeds one year
from the date of permit issuance, the
schedule shall set forth interim re-
quirements and the dates for their
achievement.
(1) The time between interim dates
shall not exceed one year.
(2) If the time necessary for comple-
tion of any interim requirement is
more than 1 year and is not readily di-
visible into stages for completion, the
permit shall specify interim dates for
the submission of reports of progress
toward completion of the interim re-
quirements and indicate a projected
completion date.
(c) The permit shall be written to re-
quire that if a schedule of compliance
813
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§147.2922
40 CFR Ch. I (7-1-04 Edition)
is applicable, progress reports be sub-
mitted no later than 30 days following
each interim date and the final date of
compliance.
§147.2922 Monitoring and reporting
requirements for wells authorized
by permit.
(a) The owner/operator shall notify
the Osage UIC office within 30 days of
the date on which injection com-
menced.
(b) The operator shall monitor the in-
jection pressure (psi) and rate (bbl/day)
at least monthly, with the results re-
ported annually. The annual reports
shall specify the types or methods used
to generate the monitoring data.
(c) The owner/operator shall notify
the Osage UIC office within 30 days of
any mechanical failure or down-hole
problems involving well integrity, well
workovers, or any noncompliance. (Op-
erators should note the obligation to
apply for and obtain a workover permit
from, the Bureau of Indian Affairs
Osage Agency before reentering an in-
jection well.) If the condition may en-
danger an USDW, the owner/operator
shall notify the Osage UIC officer
orally within 24 hours, with written no-
tice including plans for testing and/or
repair to be submitted within five days.
If all the information is not available
within five days, a followup report
must be submitted within 30 days.
(d) The owner/operator shall retain
all monitoring records for three years,
unless an enforcement action is pend-
ing, and then until three years after
the enforcement action has been re-
solved.
(e) The owner/operator shall notify
the Osage UIC office in writing of a
transfer of ownership at least 10 days
prior to such transfer.
(Approved by the Office of Management and
Budget under control number 2040-0042)
§147.2923 Corrective action for wells
authorized by permit.
All improperly sealed, completed or
abandoned wells (i.e., wells or well
bores which may provide an avenue for
movement of fluid into an UDSW)
within the zone of endangering influ-
ence (as defined in §147.2904, Area of
Beview) that penetrate the injection
zone of a Class II well, must have cor-
rective action taken to prevent move-
ment of fluid into a USDW.
(a) EPA will review completion and
plugging records of wells within the
zone of endangering influence that pen-
etrate the injection zone and will no-
tify the operator when corrective ac-
tion is required. Corrective action may
include:
(1) Well modifications, including:
(i) Becementing;
(ii) Workover;
(iii) Beconditioning; and/or
(iv) Plugging or replugging;
(2) Permit conditions to limit injec-
tion pressure so as to prevent move-
ment of fluid into a USDW;
(3) A more stringent monitoring pro-
gram; and/or
(4) Periodic testing of other wells
within the area of review to determine
if significant movement of fluid has oc-
curred. If the monitoring discussed in
paragraph (a)(3) or (a)(4) of this section
indicates the potential endangerment
of a USDW, then action as described in
paragraph (a)(l) or (a)(2) of this section
must be taken.
(b) If the Begional Administrator has
demonstrable knowledge that wells
within the zone of endangering influ-
ence will not serve as conduits for fluid
movement into a USDW, the permit
may be approved without requiring
corrective action. However, additional
monitoring shall be required to con-
firm that no significant migration will
occur.
§ 147.2924 Area permits.
(a) Area permits may be issued for
more than one injection well if the fol-
lowing conditions are met:
(1) All existing wells are described
and located in the permit application;
(2) All wells are within the same well
field, project, reservoir or similar unit;
(3) All wells are of similar construc-
tion; and
(4) All wells are operated by the same
owner/operator.
(b) Area permits shall specify:
(1) The area within which injection is
authorized; and
(2) The requirements for construc-
tion, monitoring, reporting, operation
and abandonment for all wells author-
ized by the permit.
814
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Environmental Protection Agency
§147.2925
(c) Area permits can authorize the
construction and operation of new
wells within the permit area, if:
(1) The permittee notifies the Re-
gional Administrator in the annual re-
port of when and where any new wells
have or will be drilled;
(2) The new wells meet the criteria
outlined in paragraphs (a) and (b) of
this section; and
(3) The effects of the new wells were
addressed in the permit application and
approved by the Regional Adminis-
trator.
§ 147.2925 Standard permit conditions.
(a) The permittee must comply with
all permit conditions, except as author-
ized by an emergency permit (described
in §147.2906). Noncompliance is grounds
for permit modification, permit termi-
nation or enforcement action.
(b) The permittee has a duty to halt
or reduce activity in order to maintain
compliance with permit conditions.
(c) The permittee shall take all rea-
sonable steps to mitigate any adverse
environmental impact resulting from
noncompliance.
(d) The permittee shall properly op-
erate and maintain all facilities in-
stalled or used to meet permit condi-
tions. Proper operation and mainte-
nance also includes adequate operator
staffing and training, adequate fund-
ing, and adequate engineering capa-
bility available.
(e) This permit may be modified or
terminated for cause (see §§147.2927 and
147.2928). The filing of a request by the
permittee for a permit modification or
termination, or a notification of
planned changes or anticipated non-
compliance, does not stay any permit
condition.
(f) This permit does not convey any
property rights, or any exclusive
privilege.
(g) The permittee shall furnish, with-
in a reasonable time, information that
the Regional Administrator requests,
for determination of permit compli-
ance, or if cause exists, for permit
modification or termination.
(h) The permittee shall allow EPA
representatives, upon presentation of
appropriate credentials or other docu-
mentation, to:
(1) Enter permittee's premises where
a regulated activity is conducted or lo-
cated, or where records required by
this permit are kept;
(2) Have access to and copy records
required by this permit;
(3) Inspect any facilities, equipment,
practices or operations regulated or re-
quired by this permit; and
(4) Sample or monitor any substances
or parameters at any location for pur-
pose of assuring compliance with this
permit or the SDWA.
(i) Monitoring and records.
(1) Samples and monitoring data
shall be representative of injection
activity.
(2) Permittee shall retain monitoring
records for three years.
(3) Monitoring records shall include:
(i) Date, exact place and time of sam-
pling or measurement;
(ii) Individual(s) who preformed the
measurements;
(iii) Date(s) analyses were performed;
(iv) Individual(s) who performed the
analyses;
(v) Analytical techniques or methods
used, including quality assurance tech-
niques employed to insure the genera-
tion of reliable data; and
(vi) Results of analyses.
(j) Signatory requirements. All applica-
tions, reports or information submitted
to the Regional Administrator or the
Osage UIC office must be signed by the
injection facility owner/operator or his
duly authorized representative. The
person signing these documents must
make the following certification:
"I certify under penalty of law that I have
personally examined and am familiar with
the information submitted in this document
and all attachments and that, based on my
inquiry of those individuals immediately re-
sponsible for obtaining the information, I be-
lieve that the information is true, accurate,
and complete. I am aware that there are sig-
nificant penalties for submitting false infor-
mation, including the possibility of fine and
imprisonment."
(k) Reporting requirements. (1) The
permittee shall notify the Regional Ad-
ministrator as soon as possible of any
planned changes to the facility.
(2) The permittee shall give advance
notice to the Regional Administrator
of any planned changes which may re-
sult in noncompliance.
815
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§147.2926
40 CFR Ch. I (7-1-04 Edition)
(3) This permit is not transferable to
any person except after notice to the
Regional Administrator in accordance
with §147.2926.
(1) A new injection well shall not
commence injection until construction
is complete and the Regional Adminis-
trator has been notified of completion
of construction and has given his ap-
proval to commence injection.
(The information collection requirements
contained in paragraphs (g) and (i) were ap-
proved by the Office of Management and
Budget under control number 2040-0042)
§ 147.2926 Permit transfers.
(a) Permits may be transferred to an-
other permittee:
(1) If the current permittee notifies
the Regional Administrator at least 10
days before the proposed transfer date;
and
(2) If the notice includes a written
agreement between the existing and
new permittees containing:
(i) A specific date for transfer of per-
mit responsibility, coverage and liabil-
ity; and
(ii) Assurance that the new permittee
has a surety bond on file with BIA; and
(3) If the Regional Administrator
does not respond with a notice to the
existing permittee that the permit will
be modified.
(b) If the conditions in paragraph (a)
of this section are met, the transfer is
effective on the date specified in para-
graph (a)(2)(i) of this section.
§ 147.2927 Permit modification.
(a) Permits may be modified for the
following causes only (with the excep-
tions listed in paragraph (b) of this sec-
tion regarding minor modifications):
(1) There are substantial changes to
the facility or activity which occurred
after permit issuance that justify re-
vised or additional permit conditions.
(2) The Regional Administrator has
received information (e.g., from moni-
toring reports, inspections) which war-
rants a modified permit.
(3) The regulations or standards on
which the permit was based have
changed.
(4) The Regional Administrator has
received notice of a proposed permit
transfer.
(5) An interested person requests in
writing that a permit be modified, and
the Regional Administrator determines
that cause for modification exists.
(6) Cause exists for termination
under §147.2928, but the Regional Ad-
ministrator determines that permit
modification is appropriate.
(b) Minor modifications. (1) Minor
modifications do not require that the
procedures listed in paragraph (c) of
this section be followed.
(2) Minor modifications consist of:
(i) Correcting typographical errors;
(ii) Requiring more frequent moni-
toring or reporting;
(iii) Changing ownership or oper-
ational control (see §147.2926, Permit
Transfers); or
(iv) Changing quantities or types of
injected fluids, provided:
(A) The facility can operate within
conditions of permit;
(B) The facility classification would
not change.
(c) Modification procedures. (1) A draft
permit shall be prepared with proposed
modifications.
(2) The draft permit shall follow the
general permitting procedures (i.e.,
public comment period, etc.) before a
final decision is made.
(3) Only the changed conditions shall
be addressed in the draft permit or pub-
lic review.
§ 147.2928 Permit termination.
(a) Permits may be terminated for
the following causes only:
(1) Noncompliance with any permit
condition.
(2) Misrepresentation or failure to
fully disclose any relevant facts.
(3) Determination that the permitted
activity endangers human health or
the environment.
(4) Interested person requests in writ-
ing that a permit be terminated and
the Regional Administrator determines
that request is valid.
(b) Termination procedures. (1) The Re-
gional Administrator shall issue notice
of intent to terminate (which is a type
of draft permit).
(2) Notice of intent to terminate
shall follow the general permitting
procedures (i.e., public comment pe-
riod, etc.) before a final decision is
made.
816
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Environmental Protection Agency
§147.2929
§ 147.2929 Administrative permitting
procedures.
(a) Completeness review. (1) The Re-
gional Administrator shall review each
permit application for completeness
with the application requirements in
§ 147.2918. The review will be completed
in 10 days, and the Regional Adminis-
trator shall notify the applicant
whether or not the application is com-
plete.
(2) If the application is incomplete.
the Regional Administrator shall:
(i) List the additional information
needed;
(ii) Specify a date by which the infor-
mation must be submitted; and
(ill) Notify the applicant when the
application is complete.
(3) After an application is determined
complete, the Regional Administrator
may request additional information to
clarify previously submitted informa-
tion. The application will still be con-
sidered complete.
(4) If an applicant fails or refuses to
correct deficiencies in the application,
the permit may be denied and appro-
priate enforcement actions taken.
(b) Draft permits. (1) After an applica-
tion is deemed complete, the Regional
Administrator shall either prepare a
draft permit or notice of intent to deny
the permit (which is a type of draft
permit). If the Regional Administrator
later decides the tentative decision to
deny was wrong, he shall withdraw the
notice of intent to deny and prepare a
draft permit.
(2) A draft permit shall contain at
least the following information:
(i) The standard permit conditions in
§147.2925;
(ii) Any monitoring and reporting re-
quirements;
(ill) The construction and operation
requirements; and
(iv) Plugging and abandonment re-
quirements.
(c) Statement of basis. (1) The Regional
Administrator shall prepaf? a state-
ment of basis for every draft permit.
(2) The statement of basis shall brief-
ly describe the draft permit conditions
and the reasons for them. In the case of
a notice of intent to deny or terminate,
the statement of basis shall give rea-
sons to support the tentative decision.
(3) The statement of basis shall be
sent to the applicant, and to any other
person who requests a copy,
(d) Public notice. (l)(i) The Regional
Administrator shall give public notice
when:
(A) A permit application has been
tentatively denied;
(B) A draft permit has been prepared;
(C) A hearing has been scheduled; or
(D) An appeal has been granted.
(ii) The applicant shall give public
notice that he is submitting a permit
application.
(iii) Public notice is not required
when a request for permit modification
or termination is denied. However,
written notice will be given to the per-
mittee and the requester.
(iv) Public notices may include more
than one permit or action,
(2)(i) Public notice of a draft permit
(including notice of intent to deny)
shall allow at least 15 days for public
comment.
(ii) Public notice of a hearing shall
be given at least 30 days before the
hearing.
(3)(i) Public notice given by the Re-
gional Administrator for the reasons
listed in paragraph (d)(l)(i) of this sec-
tion shall be mailed to the applicant,
and published in a daily or weekly
paper of general circulation in the af-
fected area.
(ii) Notice of application submission
required by paragraph (d)(l)(ii) of this
section shall be given to the surface
landowner, tenants on the land where
an injection well is located or is pro-
posed to be located, and to each oper-
ator of a producing lease within one-
half mile of the well location prior to
submitting the application to the Re-
gional Administrator.
(4) The notice of application submis-
sion in paragraphs (d)(l)(ii) and
(d)(3)(ii) of this section shall contain:
(i) The applicant's name and address;
(ii) The legal location of the injec-
tion well;
(iii) Nature of activity;
(iv) A si^tement that EPA will be
preparing a draft permit and that there
will be an opportunity for public com-
ment; and '.}
(v) The name and phone number of
EPA contact person.
(5) All other notices shall contain:
817
-------
§147.2929
40 CFR Ch. I (7-1-04 Edition)
(i) The name, address, and phone
number of the Osage UIC office and
contact person for additional informa-
tion and copies of the draft permit;
(ii) Name and address of permit ap-
plicant or permittee;
(iii) Brief description of nature of ac-
tivity;
(iv) Brief description of comment pe-
riod and comment procedures;
(v) Location of the information avail-
able for public review; and
(vi) In the case of a notice for a hear-
ing the notice shall also include;
(A) Date, time, and location of hear-
ing;
(B) Reference to date of previous no-
tices of the same permit; and
(C) Brief description of the purpose of
the hearing, including rules and proce-
dures.
(e) Public comments. (1) During the
public comment period, any person
may submit written comments on the
draft permit, and may request a public
hearing. A request for hearing shall be
in writing and state the issues pro-
posed to be raised in the hearing.
(2) The Regional Administrator shall
consider all comments when making
the final decision, and shall respond to
comments after the decision is made.
The response shall:
(i) Specify if any changes were made
from the draft permit to the final per-
mit decision, and why;
(ii) Briefly describe and respond to
all significant comments on the draft
permit made during the comment pe-
riod, or hearing, if held; and
(iii) Be made available to the public.
(f) Public hearings. (1) The Regional
Administrator shall hold a public hear-
ing whenever he finds a significant
amount of public interest in a draft
permit, based on the requests sub-
mitted, or at his discretion.
(2) Any person may submit oral or
written statements and data con-
cerning the draft permit. The public
comment period shall be automatically
extended to the close of any public
hearing held, or may be extended by
the hearing officer at the hearing.
(3) A tape recording or written tran-
script of the hearing shall be made
available to the public.
(g) Reopening of the comment period.
(1) If any of the information submitted
during the public comment period
raises substantial new questions about
a permit, the Regional Administrator
may:
(i) Prepare a new draft permit;
(ii) Prepare a revised statement of
basis; or
(iii) Reopen the comment period.
(2) Comments submitted during a re-
opened comment period shall be lim-
ited to the substantial new questions
that caused its reopening.
(3) Public notice about any of the
above actions shall be given and shall
define the scope of the new questions
raised.
(h) Issuance and effective date of a per-
mit. (1) After the close of the comment
period on a draft permit, the Regional
Administrator shall make a final per-
mit decision. The Regional Adminis-
trator shall notify the applicant and
each person who commented or re-
quested to receive notice. The notice
shall include reference to the proce-
dures for appealing a permit decision.
(2) A final permit decision shall be-
come effective 30 days after giving no-
tice of the decision unless:
(i) A later date is specified in the
notice;
(ii) Review is requested under
§147,2929(j); or
(iii) No comments requested a change
in the draft permit, in which case the
permit is effective immediately upon
issuance.
(i) Stays of contested permit conditions.
If a request for review of a final UIC
permit §147,2929(j) is granted, the effect
of the contested permit conditions
shall be stayed and shall not be subject
to judicial review pending final agency
action. If the permit involves a new in-
jection well or project, the applicant
shall be without a permit for the pro-
posed well pending final agency action.
Uncontested provisions which are not
severable from those contested provi-
sions shall be stayed with the con-
tested provisions.
(j) Appeal of permits. (1) Any person
who filed comments on the draft per-
mit or participated in the public hear-
ing may petition the Administrator to
review any condition of the permit de-
cision. Any person who failed to file
comments or participate in the hearing
may petition for administrative review
818
-------
Environmental Protection Agency
§147.3000
only to the extent of the changes from
the preliminary permit to the final
permit decision.
(2) A person may request review of a
final permit decision within 30 days
after a final permit decision has "been
issued. The 30-day period within which
a person may request review begins
with the service of notice of the Re-
gional Administrator's final permit de-
cision unless a later date is specified in
that notice.
(3) The petition requesting review
shall include:
(i) A demonstration that the petition
is eligible under the requirements of
paragraph (j)(l) of this section; and,
when appropriate,
(il) A showing that the condition in
question is based on:
(A) A finding of fact or conclusion of
law that is clearly erroneous; or
(B) An exercise of discretion or im-
portant policy consideration which the
Administrator, in his discretion,
should review.
(4) The Administrator may also de-
cide, on his initiative, to review any
condition of any UIC permit issued
under these requirements. The Admin-
istrator must act under this paragraph
within 30 days of the date notice was
given of the Regional Administrator's
action.
(5) Within a reasonable time fol-
lowing the filing of the petition for re-
view, the Administrator shall issue an
order either granting or denying the
request. To the extent that review is
denied, the conditions of the final per-
mit decision become final agency ac-
tion.
(6) Public notice shall be given by the
Regional Administrator of any grant of
a review petition by the Administrator.
Notice shall be sent to the applicant,
the person requesting the review, ap-
propriate persons on the Osage County
mailing list and to newspapers of gen-
eral circulation in the county. Included
in the notice shall be a briefing sched-
ule for the appeal and a statement that
any interested person may file an ami-
cus brief. Notice of denial of the review
petition will be sent only to the per-
son(s) requesting the review.
(7) A petition to the Administrator,
under paragraphs (j) (1) and (2) of this
section is a prerequisite to the seeking
of judicial review of the final agency
action. For purposes of judicial review,
final agency action occurs when a final
UIC permit is issued or denied by the
Regional Administrator and agency re-
view procedures are exhausted. A final
permit decision shall be issued by the
Regional Administrator:
(i) When the Administrator issues no-
tice to the parties involved that review
has been denied;
(ii) When the Administrator issues a
decision on the merits of the appeal
and the decision does not include a re-
mand of the proceedings; or
(iii) Upon the completion of the re-
mand proceedings if the proceedings
are remanded, unless the Administra-
tor's remand order specifically pro-
vides that the appeal of the remand de-
cision will be required to exhaust the
administrative remedies.
Subpart HHH—Lands of the Nav-
ajo, Ute Mountain lite, and All
Other New Mexico Tribes
SOURCE: 53 PR 43104, Oct. 25, 1988, unless
otherwise noted.
i 147,3000 EPA-administered program.
(a) Contents, The UIC program for the
Indian lands of the Navajo, the Ute
Mountain Ute (Class II wells only on
Ute Mountain Ute lands in Colorado
and all wells on Ute Mountain Ute
lands in Utah and New Mexico), and all
wells on other Indian lands in New
Mexico is administered by EPA. (The
term "Indian lands" is defined at 40
CFR 144.3.) The Navajo Indian lands are
in the States of Arizona, New Mexico,
and Utah; and the Ute Mountain Ute
lands are in Colorado, New Mexico and
Utah. This program consists of the UIC
program requirements of 40 CFR parts
124, 144, 146, 148, and additional require-
ments set forth in the remainder of
this subpart. The additions and modi-
fications of this subpart apply only to
the Indian lands described above.
Injection well owners and operators,
and EPA shall comply with these re-
quirements.
819
-------
§147.3001
40 CFR Ch. I (7-1-04 Edition)
(b) Effective date. The effective date
for the UIC program on these lands is
November 25, 1988.
[53 FB 43104, Oct. 25, 1988, as amended at 56
PR 9422, Mar. 6, 1991]
1147.3001 Definition.
Area of review. For the purposes of
this subpart, area of review means the
area surrounding an injection well or
project area described according to the
criteria set forth in §147.3009 of this
subpart.
§147.3002 Public notice of permit ac-
tions.
An applicant shall give public notice
of his intention to apply for a permit
as follows:
(a) Prior to submitting' an applica-
tion to the Director, the applicant
shall give notice to each landowner,
tenant, and operator of a producing
lease within one-half mile of the well
and to the affected Tribal Government.
The notice shall include:
(1) Name and address of applicant;
(2) A brief description of the planned
injection activities including well loca-
tion, name and depth of the injection
zone, maximum injection pressure and
volume, and source and description of
the fluid to be injected;
(3) Name, address, and phone number
of the EPA contact person; and
(4) A statement that opportunity to
comment will be announced to the pub-
lic after EPA prepares a draft permit.
(b) In addition to the requirements of
§144.31(e) of this chapter, a permit ap-
plicant shall submit a description of
the way the notice was given and the
names and addresses of those to whom
it was given.
(c) Upon written request and sup-
porting documentation, the Director
may waive the requirement in para-
graph (a) of this section to give indi-
vidual notice of intent to apply for per-
mits in an area where it would be im-
practical. However, notice to the af-
fected Tribal government shall not be
waived.
(d) The Director shall also provide to
the affected Tribal government all no-
tices given to State governments under
|124,10(c) of this chapter.
§ 147.8003 Aquifer exemptions.
(a) Aquifer exemptions in connection
with Class II wells. In accordance with
§144.7(b) and §146.4 of this chapter, the
portions of authorized injection zones
into which existing Class II wells are
currently injecting which are described
in appendix A are hereby exempted.
The exempted aquifers are defined by a
one-quarter mile radius from the exist-
ing injection well. The exemption in-
cludes the intended injection zone only
and is solely for the purpose of Class II
injection.
(b) Class HI wells. In addition to the
requirements of §144.7(c)(l) of this
chapter, an applicant for a uranium
mining permit which necessitates an
aquifer exemption shall submit a plug-
ging and abandonment plan containing
an aquifer cleanup plan, acceptable to
the Director, describing the methods or
techniques that will be used to meet
the standards of §147.3011. The cleanup
plan shall include an analysis of pre-in-
jection water quality for the constitu-
ents required by the Director. The Di-
rector shall consider the cleanup plan
in addition to the other information re-
quired for permit applications under
§§ 144.31(e) and 146.34 of this chapter.
§ 147.3004 Duration of rule authoriza-
tion for existing Class I and in
wells.
Notwithstanding §144.21(a)(3)(i)(B) of
this chapter, authorization by rule for
existing Class I and HI wells will expire
90 days after the effective date of this
UIC program unless a complete permit
application has been submitted to the
Director.
§ 147.3005 Radioactive waste injection
wells.
Notwithstanding §§ 144.24 and 146.51(b)
of this chapter, owners and operators
of wells used to dispose of radioactive
waste (as defined in 10 CFR part 20, ap-
pendix B, table II, but not including
high level and transuranic waste and
spent nuclear fuel covered by 40 CFR
part 191) shall comply with the permit-
ting requirements pertaining to Class I
wells in parts 124, 144 and 146 of this
chapter, as modified and supplemented
by this subpart.
820
-------
Environmental Protection Agency
§147.3009
8147,3006 Injection pressure for exist-
ing Class II wells authorized by
rule,
(a) Rule-authorized Class II saltwater
disposal wells. In addition to the re-
quirements of § 144.28(f)(3)(il) of this
chapter, the owner or operator shall,
except during well stimulation, use an
injection pressure measured at the
wellhead that is not greater than the
pressure calculated by using the fol-
lowing formula:
Pm=0.2d
where;
Pm=injection pressure at the wellhead in
pounds per square inch
d=depth In feet to the top of the injection
zone.
Owners and operators shall comply
with this requirement no later than
one year after the effective date of this
program,
(b) Rule-authorised Class II enhanced
recovery and hydrocarbon storage wells.
(1) In addition to the requirements of
§ 144.28(f)(3)(ii) of this chapter, owners
and operators shall use an injection
pressure no greater than the pressure
established by the Director for the field
or formation in which the well is lo-
cated. The Director shall establish
such maximum pressure after notice
(including notice to the affected Tribe),
opportunity for comment, and oppor-
tunity for public hearing according to
the provisions of part 124, subpart A, of
this chapter, and shall inform owners
and operators and the affected Tribe in
writing of the applicable maximum
pressure; or
(2) An owner or operator may inject
at a pressure greater than that speci-
fied in paragraph (b)(l) of this section
for the field or formation in which he is
operating after demonstrating in writ-
ing to the satisfaction of the Director
that such injection pressure will not
violate the requirements of
§144.28(f)(3)(ii) of this chapter. The Di-
rector may grant such a request after
notice (including notice to the affected
Tribe), opportunity for comment and
opportunity for a public hearing ac-
cording to the provisions of part 124,
subpart A of this chapter,
(3) Prior to the time that the Direc-
tor establishes rules for maximum in-
jection pressure under paragraph (b)(l)
of this section the owner or operator
shall:
(i) Limit injection pressure to a
value which will not exceed the oper-
ating requirements of § 144.28(f)(3)(ii);
and
(ii) Submit data acceptable to the Di-
rector which defines the fracture pres-
sure of the formation in which injec-
tion is taking place, A single submis-
sion may be made on behalf of two or
more operators conducting operations
in the same field and formation, if the
Director approves. The data shall be
submitted to tlie Director within one
year of the effective date of this pro-
gram.
§ 147.3007 Application for a permit,
(a) Notwithstanding the require-
ments of §144.31(c)(l) of this chapter,
the owner or operator of an existing
Class I or III well shall submit a com-
plete permit application no later than
90 days after the effective date of the
program.
(b) The topographic map (or other
map if a topographic map is unavail-
able) required by §144.31(e)(7) of this
chapter, shall extend two miles from
Class II wells, and ZVz miles from Class
I and III wells. These maps will show
all the information listed in paragraph
144,31(e)(7) within ¥2 mile for Class II
wells and 2M> miles for Class I and III
wells.
§147.3008 Criteria for aquifer exemp-
tions.
The aquifer exemption criterion in
§146.4(c) of this chapter shall not be
available for this program.
§ 147.3009 Area of review.
The area of review shall be defined as
follows:
(a) Class // wells. The area of review
for Class II permits and area permits
shall be defined by a fixed radius as de-
scribed in §146.6(b) (1) and (2) of this
chapter except that the radius shall be
one-half mile.
(b) Class I and III wells. The area of
review for Class I and III wells are well
fields which may be either:
(1) An area defined by a radius two
and one-half miles from the well or
well field; or
821
-------
§147.3010
40 CFR Ch. I (7-1-04 Edition)
(2) An area one-quarter mile from the
well or well field where the well field
production at the times exceeds injec-
tion to produce a net withdrawal; or
(3) A suitable distance, not less than
one-quarter mile, proposed by the
owner or operator and approved by the
Director based upon a mathematical
calculation such as that found in
§146.6(a)(2) of this chapter.
§ 147.3010 Mechanical integrity tests.
The monitoring of annulus pressure
listed in § 146.8(b)(l) of this chapter will
only be acceptable if preceded by a
pressure test, using liquid or gas that
clearly demonstrates that mechanical
integrity exists at the time of the pres-
sure test.
§ 147.3011 Plugging and abandonment
of Class III wells.
To meet the requirements of
§146.10(d) of this chapter, owners and
operators of Class III uranium projects
underlying or in aquifers containing up
to 5,000 mg/1 TDS which have been ex-
empted under §146.4 of this chapter
shall:
(a) Include in the required plugging
and abandonment plan a plan for aqui-
fer clean-up and monitoring which
demonstrates adequate protection of
surrounding USDWs.
(1) The Director shall include in each
such permit for a Class III uranium
project the concentrations of contami-
nants to which aquifers must be
cleaned up in order to protect sur-
rounding USDWs.
(2) The concentrations will be set as
close as is feasible to the original con-
ditions.
(b) When requesting permission to
plug a well, owners and operators shall
submit for the Director's approval a
schedule for the proposed aquifer
cleanup, in addition to the information
required by §146.34(c).
(c) Cleanup and monitoring shall be
continued until the owner or operator
certifies that no constituent listed in
the permit exceeds the concentrations
required by the permit, and the Direc-
tor notifies the permittee in writing
that cleanup activity may be termi-
nated.
§ 147.3012 Construction
for Class I wells.
requirements
In addition to the cementing require-
ment of §146.12(b) of this chapter, own-
ers and operators of Class I wells shall,
through circulation, cement all casing
to the surface.
§ 147.3013 Information to be consid-
ered for Class I wells.
(a) In addition to the information
listed in §146.14(a) of this chapter, the
Director shall consider the following
prior to issuing any Class I permit:
(1) Expected pressure changes, native
fluid displacement, and direction of
movement of the injected fluid; and
(2) Methods to be used for sampling,
and for measurement and calculation
of How.
(b) In addition to the information
listed in §146.14(b) of this chapter, the
Director shall consider any informa-
tion required under §146.14(a) of this
chapter (as supplemented by this sub-
part) that has been gathered during
construction.
§ 147.3014 Construction
for Class III wells.
requirements
(a) In addition to the requirements of
§146.32(c)(3) of this chapter, radio-
logical characteristics of the formation
fluids shall be provided to the Director.
(b) In addition to the requirements of
§146.32(e) of this chapter, the Director
may require monitoring wells to be
completed into USDWs below the injec-
tion zone if those USDWs may be af-
fected by mining operations.
§ 147.3015 Information to be consid-
ered for Class III wells.
(a) In addition to the requirements of
§ 146.34(a) of this chapter, the following
information shall be considered by the
Director:
(1) Proposed construction procedures,
including a cementing and casing pro-
gram, logging procedures, deviation
checks, and a drilling, testing and cor-
ing program.
(2) Depth to the proposed injection
zone, and a chemical, physical and ra-
diological analysis of the ground water
in the proposed injection zone suffi-
cient to define pre-injection water
quality as required for aquifer cleanup
by §147.3011 of this subpart.
822
-------
Environmental Protection Agency
(3) An aquifer cleanup plan if re-
quired by §147.3003(b) of this subpart.
(4) Any additional information that
may be necessary to demonstrate that
cleanup will reduce the level of con-
taminants in the surrounding USDWs
as close as feasible to the original con-
ditions,
(b) In addition to the requirements of
§146.34(b) of this chapter, the Director
shall consider any information re-
quired under §146,34(a) of this chapter
(as supplemented by this subpart) that
has been gathered during construction.
Pt. 147, Subpt. HHH, App. A
§147.3016 Criteria and standards ap-
plicable to Class V wells.
In addition to the criteria and stand-
ards applicable to Class V wells set
forth in subpart P of part 146 of this
chapter, owners and operators of wells
that do not fall within the Class IV
category but that are used to dispose of
radioactive wastes (as defined in 10
CFR part 20, appendix B, table II. col-
umn 2, but not including high level and
transuranic wastes and spent nuclear
fuel covered by 40 CPR part 191) shall
comply with all of the requirements
applicable to Class I injection wells in
40 CFR parts 124, 144 and 146 as supple-
mented by this subpart.
APPENDIX A TO SUBPART HHH OF PART 147—EXEMPTED AQUIFERS IN NEW MEXICO
The areas described by a one-quarter mile radius around the following Class II wells in the
listed formations are exempted for the purpose of Class II injection.
Sec.
Well
Mo.
Arco Oil & Gas Co.—Operator/Horseshoe Gallup—Field/Gallup—Formation
SE/NE 5
NW/NW 30
SE/SW 28
NW/SE 33
SE/NW 35
NW/NW 4
NW/SW 33
NW/SE 27
SEISE 30
NW/NW 34
NW/NE 34
NW/NE 2
NW/NW 29
NW/SW 13
NW/SE 29
SE/SW 27
NW/SW 35
SE/NW 30
NW/NE 31
NW/NE 4
NW/NE 29
SE/NE 34
SE/SE 31
NE/SW 14
NE/NW 14
SE/NW 10
SE/SE 29
SE/NE 30
SE/NW 29
NW/SE 25
SE/SW 32
NW/SW 30
SE/SW 13
NW/NW 27
SEISE 28
NW/SW 29
SE/NW 34
SONW 29
NW/SW 27
NE/SE 23
NW/SW 24
T30N
T31N
T31N
T31N
T31N
T30N
T31N
T31N
T31N
T31N
T31N
T30N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T30N
T31N
T31N
T31N
T31N
T31N
T30N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
T31N
R16W
H16W
R16W
R16W
R16W
R18W
R18W
R16W
R16W
R16W
R16W
R16W
R16W
R17W
R16W
R16W
R16W
R16W
R16W
R16W
R16W
R16W
R16W
R17W
R17W
R16W
R16W
R16W
R16W
R17W
R16W
R16W
R17W
R16W
R18W
H16W
R16W
H16W
R16W
R17W
R17W
1650'FNL
660'FNL
790'FSL
1710'FSL
2105'FNL
455'FNL
1980'FSL
1980'FSL
660'FSL
730'FNL
813'FNL
720'FNL
660'FNL
1975'FSL
1980'FSL
660'FSL
1980'FSL
1980'FNL
660'FNL
330'FNL
660'FNL
1990'FNL
640'FSL
2250'FSL
625'FNL
1900'FNL
560'FSL
1980'FNL
2080'FNL
1980'FSL
660'FSL
2021'FSL
660'FSL
520'FNL
660'FSL
1980'FSL
2310'FNL
660'FSL
1650'FSL
1BSOTSL
2050'FSL
330'FEL
703'FWL
2150'FWL
2310'FEL
2105'FWL
4435'FEL
386'FWL
2080'FEL
660'FEL
515'FWL
2036'FEL
2040'FEL
660'FWL
670'FWL
1980'FEL
1980'FWL
660'FWL
2061'FWL
1980'FEL
2160'FEL
1980'FEL
645'FEL
660'FEL
2630'FWL
199S'FWi,
2080'FWL
660'FEL
1980'FWL
1980'FEL
1980'FWL
742'FWL
1980'FWL
660'FWL
660'FEL
660'FWL
1650'FWL
1980'FWL
330'FWL
340'FEL
990'FWL
134
8
167
199
196
219
65
164
5
180
182
229
24
77
22
171
205
7
17
221
26
194
27
94
69
271
21
10
23
122
14
19
82
150
169
11
192
12
162
96
97
823
203-160 D-27
-------
M. 147, Subpt. HHH, App. A
40 CFR Ch. I (7-1-04 Edition)
Sec.
Well
No,
SE/NW 4 T30N R16W 2060'FNL 1710'FWL 232
NW/NW 31 T31N R16W 620TNL 701'FWL 30
NW/SE 35 T31N R16W 1980'FSL 1980'FEL 207
SE/NE , , 32 T31N R16W 1980'FNL 417'FEL 20
NE/NW 28 T31N R16W 1980'FNL 1980'FEL 15Z
NE/NW 34 T31N R16W 2140'FSL 735'FWL 201
SE/NW 3 T30N R16W 2310'FNL 1640'FWL 236
SE/SW 34 T31N R16W 660'FSL 1980'FWL 213
NW/NE 30 T31N R16W 660'FNL 1980'FFL 9
SE/SW 26 T31N R16W 660'FSL 1980'FWL 175
NW/SE 30 T31N R16W 1980'FSL 1980'FEL 6
SE/NW 9 T30N R16W 1650'FNL 2131'FWL 284
NW/SW 4 T30N R16W 2310'FSL 4390'FEL 242
NW/SW 2 T30N R16W 1980'FSL 660'FWL 250
NW/NW 33 T31N R16W 660'FNL 386'FWL 66
NE/NE 15 T31N R17W 660'FNL 660'FEL 67
NW/NE 33 T31N R16W 660'FNL 1980'FEL 178
NW/SE 24 T31N R17W 1875'FSL 1900'FEL 99
NW/NE 28 T31N R16W 660'FNL 1980'FEL 148
NW/NW 19 T31N R16W 680'FNL 682'FWL 89
NW/SE 4 T30N R16W 1820'FSL 2130'FEL 244
SE/SW 20 T31N R16W 660'FSL 1980'FWL 115
NW/NE , 25 T31N R17W 660'FNL 1980'FEL 118
SE/SW 4 T30N R16W 660'FSL 3300'FEL 253
NW/SW 19 T31N R16W 1980'FSL 706'FWL 101
NW/SE 32 T31N R16W ISSOTSL 1980'FEL 22
NW/NW 35 T31N R16W 605'FNL 690'FWL 184
SE/NE 29 T31N R16W 1980'FNL 417'FEL 25
SE/NW 19 T31N R16W 1980'FNL 2023'FWL 95
NW/NW 32 T31N R16W 660'FNL 660'FWL 4
SE/SW 24 T31N R17W 660'FSL 3300'FEL 107
SEINE 28 T31N R16W 2105'FNL 940'FEL 154
NW/NE 35 T31N R16W 610'FNL 2000'FEL 186
SE/SW 5 T31N R16W 990TSL 2310TWL 138
NW/SE 28 T31N R16W 1980'FSL 1980'FEL 160
SE/SE 33 T31N R16W 330'FSL 990'FEL 211
NW/NE 5 T30N R16W 330'FNL 1650'FEL 128
SE/NW 27 T31N R16W 1900'FNL 2050'FWL 156
SE/SW 35 T31N R16W 660'FSL 1980'FWL 217
NW/NW 10 T30N H16W 526'FNL 330'FWL 26S
NE/SW 21 T31N R16W 1880TSL 1980'FWL 143
NW/NE 24 T31N R17W 409'FNL 1914'FEL 87
NW/SW 32 T31N R16W 1980'FSL 660'FWL 15
SE/SE 34 T31N R16W 960'FSL 91CCFEL 215
SW/SE 21 T31N R16W 820'FSL 1820'FEL 145
SE/SE 27 T31N R16W 610'FSL 640'FEL 173
NW/SW 3 T30N R16W 1920'FSL 350'FWL 246
SE/SW 19 T31N R16W 601'FSL 2002'FWL 111
SW/SE 14 T31N R17W 330'FSL 1900'FEL 79
NW/NW 27 T31N R16W 520'FNL 660'FWL 150
SE/NW 31 T31N R16W 1724'FNL 2067'FWL 29
NW/NE 32 T31N R16W 660'FNL 1980'FEL 13
SE/NE 24 T31N R17W 1998'FNL 702TEL 93
NW/NW 5 T30N R16W 660'FNL 660'FWL 126
NW/SW 28 T31N R16W 1740'FSL 590'FWL 158
SE/NE 31 T31N H16W 1980'FNL 660'FEL 16
NW/NW , 24 T31N R17W 660'FNL 760TWL 85
Energy Reserve Backup Inc.—Operator/Horseshoe Gallup—Field/Gallup—Formation
SeSE 5 T31N R17W 660'FSL 660'FEL 4
NE/SW 10 T30N R16W 1970'FSL 2210'FWL 31
SE/NW 11 T30N R16W 2090'FNL 2190'FWI 29
SE/SE 10 T30N R16W 700'FSL 500'FEL 37
Solar Petroelum Inc.—Operator/Horseshoe—Field/Gallup—Formation
SW/SE 11 T31N R17W 736'FSL 2045'FEL 205
SE/NE 9 T31N R17W 1980'FNL 660'FEL 122
NW/SE 4 T31N R17W 1980'FSL 1980'FFL 127
NE/NE 10 T31N R17W 660'FNL 660'FEL 136
SE/SW 4 T31N R17W 660'FSL 1980'FWL 125
SW/NW 11 T31N R17W 2300'FNL 660'FWL 206
824
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Environmental Protection Agency
Pt. 147, Subpt. HHH, App. A
NW'SW
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SW/NW
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SW/SE
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NW/NE
SE/NE ,
NW/SW
SE/NE
NW/NW
SE/SE
SE/NE
SE/NW
NW/SE
NE/NE
SE/SW
Sec.
4 T31N R17W 1980'FSL
, 4 T31N R17W 1989'FNL
4 T31N R17W 660'FNL
10 T31N R17W 1980'FNL
10 T31N R17W 1980'FNL
10 T31N R17W 660'FSL
3 T31N R17W 330'FSL
5 T31N R17W 1980'FNL
5 T31N R17W 1980'FNL
9 T31N R17W 990'FSL
10 T31N R17W 660'FNL
11 T31N R17W 660TSL
9 T31N R17W 1980'FSL
10 T31N R17W 990'FSL
9 T31N R17W 660'FNL
10 T31N R17W 1980'FSL
11 T31N H17W 1980'FSL
9 T31N R17W 1980'FNL
3 T31N R17W 1980'FSL
3 T31N R17W 560'FSL
9 T31N H16W 660'FNL
4 T31N R17W 660'FSL
WTR Oil Co. — Operator/Horseshoe Gallup — Field/Gallup — Formation
33 T32N R17W 1980'FSL
Arco Oil & Gas Co. — Operator/Many Rocks Gallup — Field/Gallup — Formation
7 T31N R16W 898'FNL
17 T31N R16W 1673'FNL
17 T31N H16W 1890'FSL
7 T31N R16W 2310'FNL
B T31N R16W 1650'FSL
17 T31N R16W 660'FNL
18 T31N R16W 360'FNL
7 T31N R16W 716'FSL
17 T31N R16W 660'FSL
17 T31N R16W 2040TSL
6 T31N R16W 330'FSL
17 T31N R16W 2073'FNL
.. 17 T31N R16W 1967'FSL
James P. Woosley — Operator/Many Rocks Gallup — Field/Gallup — Formation
20 T32N R17W 330'FNL
27 T32N R17W 660'FSL
17 T32N R17W 2310'FWL
. 27 T32N R17W 260'FWL
, . , . 27 T32N R17W 1980'FSL
18 T32N R17W 2474'FSL
27 T32N H17W 625'FNL
28 T32N H17W 1980'FSL
Solar Petroleum Inc. — Operator/Many Rocks Gallup — Field/Gallup — Formation
1 T31N R17W 1980'FNL
2 T31N R17W 805'FNL
2 T31N R17W 1980'FNL
1 T31N R17W 2310TSL
12 T31N B17W 1820'FNL
WTR Oil Co. — Operator/Many Rocks Gallup — Field/Gallup — Formation
35 T32N R17W 810'FNL
35 T32N R17W 660'FSL
34 T32N R17W 775'FEL
35 T32N R16W 1980'FNL
35 T32N R17W 1980'FSL
Chaco Oil Co.—Operatof/Red Mtn Meseyerde— Field/Menefee — Formation
29 T20N R9W 395'FNL
20 T20N R9W 442'FSL
660'FWL
1980'FWL
660'FWL
1980'FEL
660'FWL
660'FWL
2310'FEL
660'FEL
1050'FEL
850'FEL
1980'FWL
660'FWL
1980'FEL
1980'FEL
1980'FEL
1980'FWL
1980'FWL
1980'FWL
660'FWL
660'FWL
660'FWL
660'FEL
1989'FWL
500'FWL
1789'FEL
2150'FEL
2310'FEL
1 650'FWL
2030'FWL
855'FEL
2185'FWL
660'FEL
2070'FWL
330'FWL
641'FWL
981'FWL
2310'FEL
990'FWL
330'FWL
1 360'FNL
1980'FWL
133'FEL
2000'FEL
330'FEL
1980'FWL
940'FEL
660'FEL
990'FNL
500'FEL
510'FWL
660'FEL
1980'FNL
1980'FWL
1980'FEL
1265'FEL
2430'FWL
Well
No.
103
128
101
117
108
114
143
302
307
140
118
204
115
144
123
109
203
134
132
110
133
124
2
2
21
23
6
12
18
16
13
26
22
1
19
8
13
1
4
11
6
18
3
12
216
215
218
223
217
11
6
8
9
7
6
17
825
-------
§147.3100
40 CFR Ch. i (7-1-04 Edition)
Sec.
Well
No.
Geo Engineering Inc.—Operator/Red Mtn Meseverde—Fieid/Menefee—Formation
NW/NE
NE/NE
SE/NW
NW/NE
NE/NW
SW/SE
NE/NE
SE/SE
SE/SE
NW/NE
SE/SE
29
29
29
29
29
20
29
20
20
29
20
T20N
T20N
T20N
T20N
T20N
T20N
T20N
T20N
T20N
T20N
T20N
R9W
R9W
R9W
R9W
R9W
R9W
R9W
R9W
R9W
R9W
R9W
160'FNL
225'FNL
1344'FNL
615'FNL
834'FNL
265'FSL
5'FNL
4SOTSL
990'FSL
1115'FNL
106STSL
2135'FEL
1265'FEL
2555'FWL
1920'FEL
2113'FWL
2150'FEL
1130'FEL
1145'FEL
1280'FEL
2325'FEL
8WFEL
35
7
20
5
21
36
8
24
10
22
12
Tesoro Petroleum Co.—Qperator/S. Hospah Lower Sand—Fleld/Hospah—Formation
NW/SE
SW/SE
SW/SW
SE/SW
6
6
6
6
T17N R8W
T17N R8W
T17N R8W
T17N R8W
2310'FSL
990'FSL
5'FSL
5'FSL
2310TEL
2310'FFL
20'FWL
2635'FWL
28
34
18
20
Subpart 111—Lands of Certain
Oklahoma Indian Tribes
SOURCE: 53 PR 43109, Oct. 25, 1988, unless
otherwise noted.
§ 147.3100 EPA-administered program.
(a) Contents. The UIC program for the
Indian lands In Oklahoma, except for
that covering the Class II wells of the
Five Civilized Tribes, is administered
by EPA. The UIC program for all wells
on Indian lands in Oklahoma, except
Class II wells on the Osage Mineral Re-
serve (found at 40 CFR part 147, Sub-
part GGG) and the Class II program for
the Five Civilized Tribes, consists of
the UIC program requirements of 40
CFR parts 124, 144, 146, 148, and addi-
tional requirements set forth in the re-
mainder of this subpart. Injection well
owners and operators, and EPA shall
comply with these requirements.
(b) Effective date. The effective date
for the UIC program for all wells on In-
dian lands except Class n wells on the
Osage Mineral Reserve and Class II
wells on the lands of the Five Civilized
Tribes is November 25,1988.
[53 FR 43109, Oct. 25, 1988, AS amended at 56
FR 9422, Mar. 6, 1991]
§ 147.3101
tions.
Public notice of permit ac-
(a) In addition to the notice require-
ments of §124.10 of this chapter, the Di-
rector shall provide to the affected
Tribal government all notices given to
an affected State government under
§124.10(c) of this chapter.
(b) Class 1 and III wells. In addition to
the notice requirements of §124.10 of
this chapter:
(1) Owners and operators of Class I
and III wells shall notify the affected
Tribal government prior to submitting
an application for a permit, shall pub-
lish such notice in at least two news-
papers of general circulation in the
area of the proposed well, and shall
broadcast notice over at least one local
radio station.
(2) The Director shall publish a no-
tice of availability of a draft permit in
at least two newspapers of general cir-
culation in the area of the proposed
well, and broadcast notice over at least
one local radio station. The public no-
tice shall allow at least 45 days for pub-
lic comment.
(c) Class // wells. In addition to the
notice requirements of §124.10 of this
chapter:
(1) Owners and operators of Class II
wells shall give notice of application
for a permit to the affected Tribal gov-
ernment prior to submitting the appli-
cation to the Director.
(2) In addition to the public notice re-
quired for each action listed in
§124.10(a) of this chapter, the Director
shall also publish notice in a daily or
weekly newspaper of general circula-
tion in the affected area for actions
concerning Class II wells.
826
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Environmental Protection Agency
§147.3107
§147.3102 Plugging and abandonment
plans.
In lieu of the requirements of
§144,28(c)(l) and (2) (i)-(iii) of this chap-
ter, owners and operators of Class II
wells shall comply with the plugging
and abandonment provisions of
§ 147.3108 of this subpart.
§147.3108 Fluid seals.
Notwithstanding §§ 144.28(f)(2) and
146.12(c) of this chapter, owners and op-
erators shall not use a fluid seal as an
alternative to a packer.
§ 147.3104 Notice of abandonment.
(a) In addition to the notice required
by §144J8(j)(2) of this chapter, the
owner or operator shall at the same
time submit plugging information in
conformance with §147.3108 of this sub-
part including:
(1) Type and number of plugs;
(2) Elevation of top and bottom of
each plug;
(3) Method of plug placement; and
(4) Type, grade and quantity of ce-
ment to be used.
(b) In addition to the permit condi-
tions specified in §§144.51 and 144.52 of
this chapter, each owner and operator
shall submit and each permit shall con-
tain the following information (in con-
formance with §146.3108 of this sub-
part):
(1) Type and number of plugs;
(2) Elevation of top and bottom of
each plug;
(3) Method of plug placement; and
(4) Type, grade and quantity of ce-
ment to be used.
§147.3105 Plugging and abandonment
report,
(a) In lieu of the time periods for sub-
mitting a plugging report in §144.28(k)
of this chapter, owners and operators
of Class I and III wells shall submit the
report within 15 days of plugging the
well and owners or operators of Class II
wells within 30 days of plugging, or at
the time of the next required oper-
ational report (whichever is less.) If the
required operational report is due less
than 15 days following' completion of
plugging, then the plugging report
shall be submitted within 30 days for
Class II wells and 15 days for Class I
and III wells.
(b) In addition to the requirement of
§ 144.28(k)(l) of this chapter, owners and
operators of Class II wells shall include
a statement that the well was plugged
in accordance with §146.10 of this chap-
ter and §147.3109 of this subpart, and, if
the actual plugging differed, specify
the actual procedures used.
(c) The schedule upon which reports
of plugging must be submitted are
changed from those in §144.51(o) to
those specified in paragraph (a) of this
section.
§ 147.3106 Area of review.
(a) When determining the area of re-
view under §146.6(b) of this chapter, the
fixed radius shall be no less than one
mile for Class I wells and one-half mile
for Class II and III wells. In the case of
an application for an area permit, de-
termination of the area of review under
§146.6(b) shall be a fixed width of not
less than one mile for the circum-
scribing area of Class I projects and
one-half mile for the circumscribing
area of Class II and III projects.
(b) However, in lieu of §146.6(c) of
this chapter, if the area of review is de-
termined by a mathematical model
pursuant to paragraph § 146.6(a) of this
chapter, the permissible radius is the
result of such calculation even if it is
less than one mile for Class I wells and
one-half for Class II and III wells.
§ 147.3107 Mechanical integrity.
(a) Monitoring of annulus pressure
conducted pursuant to §146.8(b)(l) shall
be preceded by an initial pressure test.
A positive gauge pressure on the cas-
ing/tubing annulus (filled with liquid)
shall be maintained continuously. The
pressure shall be monitored monthly.
(b) Pressure tests conducted pursuant
to §146.8(b)(2) of this chapter shall be
performed with a pressure on the cas-
ing/tubing annulus of at least 200 p.s.i.
unless otherwise specified by the Direc-
tor. In addition, pressure tests con-
ducted during well operation shall
maintain an injection/annulus pressure
differential of at least 100 p.s.i.
throughout the tubing length.
(c) Monitoring of enhanced recovery
wells conducted pursuant to
1146.8(b)(3), must be preceded by an ini-
tial pressure test that was conducted
827
-------
§147.3108
40 CFR Ch. I (7-1-04 Edition)
no more than 90 days prior to the com-
mencement of monitoring.
§ 147,3108 Plugging Class I, II, and III
wells.
In addition to the requirements of
§146.10 of this chapter, owners and op-
erators shall comply with the following
when plugging a well:
(a) For Class I and III wells:
(1) The well shall be filled with mud
from the bottom of the well to a point
one hundred (100) feet below the top of
the highest disposal or injection zone
and then with a cement plug from
there to at least one hundred (100) feet
above the top of the disposal or injec-
tion zone.
(2) A cement plug shall also be set
from a point at least fifty (50) feet
below the shoe of the surface casing to
a point at least five (5) feet above the
top of the lowest USDW.
(3) A final cement plug shall extend
from a point at least thirty feet below
the ground surface to a point five (5)
feet below the ground surface.
(4) All intervals between plugs shall
be filled with mud.
(5) The top plug shall clearly show by
permanent markings inscribed in the
cement or on a steel plate embedded in
the cement the well permit number and
date of plugging.
(b) For Class n wells:
(1) The well shall be kept full of mud
as casing is removed. No surface casing
shall be removed without written ap-
proval from the Director.
(2) If surface casing is adequately set
and cemented through all USDWs (set
to at least 50 feet below the base of the
USDW), a plug shall be set at least 50
feet below the shoe of the casing and
extending at least 50 feet above the
shoe of the casing; or
(3) If the surface casing and cement-
ing is inadequate, the well bore shall be
filled with cement from a point at least
50 feet below the base of the USDW to
a point at least 50 feet above the shoe
of the surface casing, and any addi-
tional plugs as required by the Direc-
tor.
(4) In all cases, the top 20 feet of the
well bore below 3 feet of ground surface
shall be filled with cement. Surface
casing shall be cut off 3 feet below
ground surface and covered with a se-
cure steel cap on top of the surface
pipe. The remaining 3 feet shall be
filled with dirt.
(5) Except as provided in sub-para-
graph (b)(6) of this section, each pro-
ducing or receiving formation shall be
sealed off with at least a 50-foot ce-
ment plug placed at the base of the for-
mation and at least a 50-foot cement
plug placed at the top of the formation.
(6) The requirement in sub-paragraph
(b)(5) of this section does not apply if
the producing/receiving formation is
already sealed off from the well bore
with adequate casing and cementing
behind casing, and casing is not to be
removed, or the only openings from the
producing/receiving formation into the
well bore are perforations in the cas-
ing, and the annulus between the cas-
ing and the outer walls of the well is
filled with cement for a distance of 50
feet above the top of the formation.
When such conditions exist, a bridge
plug capped with at least 10 feet of ce-
ment set at the top of the producing
formation may be used.
(7) When specified by the Director,
any uncased hole below the shoe of any
casing to be left in the well shall be
filled with cement to a depth of at
least 50 feet below the casing shoe, or
the bottom of the hole, and the casing-
above the shoe shall be filled with ce-
ment to at least 50 feet above the shoe
of the casing. If the well has a screen
or liner which is not to be removed, the
well bore shall be filled with cement
from the base of the screen or liner to
at least 50 feet above the top of the
screen or liner.
(8) All intervals between cement
plugs in the well bore must be filled
with mud,
(c) For the purposes of this section
mud shall be defined as: mud of not less
than thirty-six (36) viscosity (API Full
Funnel Method) and a weight of not
less than nine (9) pounds per gallon.
§ 147.3109 Timing of mechanical integ-
rity test.
The demonstrations of mechanical
integrity required by §146.14(b)(2) of
this chapter prior to approval for the
operation of a Class I well shall, for an
existing well, be conducted no more
than 90 days prior to application for
the permit and the results included in
828
-------
Environmental Protection Agency
§148.3
the permit application. The owner or
operator shall notify the Director at
least seven days in advance of the time
and date of the test so that EPA ob-
servers may be present.
PART 148—HAZARDOUS WASTE
INJECTION RESTRICTIONS
Subpart A—General
Sec.
148.1 Purpose, scope and applicability.
148.2 Definitions.
148.3 Dilution prohibited as a substitute for
treatment.
148.4 Procedures for ease-by-case extensions
to an effective date.
148.5 Waste analysis.
Subpart B—Prohibitions on Injection
148.10 Waste specific prohibitions—solvent
wastes.
148.11 Waste specific prohibitions—dioxin-
containing wastes.
148,12 Waste specific prohibitions—Cali-
fornia list wastes.
148.14 Waste specific prohibitions—first
third wastes.
148.15 Waste specific prohibitions—second
third wastes,
148.18 Waste specific prohibitions—third
third wastes.
148.17 Waste specific prohibitions; newly
listed wastes.
148,18 Waste specific prohibitions-newly
listed and identified wastes.
Subpart C-
-Pefltion Standards and
Procedures
148.20 Petitions to allow injection of a
waste prohibited under subpart B.
148.21 Information to be submitted in sup-
port of petitions.
148.22 Requirements for petition submis-
sion, review and approval or denial.
148.23 Review of exemptions granted pursu-
ant to a petition.
148.24 Termination of approved petition.
AUTHORITY; Sees. 3004, Resource Conserva-
tion and Recovery Act, 42 U.S.C, 6901 et seg.
SOUBCB; 53 FR 28154, July 26, 1988, unless
otherwise noted.
Subpart A—General
§ 148.1 Purpose, scope and applica-
bility.
(a) This part identifies wastes that
are restricted from disposal into Class
I wells and defines those circumstances
under which a waste, otherwise prohib-
ited from injection, may be injected.
(b) The requirements of this part
apply to owners or operators of Class I
hazardous waste injection wells used to
inject hazardous waste.
(c) Wastes otherwise prohibited from
injection may continue to be injected:
(1) If an extension from the effective
date of a prohibition has been granted
pursuant to §148.4 with respect to such
wastes; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition filed under §148.20 to allow in-
jection of restricted wastes with re-
spect to those wastes and wells covered
by the exemption; or
(3) If the waste is generated by a con-
ditionally exempt small quantity gen-
erator, as defined in §261.5; or
(d) Wastes that are hazardous only
because they exhibit a hazardous char-
acteristic, and which are otherwise
prohibited under this part, or part 268
of this chapter, are not prohibited if
the wastes:
(1) Are disposed into a nonhazardous
or hazardous injection well as defined
under 40 CFR §146.6(a); and
(2) Do not exhibit any prohibited
characteristic of hazardous waste iden-
tified in 40 CFR part 261, subpart C at
the point of injection.
[53 FR 28154, July 26, 1988, as amended at 55
FR 22683, June 1, 1990: 57 FR 8088, Mar. 6,
1992; 57 FR 31783, July 20, 1992; 60 FR 33932,
June 29, 1995; 61 FR 15596, Apr. 8, 1996; 61 FR
33682, June 28, 1996]
§ 148.2 Definitions.
Injection interval means that part of
the injection zone in which the well is
screened, or in which the waste is oth-
erwise directly emplaced.
Transmissive fault or fracture is a fault
or fracture that has sufficient perme-
ability and vertical extent to allow
fluids to move between formations.
1148.3 Dilution prohibited as a sub-
stitute for treatment.
The prohibition of §268.3 shall apply
to owners or operators of Class I haz-
ardous waste Injection wells.
829
-------
§148.4
40 CFR Ch. I (7-1-04 Edition)
§ 148.4 Procedures for case-by-case ex-
tensions to an effective date.
The owner or operator of a, Class I
hazardous waste injection well may
submit an application to the Adminis-
trator for an extension of the effective
date of any applicable prohibition es-
tablished under subpart B of this part
according to the procedures of §268.5.
§ 148.S Waste analysis.
Generators of hazardous wastes that
are disposed of into Class I injection
wells must comply with the applicable
requirements of §268.7 (a) and (b). Own-
ers or operators of Class I hazardous
waste injection wells must comply
with the applicable requirements of
§268.7(c).
Subpart B—Prohibitions on
Injection
§148.10 Waste specific prohibitions-
solvent wastes,
(a) Effective August 8, 1988, the spent
solvent wastes specified in §261.31 as
EPA Hazardous Waste Nos. F001, F002,
F003, F004, and F005 are prohibited
from underground injection unless the
solvent waste is a solvent-water mix-
ture or solvent-containing sludge con-
taining less than 1 percent total F001-
F005 solvent constituents listed in
Table A of this section.
(b) Effective August 8, 1990, all spent
F001-F005 solvent wastes containing
less than 1 percent total FOQ1-F005 sol-
vent constituents listed in Table A of
this section are prohibited from injec-
tion.
(c) Effective August 8, 1990, all spent
F002 and F005 wastes containing sol-
vent constituents listed in Table B of
this section are prohibited from under-
ground injection at off-site injection
facilities.
(d) Effective November 8, 1990, the
wastes specified in paragraph (c) of this
section are prohibited from under-
ground injection at on-site injection
facilities.
(e) The requirements of paragraphs
(a) and (b) of this section do not apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148.4
of this part.
TABLE A
Acetone
n-Butyl alcohol
Carbon disulfide
Carbon tetraehloride
Chlorobenzene
Cresols and cresylic acid
Cyclohexanone
1,2-diehlorobenzene
Ethyl acetate
Ethyl benzene
Ethyl ether
Isobutanol
Methanol
Methylene chloride
Methylene chloride (from the pharma-
ceutical industry)
Methyl ethyl ketone
Methyl isobutyl ketone
Nitrobenzene
Pyridine
Tetrachloroethylene
Toulene
1,1,1-Triohloroe thane
l,2,2-Trichloro-l,2,2-trifluoroethane
Trichloroethylene
Trichlorofluorornethane
Xyleae
TABLE B
Benzene
2-Bthoxyethanol
2-Nitropropane
1,1,2-Trichloroetliane
[53 PR 28154, July 26, 1988, aa amended at 54
PR 25422, June 14, 1989; 56 PR 3876, Jan. 31,
1991; 57 PR 8088, Mar. 6, 1992]
§148.11 Waste specific prohibitions—
dioxin-containing wastes.
(a) Effective August 8, 1988, the
dioxin-containing wastes specified in
§261.31 as EPA Hazardous Waste Nos.
F020, F021, F022, F023, F026, F027, and
F028, and prohibited from underground
injection.
(b) The requirements of paragraph (a)
of this section do not apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
830
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Environmental Protection Agency
§148.14
petition under subpart C of this part;
or
(3) During- the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148.4
of this part.
[53 FR 28154, July 26, 1988, as amended at 54
PR 25422, June 14, 1989]
§ 148,12 Waste specific prohibitions—
California list wastes.
(a) Effective August 8, 1988, the haz-
ardous wastes listed in 40 OPB 268.32
containing polychlorinated biphenyls
at concentrations greater than or equal
to 50 ppm or halogenated organic com-
pounds at concentrations greater than
or equal to 10,000 mg/kg are prohibited
from underground injection.
(b) Effective August 8, 1990, the fol-
lowing hazardous wastes are prohibited
from underground injection:
(1) Liquid hazardous wastes, includ-
ing free liquids associated with any
solid or sludge, containing free
cyanides at concentrations greater
than or equal to 1,000 mg/1;
(2) Liquid hazardous wastes, includ-
ing free liquids associated with any
solid or sludge, containing the fol-
lowing metals (or elements) or com-
pounds of these metals (or elements) at
concentrations greater than or equal to
those specified below:
(i) Arsenic and/or compounds (as As)
500 mg/1;
(ii) Cadmium and/or compounds (as
Cd) 100 mg/1;
(lii) Chromium (VI) and/or com-
pounds (as Or VI) 500 mg/1;
(iv) Lead and/or compounds (as Pb)
500 mg/1;
(v) Mercury and/or compounds (as
Hg-) 20 mg/1;
(vi) Nickel and/or compounds (as Ni)
134 mg/1;
(vii) Selenium and/or compounds (as
Se) 100 mg/1; and
(viii) Thallium and/or compounds (as
Tl) 130 mg/1;
(3) Liquid hazardous waste having a
pH less than or equal to two (2.0); and
(4) Hazardous wastes containing halo-
genated organic compounds in total
concentration less than 10,000 mg/kg
but greater than or equal to 1,000 rag/
kg.
(c) The requirements of paragraphs
(a) and (b) of this section do not apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension is granted under §148.4 of this
part.
[53 FR 30918, Aug. 16, 1988, as amended at 53
PR 41602, Oct. 24, 1988]
§148.14 Waste specific prohibitions—
first third wastes.
(a) Effective June 7, 1889, the wastes
specified in 40 CPR 261.31 as EPA Haz-
ardous Waste numbers F006 (nonwaste-
waters) and the wastes specified in 40
CFR 261.32 as EPA Hazardous Waste
numbers K001, K015 (wastewaters), K016
(at concentrations greater than or
equal to 1%), K018, K019, K020, K021
(nonwastewaters generated by the
process described in the waste listing
description and disposed after August
17, 1988, and not generated in the
course of treating wastewater forms of
these wastes), K022 (nonwastewaters),
K024, K030, K036 (nonwastewaters gen-
erated by the process described in the
waste listing description and disposed
after August 17, 1988, and not generated
in the course of treating wastewater
forms of these wastes), K037, K044,
K045, nonexplosive K046 (nonwaste-
waters), K047, K048, K060 (nonwaste-
waters generated by the process de-
scribed in the waste listing description
and disposed after August 17, 1988, and
not generated in the course of treating
wastewater forms of these wastes),
K061 (nonwastewaters), noncalcium
sulfate K069 (nonwastewaters gen-
erated by the process described in the
waste listing description and disposed
after August 17, 1988, and not generated
in the course of treating wastewater
forms of these wastes), K086 solvent
washes, K087, K099, K101 (all waste-
waters and less than 1% total arsenic
nonwastewaters), K102 (all wastewaters
and less than 1% total arsenic non-
wastewaters), and K103 are prohibited
from underground injection.
831
-------
§148.15
40 CFR Ch. I (7-1-04 Edition)
(b) Effective June 8, 1989, the waste
specified in 40 OFR 261.32 as EPA Haz-
ardous Waste number K036 (waste-
waters); and the wastes specified in 40
CPE 261.33 as P030, P039, P041, P063,
P071, P089, P094, P097, U221, and U223
are prohibited from underground injec-
tion.
(c) Effective July 8, 1989, the wastes
specified in 40 CPE 261.31 as EPA Haz-
ardous Waste numbers F008 and F009
are prohibited from underground injec-
tion.
(d) Effective August 8, I960, the
wastes specified in 40 CFE 261.31 as
EPA Hazardous Waste Number F006
(wastewaters) and F019; the wastes
specified in 40 CFE 261.32 as EPA Haz-
ardous Waste Numbers K004, K008, K015
(nonwastewaters), K017, K021
(wastewaters), K022 (wastewaters),
K031, K035, K046 (reactive nonwaste-
waters and all wastewaters), K060
(wastewaters), K061 (wastewaters), K069
(calcium sulfate nonwastewaters and
all wastewaters), K073, K083, K084, K085,
K086 (all but solvent washes), K101
(high arsenic nonwastewaters), K102
(high arsenic nonwastewaters), and
K106; and the wastes specified in 40
CFE part 261.33 as EPA Hazardous
Waste Numbers P001, P004, P005, P010,
P011, P012, P015, P016, P018, P020, P036,
P037, P048, P050, P058, P059, P068, P069,
P070, P081, P082, P084, P087, P092, P102,
P105, P108, P110, P115, P120, P122, P123,
U007, U009, U010, U012, TJ016, U018, U019,
U022, U029, U031, U036, U037, U041, U043,
U044, U046, U050, U051, U053, U061, U063,
U064, U066, U067, U074, U077, U078, U086,
U089, U103, U105, U108, U115, U122, U124,
U129, U130, U133, U134, U137, U151, U154,
U155, U157, U158, U159. U171, U177, U180,
U185, U188, U192, U200, U209, U210, U211,
U219, U220, U226, U227, U228, U237, U238,
U248, and U249 are prohibited from un-
derground injection at off-site injec-
tion facilities.
(e) Effective August 8, 1990, the
wastes specified in 40 CFE 261.32 as
EPA Hazardous Waste numbers K049,
K050, K051, K052, K062, K071, and K104
are prohibited from underground injec-
tion.
(f) Effective November 8, 1990, the
wastes specified in paragraph (d) of this
section are prohibited from under-
ground injection at on-site injection
facilities.
(g) Effective June 7, 1991, the wastes
specified in 40 CFE 261.32 as EPA Haz-
ardous Waste numbers K016 (at con-
centrations less than 1%) are prohib-
ited from underground injection.
(h) Effective June 8, 1991, the waste
specified in 40 CFE 261.31 as EPA Haz-
ardous Waste number F007; and the
wastes specified in 40 CFE 261.32 as
K011 (nonwastewaters) and K013 (non-
wastewaters) are prohibited from un-
derground injection.
(i) Effective May 8, 1992, the wastes
specified in 40 CFE 261.32 and 261.33 as
EPA Hazardous Waste Numbers K011
(wastewaters), K013 (wastewaters), and
K014 are prohibited from underground
injection.
(j) The requirements of paragraphs
(a) through (i) of this section do not
apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148.4
of this part.
[54 FB 25423, June 14, 1989, as amended at 54
PR 26647, June 23, 1989; 54 FB 35328, Aug. 25,
1989; 55 PR 22683, June 1, 1990]
§ 148.15 Waste specific prohibitions—
second third wastes.
(a) Effective June 7, 1989, the wastes
specified in 40 CFE 261.32 as EPA Haz-
ardous Waste numbers K025 (non-
wastewaters generated by the process
described in the waste listing descrip-
tion and disposed after August 17, 1988,
and not generated in the course of
treating wastewater forms of these
wastes) are prohibited from under-
ground injection.
(b) Effective June 8, 1989, the wastes
specified in 40 CFE 261.31 as EPA Haz-
ardous Waste numbers F010, F024; the
wastes specified in 40 CFE 261.32 as
K009 (nonwastewaters), K010, K027,
K028, K029 (nonwastewaters), K038,
K039, K040, K043, K095 (nonwaste-
waters), K096 (nonwastewaters), K113,
K114, K115, K116; and wastes specified
in 40 CFE 261.33 as P029, P040, P043,
P044, P062, P074, P085, P098, P104, P106,
832
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Environmental Protection Agency
§148.16
Pill, TJ028, U058, U107, and U235 are pro-
hibited from underground injection.
(c) Effective July 8, 1989, and con-
tinuing until December 8, 1989, the
wastes specified in 40 CFR 261,31 as
EPA Hazardous Waste numbers P011
and F012 are prohibited from under-
ground injection pursuant to the treat-
ment standards specified in §§268.41 and
268.43 applicable to F007, F008, and POOS
wastewaters and nonwastewaters. Ef-
fective December 8, 1989, P011 (non-
wastewaters) and F012 (nonwaste-
waters) are prohibited pursuant to the
treatment standards specified in
§§268.41 and 268.43 applicable to P011
and P012 wastewaters and nonwaste-
waters.
(d) Effective August 8, 1990, the
wastes specified in 40 CFE 261.32 as
EPA Hazardous Waste Number K025
(wastewaters), K029 (wastewaters),
K041, K042, K095 (wastewaters), K096
(wastewaters), K097, K098, and K105;
and the wastes specified in 40 CFR part
261.33 as P002, POOS, P007, POOS, POM,
P026, P027, P049, P054, P057, P060, P066,
P067, P072, P107, P112, P113, P114, U002,
U003, U005, U008, U011, U014, U015, U020,
U021, U023, U025, U026, D032, TJ035, UQ47,
U049, U057, U059, U060, U062, U070, U073.
U080, U083, U092. U093, U094, U095, U097,
U098, U099, U101, U106, U109, U110, Ulll.
U114, U116, U119, U127, U128, U131, U135,
U138, U140, U142, U143, U144, U146, U147,
U149, U150, U161, U162, U163, U164, U165,
U168, U169, U170, U172. U173, U174, U176,
TJ178, U179, U189, U193, U196, U203, U205,
U206, U208. U213, TJ214. U215, U216, U217,
U218, U239, and U244 are prohibited
from underground injection at off-site
injection facilities.
(e) Effective June 8, 1991. the waste
specified in 40 CFR 261.32 as EPA Haz-
ardous Waste number K009 (waste-
waters) is prohibited from underground
injection.
(f) Effective November 8, 1990, the
wastes specified in paragraph (d) of this
section are prohibited from under-
ground injection at on-site injection
facilities.
(g) The requirements of paragraphs
(a) through (f) of this section do not
apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148.4
of this part.
[54 FR 25423, June 14, 1989, as amended at 54
PR 26647, June 23. 1989; 55 FR 22683, June 1,
1990]
§148.16 Waste specific prohibitions—
third third wastes.
(a) Effective June 7, 1989, the wastes
specified in 40 CFR 261.32 as EPA Haz-
ardous Waste numbers K100 (nonwaste-
waters generated by the process de-
scribed In the waste listing description
and disposed after August 17, 1988, and
not generated in the course of treating
wastewater forms of these wastes) are
prohibited from underground Injection.
(b) Effective June 8, 1989, the wastes
specified in 40 CPR 261.32 as EPA Haz-
ardous Waste numbers K005 (nonwaste-
waters), K007 (nonwastewaters), K023,
K093, K094; and the wastes specified in
40 CFR 261.33 as P013, P021, P099, P109,
P121, U069, UQ87, U088, U102, and U190
are prohibited from underground injec-
tion.
(c) Effective August 8, 1990, the
wastes identified in 40 CPR 261,31 as
EPA Hazardous Waste Number P039
(nonwastewaters); the wastes specified
In 40 CFE 261.32 as EPA Hazardous
Waste Numbers K002, K003, K005 (waste-
waters), K006, K007 (wastewaters), K026,
K032, K033, K034, and K100 (waste-
waters); the wastes specified in 40 CPR
261.33 as P006, P009, P017, P022, P023,
P024, P028, P031, P033, P034, P038, P042,
P045, P046, P047, P051, P056, P064. P065,
P073, P075, P076, P077, P078, P088, P093,
P095, P096, P101, P103, P116, P118, P119,
U001, U004, U006, U017. U024, U027, U030,
U033, U034, U038, U039, U042, U045, U048,
U052, U055, TJ056, U068, U071, U072, U075.
U076, U079, U081. U082, U084, U085, U090,
U091. TJ098, U112, U113, U117, U118, U120,
U121, U123. U125, U126, U132, U136, U141,
U145, U148, U152, U153, U156, U160, U166,
U167, U181, U182, U183, U184, U186, U187,
U191, U194, U197, U201, U202, U204, U207,
U222, U225, U234, U236, U240, U243, U246,
and U247; and the wastes identified in
40 CPR 261.21, 261.23 or 261.24 as haz-
ardous based on a characteristic alone.
833
-------
§148.17
40 CFR Ch.! (7-1-04 Edition)
designated as D001, D004, D005, DOM,
D008, D009 (wastewaters), D010, D011,
D012, D013, DQ14, D015, D016, D017, and
newly listed waste P025 are prohibited
from underground Injection at off-site
injection facilities.
(d) Effective August 8, 1990, mixed ra-
dioactive/hazardous waste in 40 CFR
268.10, 268.11, and 268.12, that are mixed
radioactive and hazardous wastes, are
prohibited from underground injection.
(e) Effective November 8, 1990, the
wastes specified in paragraph (c) of this
section are prohibited from under-
ground injection at on-site injection
facilities. These effective dates do not
apply to the wastes listed in 40 CPE
148.12(b) which are prohibited from un-
derground injection on August 8,1990.
(f) Effective May 8, 1992, the waste
identified in 40 CPE 261.31 as EPA Haz-
ardous Waste Number P039 (waste-
waters); the wastes Identified in 40 CFR
261.22, 261.23 or 261.24 as hazardous
based on a characteristic alone, des-
ignated as D002 (wastewaters and non-
wastewaters), D003 (wastewaters and
nonwastewaters), D007 (wastewaters
and nonwastewaters), and D009 (non-
wastewaters) are prohibited from un-
derground injection. These effective
dates do not apply to the wastes listed
in 40 CPR 148.12(b) which are prohibited
from underground Injection on August
8, 1990.
(g) The requirements of paragraphs
(a) through (f) of this section do not
apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148.4
of this part.
[54 PR 25423, June 14, 1989, as amended at 54
PR 26647, June 23, 1989; 55 PR 22683, June 1,
1990; 55 PR 33694, Aug. 17, 1990; 56 PR 3876,
Jan. 31,1991]
§148.17 Waste specific prohibitions;
newly listed wastes.
(a) Effective November 9, 1992, the
wastes specified in 40 CPR part 261 as
EPA hazardous waste numbers P037,
F038, K107, K108, K109, K110, Kill, K112,
K117, K118, K123, K124, K125, K126, K131,
K136, U328, U353, and U359 are prohib-
ited from underground injection.
(b) Effective December 19, 1994 the
wastes specified in 40 CPR 261.32 as
EPA Hazardous waste numbers K141,
K142, K143, K144, K145, K147, K148, K14.9,
K150, and K151, are prohibited from un-
derground injection.
(c) [Reserved]
(d) Effective June 30, 1995, the wastes
specified in 40 CPR part 261 as EPA
Hazardous waste numbers K117, K118,
K131, and K132 are prohibited from un-
derground injection.
(e) The requirements of paragraphs
(a) and (b) of this section do not apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under §148,4
of this part,
[57 PR 37263, Aug. 18, 1992, as amended at 59
PR 48041, Sept. 19, 1994; 61 PR 15662, Apr. 8,
1996]
§148.18 Waste specific prohibitions—
newly listed and identified •wastes.
(a) Effective August 24, 1998, all
newly Identified D004-D011 wastes and
characteristic mineral processing
wastes, except those identified in para-
graph (b) of this section, are prohibited
from underground injection.
(b) Effective May 26, 2000, char-
acteristic hazardous wastes from tita-
nium dioxide mineral processing, and
radioactive wastes mixed with newly
identified D004-D011 or mixed with
newly identified characteristic mineral
processing wastes, are prohibited from
underground injection.
(c) Effective August 11, 1997, the
wastes specified in 40 CFR part 261 as
BPA Hazardous waste numbers F032,
F034, F035 are prohibited from under-
ground injection.
(d) Effective May 12, 1999, the wastes
specified in 40 CFR part 261 as EPA
Hazardous waste numbers F032, F034,
F035 that are mixed with radioactive
834
-------
Environmental Protection Agency
§148.20
wastes are prohibited from under-
ground injection.
(e) On July 8, 1996, the wastes speci-
fied in 40 CFR 261.32 as EPA Hazardous
waste numbers K156-K161, P127, P128,
P185, P18a-P192, P194, P196-P199, P201-
P205, U271, U277-U280, U364-U367, U372,
U373, U375-U379, U381-387. U389^U396,
U40O-U404, U407, and U409-U411 are pro-
hibited from underground injection.
(f) On January 8. 1997, the wastes
specified in 40 CFR 261.32 as EPA Haz-
ardous waste number K088 is prohibited
from underground injection.
(g) On April 8, 1998, the wastes speci-
fied in 40 CPR part 261 as EPA Haz-
ardous waste numbers D018-043. and
Mixed TC/Radioactive wastes, are pro-
hibited from underground injection.
(h) [Reserved]
(i) Effective February 8, 1999, the
wastes specified in 40 CPR 261.32 as
EPA Hazardous Waste Numbers K169,
K170, K171, and K172 are prohibited
from underground injection.
(j) Effective May 8, 2001, the wastes
specified in 40 CPR 261.32 as EPA Haz-
ardous Waste Numbers K174 and K175
are prohibited from underground injec-
tion.
(k) Effective May 20, 2002, the wastes
specified in 40 CFR 261.32 as EPA Haz-
ardous Waste Numbers K176, K177, and
K178 are prohibited from underground
injection.
(1) The requirements of paragraphs
(a) through (k) of this section do not
apply:
(1) If the wastes meet or are treated
to meet the applicable standards speci-
fied in subpart D of 40 CPR part 268; or
(2) If an exemption from a prohibi-
tion has been granted in response to a
petition under subpart C of this part;
or
(3) During the period of extension of
the applicable effective date, if an ex-
tension has been granted under § 148.4.
[61 FR 15662, Apr. 8, 1996, as amended at 62
PR 26018, May 12, 1997; 63 FE 24624, May 4,
1998; 63 FB 28636, May 26, 1998; 63 FB 35149,
June 29, 1998; 63 FB 42184, Aug. 6, 1998; 66 PR
14474, Mar. 17. 2000; 65 PR 36366, June 8, 2000;
65 PR 67126, Nov. 8, 2000; 66 FB 58297, Nov. 20,
2001]
Subpart C—Petition Standards and
Procedures
§ 148.20 Petitions to allow injection of
a waste prohibited under subpart
B.
(a) Any person seeking an exemption
from a prohibition under subpart B of
this part for the injection of a re-
stricted hazardous waste into an injec-
tion well or wells shall submit a peti-
tion to the Director demonstrating
that, to a reasonable degree of cer-
tainty, there will be no migration of
hazardous constituents from the injec-
tion zone for as long as the waste re-
mains hazardous. This demonstration
requires a showing that:
(1) The hydrogeological and geo-
chemical conditions at the sites and
the physiochemical nature of the waste
stream(s) are such that reliable pre-
dictions can be made that:
(i) Fluid movement conditions are
such that the injected fluids will not
migrate within 10,000 years:
(A) Vertically upward out of the in-
jection zone; or
(B) Laterally within the injection
zone to a point of discharge or inter-
face with an Underground Source of
Drinking Water (USDW) as defined in
40 CPR part 146; or
(ii) Before the injected fluids migrate
out of the injection zone or to a point
of discharge or interface with USDW,
the fluid will no longer be hazardous
because of attenuation, transforma-
tion, or immobilization of hazardous
constituents within the injection aone
by hydrolysis, chemical interactions or
other means; and
(2) For each well the petition has:
(i) Demonstrated that the injection
well's area of review complies with the
substantive requirements of §146.63;
(ii) Located, identified, and ascer-
tained the condition of all wells within
the injection well's area of review (as
specified in §146.63) that penetrate the
injection zone or the confining zone by
use of a protocol acceptable to the Di-
rector that meets the substantive re-
quirements of § 146.64;
(iii) Submitted a corrective action
plan that meets the substantive re-
quirements of §146.64, the implementa-
tion of which shall become a condition
of petition approval; and
835
-------
§148.21
40 CFR Ch. I (7-1-04 Edition)
(iv) Submitted the results of pressure
and radioactive tracer tests performed
within one year prior to submission of
the petition demonstrating the me-
chanical integrity of the well's long
string casing, injection tube, annular
seal, and bottom hole cement. In cases
where the petition has not been ap-
proved or denied within one year after
the initial demonstration of mechan-
ical integrity, the Director may re-
quire the owner or operator to perform
the tests again and submit the results
of the new tests.
NOTE: The requirements of §148.20(a)(2)
need not be incorporated in a permit at the
time of petition approval.
(b) A demonstration under
§148.2Q(a)(l)(i) shall identify the strata
within the injection zone which will
confine fluid movement above the in-
jection interval and include a showing
that this strata is free of known
transmissive faults of fractures and
that there is a confining zone above the
injection zone.
(c) A demonstration under
§148.20(a)(l)(ii) shall identify the strata
within the injection zone where waste
transformation will be accomplished
and include a showing that this strata
is free of known transmissive faults or
fractures and that there is a confining
zone above the injection zone.
(d) A demonstration may include a
showing that:
(1) Treatment methods, the imple-
mentation of which shall become a
condition of petition approval, will be
utilized that reduce the toxicity or mo-
bility of the wastes; or
(2) A monitoring- plan, the implemen-
tation of which shall become a condi-
tion of petition approval, will be uti-
lized to enhance confidence in one or
more aspects of the demonstration.
(e) Any person who has been granted
an exemption pursuant to this section
may submit a petition for reissuance of
the exemption to include an additional
restricted waste or wastes or to modify
any conditions placed on the exemp-
tion by the Director, The Director
shall reissue the petition if the peti-
tioner complies with the requirements
of paragraphs (a), (b) and (c) of this sec-
tion.
(f) Any person who has been granted
an exemption pursuant to this section
may submit a petition to modify an ex-
emption to include an additional (haz-
ardous) waste or wastes. The Director
may grant the modification if he deter-
mines, to a reasonable degree of cer-
tainty, that the additional waste or
wastes will behave hydraulically and
chemically in a manner similar to pre-
viously included wastes and that it will
not interfere with the containment ca-
pability of the injection zone.
1148.21 Information to be submitted
in support of petitions,
(a) Information submitted in support
of §148.20 must meet the following cri-
teria:
(1) All waste analysis and any new
testing performed by the petitioner
shall be accurate and reproducible and
performed in accordance with quality
assurance standards;
(2) Estimation techniques shall be ap-
propriate, and EPA-certified test pro-
tocols shall be used where available
and appropriate;
(3) Predictive models shall have been
verified and validated, shall be appro-
priate for the specific site, waste
streams, and injection conditions of
the operation, and shall be calibrated
for existing sites where sufficient data
are available;
(4) An approved quality assurance
and quality control plan shall address
all aspects of the demonstration;
(5) Reasonably conservative values
shall be used whenever values taken
from the literature or estimated on the
basis of known information are used in-
stead of site-specific measurements;
and
(6) An analysis shall be performed to
identify and assess aspects of the dem-
onstration that contribute signifi-
cantly to uncertainty. The petitioner
shall conduct a sensitivity analysis to
determine the effect that significant
uncertainty may contribute to the
demonstration. The demonstration
shall then be based on conservative as-
sumptions identified in the analysis.
(b) Any petitioner under
§148.20(a)(l)(i) shall provide sufficient
site-specific information to support the
demonstration, such as:
(1) Thickness, porosity, permeability
and extent of the various strata in the
injection zone;
836
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Environmental Protection Agency
§148,24
(2) Thickness, porosity, permeability,
extent, and continuity of the confining
zone;
(3) Hydraulic gradient in the injec-
tion zone;
(4) Hydrostatic pressure in the injec-
tion zone; and
(5) G-eoehemical conditions of the
site.
(c) In addition to the information in
§148.21(b), any petitioner under
§i48,20(a)(l)(ii) shall provide sufficient
waste-specific information to ensure
reasonably reliant predictions about
the waste transformation. The peti-
tioner shall provide the information
necessary to support the demonstra-
tion, such as:
(1) Description of the chemical proc-
esses or other means that will lead to
waste transformation; and
(2) Results of laboratory experiments
verifying the waste transformation.
§ 148,22 Requirements for petition sub-
mission, review and approval or de-
nial.
(a) Any petition submitted to the Di-
rector pursuant to §148.20(a) shall in-
clude the following components:
(1) An identification of the specific
waste or wastes and the specific injec-
tion well or wells for which the dem-
onstration will be made;
(2) A waste analysis to describe fully
the chemical and physical characteris-
tics of the subject wastes;
(3) Such additional information as is
required by the Director to support the
petition under §§148.20 and 148.21; and
(4) This statement signed by the peti-
tioner or an authorized representative:
I certify under penalty of law that I have
personally examined and am familiar with
the information submitted in this petition
and all attached documents, and that, based
on my inquiry of those individuals imme-
diately responsible for obtaining the infor-
mation, I believe that submitted information
is true, accurate, and complete. I am aware
that there are significant penalties for sub-
mitting false information, including the pos-
sibility of fine and imprisonment.
(b) The Director shall provide public
notice and an opportunity for public
comment in accordance with the proce-
dures in §124.10 of the intent to approve
or deny a petition. The final decision
on a petition will be published in the
FEDERAL REGISTER.
(c) If an exemption is granted it will
apply only to the underground injec-
tion of the specific restricted waste or
wastes identified in the petition into a
Class I hazardous waste injection well
or wells specifically identified in the
petition (unless the exemption is modi-
fied or reissued pursuant to §148.20(e)
or (f).
(d) Upon request by any petitioner
who obtains an exemption for a well
under this subpart, the Director shall
initiate and reasonably expedite the
necessary procedures to issue or re-
issue a permit or permits for the haz-
ardous waste well or wells covered by
the exemption for a term not to exceed
ten years.
§ 148.23 Review of exemptions granted
pursuant to a petition.
(a) When considering whether to re-
issue a permit for the operation of a
Class I hazardous waste injection well,
the Director shall review any petition
filed pursuant to §148.20 and require a
new demonstration if information
shows that the basis for granting the
exemption may no longer be valid.
(b) Whenever the Director determines
that the basis for approval of a petition
may no longer be valid, the Director
shall require a new demonstration in
accordance with §148.20.
§ 148.24 Termination of approved peti-
tion.
(a) The Director may terminate an
exemption granted under § 148.20 for the
following causes:
(1) Noncompliance by the petitioner
with any condition of the exemption;
(2) The petitioner's failure in the pe-
tition or during the review and ap-
proval to disclose fully all relevant
facts, or the petitioner's misrepresen-
tation of any relevant facts at any
time; or
(3) A determination that new infor-
mation shows that the basis for
approval of the petition is no longer
valid.
(b) The Director shall terminate an
exemption granted under §148.20 for the
following causes:
(1) The petitioner's willful with-
holding during the review and approval
837
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Pt. 149
40 CFR Ch. I (7-1-04 idfflon)
of the petition of facts directly and ma-
terially relevant to the Director's deci-
sion on the petition;
(2) A determination that there has
been migration from the injection zone
or the well that is not in accordance
with the terms of the exemption, ex-
cept that the Director may at his dis-
cretion decide not to terminate where:
(i) The migration resulted from a me-
chanical failure of the well that can be
corrected promptly through a repair to
the injection well itself or from an un-
detected well or conduit that can be
plugged promptly; and
(ii) The requirements of §146.67(1) are
satisfied.
(c) The Director shall follow the pro-
cedures in § 124.5 in terminating any ex-
emption under this section.
PART 149—SOLE SOURCE AQUIFERS
Subpart A—Criteria for Identifying Critical
Aquifer Protection Areas
Sec.
149,1 Purpose.
149.2 Definitions.
149.3 Critical Aquifer Protection Areas.
Subpart B—Review of Projects Affecting
the Edwards Underground Reservoir, A
Designated Sole Source Aquifer in the
San Antonio, Texas Area
149.100 Applicability.
149.101 Definitions.
149.102 Project review authority.
149.103 Public information.
149.104 Submission of petitions.
149.105 Decision to review.
149.106 Notice of review.
149.107 Bequest for information.
149.108 Public hearing.
149.109 Decision under section 1424{e).
149.110 Besubmittal of redesigned projects.
149.111 Funding to redesigned projects.
AUTHORITY: Sec. 1424(e), Safe Drinking
Water Act (42 U.S.C. 300h-3(e); sec. 1427 of the
Safe Drinking Water Act, (42 U.S.C. 3QOB-6).
Subpart A—Criteria for Identifying
Critical Aquifer Protection Areas
SOURCE: 52 PE 23986, June 26, 1987, unless
otherwise noted.
§ 149.1 Purpose.
The purpose of this subpart is to pro-
vide criteria for identifying critical aq-
uifer protection areas, pursuant to sec-
tion 1427 of the Safe Drinking Water
Act (SDWA).
§ 149.2 Definitions.
(a) Aquifer means a geological forma-
tion, group of formations, or part of a
formation that is capable of yielding a
significant amount of water to a well
or spring.
(b) Recharge means a process, natural
or artificial, by which water is added to
the saturated zone of an aquifer.
(c) Recharge Area means an area in
which water reaches the zone of satura-
tion (ground water) by surface infiltra-
tion; in addition, a major recharge area
is an area where a major part of the re-
charge to an aquifer occurs.
(d) Sole or Principal Source Aquifer
(SSA) means an aquifer which is des-
ignated as an SSA under section 1424(e)
of the SDWA.
[54 FE 6843, Feb. 14, 1989]
§149.8 Critical Aquifer Protection
Areas.
A Critical Aquifer Protection Area is
either:
(a) All or part of an area which was
designated as a sole or principal source
aquifer prior to June 19, 1986, and for
which an areawide ground-water qual-
ity protection plan was approved,
under section 208 of the Clean Water
Act, prior to that date; or
(b) All or part of a major recharge
area of a sole or principal source aqui-
fer, designated before June 19, 1988, for
which:
(1) The sole or principal source aqui-
fer is particularly vulnerable to con-
tamination due to the hydrogeologic
characteristics of the unsaturated or
saturated zone within the suggested
critical aquifer protection area; and
(2) Contamination of the sole or prin-
cipal source aquifer is reasonably
likely to occur, unless a program to re-
duce or prevent such contamination is
implemented; and
(3) In the absence of any program to
reduce or prevent contamination, rea-
sonably foreseeable contamination
would result in significant cost, taking
into account:
(i) The cost of replacing the drinking
water supply from the sole or principal
source aquifer, and
838
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Environmental Protection Agency
§149.101
(ii) Other economic costs and envi-
ronmental and social costs resulting
from such contamination.
[54 FB 6843, Feb. 14, 1989]
Subpart B—Review of Projects Af-
fecting the Edwards Under-
ground Reservoir, A Des-
ignated Sole Source Aquifer in
the San Antonio, Texas Area
SOURCE: 42 FE 51574, Sept. 29, 1977, unless
otherwise noted. Redesignated at 52 PR 23986,
June 26, 1987.
§ 149.100 Applicability.
This subpart sets forth, pursuant to
sections 1424(e) and 1450 of the Public
Health Service Act, as amended by the
Safe Drinking Water Act, Pub. L. 93-
523, regulations relating the Edwards
Underground Reservoir which is the
sole or principal drinking water source
for the San Antonio area and which, if
contaminated, would create a signifi-
cant hazard to public health.
[42 FR 51574, Sept. 29, 1977. Redesignated and
amended at 52 FB 23986, Jane 26,1987]
§ 149.101 Definitions.
As used in this subpart and except as
otherwise specifically provided, the
term(s):
(a) Act means the Public Health Serv-
ice Act, as amended by the Safe Drink-
ing Water Act, Public Law 93-623.
(b) Contaminant means any physical,
chemical, biological, or radiological
substance or matter in water.
(c) Recharge zone means the area
through which water enters the Ed-
wards Underground Reservoir as de-
fined in the December 16, 1975, Notice
of Determination.
(d) Administrator (Regional Adminis-
trator) means the Administrator (Re-
gional Administrator) of the United
States Environmental Protection
Agency.
(e) Person means an individual, cor-
poration, company, association, part-
nership, State, or municipality.
(f) Project means a program or action
for which an application for Federal fi-
nancial assistance has been made.
(g) Federal financial assistance means
any financial benefits provided directly
as aid to a project by a department,
agency, or instrumentality of the Fed-
eral government in any form including
contracts, grants, and loan guarantees.
Actions or programs carried out by the
Federal government itself such as
dredging performed by the Army Corps
of Engineers do not involve Federal fi-
nancial assistance. Actions performed
for the Federal government by contrac-
tors, such as construction of roads on
Federal lands by a contractor under
the supervision of the Bureau of Land
Management, should be distinguished
from contracts entered into specifi-
cally for the purpose of providing fi-
nancial assistance, and will not be con-
sidered programs or actions receiving
Federal financial assistance. Federal
financial assistance is limited to bene-
fits earmarked for a specific program
or action and directly awarded to the
program or action. Indirect assistance,
e.g., in the form of a loan to a devel-
oper by a lending institution which in
turn receives Federal assistance not
specifically related to the project in
question is not Federal financial assist-
ance under section 1424(e).
(h) Commitment of Federal financial as-
sistance means a written agreement en-
tered into by a department, agency, or
instrumentality of the Federal Govern-
ment to provide financial assistance as
defined in paragraph (g) of this section.
Renewal of a commitment which the
issuing agency determines has lapsed
shall not constitute a new commitment
unless the Regional Administrator de-
termines that the project's impact on
the aquifer has not been previously re-
viewed under section 1424(e). The deter-
mination of a Federal agency that a
certain written agreement constitutes
a commitment shall be conclusive with
respect to the existence of such a com-
mitment.
(i) Stream/low source zone means the
upstream headwaters area which drains
into the recharge zone as defined in the
December 16, 1975, Notice of Deter-
mination.
(j) Significant hazard to public health
means any level of contaminant which
causes or may cause the aquifer to ex-
ceed any maximum contaminant level
set forth in any promulgated National
Primary Drinking Water Standard at
any point where the water may be used
for drinking- purposes or which may
839
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§149.102
40 CFR Ch. I (7-1-04 Edition)
otherwise adversely affect the health of
persons, or which may require a public
water system to install additional
treatment to prevent such adverse ef-
fect.
(k) Aquifer means the Edwards Under-
ground Reservoir.
[42 PR 51574, Sept. 29, 1977. Redeslgnated and
amended at 52 FR 23986, June 26, 1987]
§ 149.102 Project review authority.
(a) Once an area is designated, no
subsequent commitments of Federal fi-
nancial assistance may be made to
projects which the Administrator de-
termines may contaminate the aquifer
so as to create a significant hazard to
public health.
(b) The Regional Administrator is
hereby delegated the authority and as-
signed responsibility for carrying out
the project review process assigned to
the Administrator under-section 1424(e)
of the Act, except the final determina-
tion that a project may contaminate
the aquifer through its recharge zone
so as to create a significant hazard to
public health.
(c) The Regional Administrator may
review any project which he considers
may potentially contaminate the aqui-
fer through its recharge zone so as to
create a significant hazard to public
health.
§ 149.103 Public information.
After the area is designated under
section 1424(e), Federal agencies, for
projects, located in the recharge zone
and streamflow source zones, are re-
quired to:
(a) Maintain a list of projects for
which environmental impact state-
ments will be prepared in accordance
with the National Environmental Pol-
icy Act (NEPA);
(b) Revise the list at regular inter-
vals and submit to EPA; and
(c) Make the list available to the
public upon request,
§ 149.104 Submission of petitions.
Any person may submit a petition re-
questing the Regional Administrator
to review a project to determine if such
project may contaminate the aquifer
through its recharge zone so as to
create a significant hazard to public
health. Any such petition shall iden-
tify:
(a) The name, address, and telephone
number of the individual, organization,
or other entity submitting the peti-
tion;
(b) A brief statement of the request-
ing person's interest in the Regional
Administrator's determination;
(c) The name of the project and Fed-
eral agency involved;
In addition, the petitioner is requested
to submit to EPA available informa-
tion on:
(d) Applicable action already taken
by State and local agencies including
establishment of regulations to prevent
contamination of the aquifer and why,
in the petitioner's judgment, the ac-
tion was inadequate.
(e) Any actions taken under the Na-
tional Environmental Policy Act and
why, in the petitioner's judgment, that
action was inadequate in regard to
evaluation of potential effect on the
aquifer.
(f) The potential contaminants in-
volved;
(g) The means by which the contami-
nant might enter the aquifer: and
(h) The potential impact of the pro-
posed project.
§ 149.105 Decision to review.
(a) The Regional Administrator shall
review under section 1424(e) all projects
located in the recharge or streamflow
source zone of the aquifer for which a
draft or final EIS is submitted which
may have an impact on ground water
quality and which involve Federal fi-
nancial assistance as defined in these
regulations.
(b) Upon receipt of a public petition,
the Regional Administrator shall de-
cide whether the project which is the
subject of the petition should be re-
viewed under section 1424(e).
(c) The Regional Administrator may
decide to review a project upon his own
motion.
(d) In determining whether to review
a project upon receipt of a public peti-
tion or upon his own motion, the Re-
gional Administrator shall consider
whether the project is likely to di-
rectly or indirectly cause contamina-
tion of the aquifer through its recharge
840
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Environmental Protection Agency
§149.109
zone, taking into account any factors
he deems relevant, including:
(1) The location of the project, and
(2) The nature of the project.
(e) In determining whether to review
a project upon receipt of a public peti-
tion or upon his own motion, the Re-
gional Administrator may consult
with, or request information from, the
Federal agency to which the project
application has been made, the appli-
cant seeking Federal assistance, appro-
priate State and local agencies, and
other appropriate persons or entities.
(f) In determining whether to review
a project which is the subject of a pub-
lic petition, the Regional Adminis-
trator may request such additional in-
formation from the petitioner as he
deems necessary.
§ 149.106 Notice of review.
(a) Notice to Federal agency. If the Re-
gional Administrator decides upon re-
ceipt of a public petition or upon his
own motion to review a project under
section 1424(e), he shall give written
notification of the decision to the Fed-
eral agency from which financial as-
sistance is sought. The notification
shall include a description and identi-
fication of the project.
(b) Notice to public. When the Re-
gional Administrator undertakes to re-
view a project pursuant to §149.13
above, he shall provide public notice of
project review by such means as he
deems appropriate. The notice shall set
forth the availability for public review
of all data and information available,
and shall solicit comments, data and
information with respect to the deter-
mination of impact under section
1424(e). The period for public comment
shall be 30 days after public notice un-
less the Regional Administrator ex-
tends the period at his discretion or a
public hearing is held under §149.16.
§ 149.107 Request for information.
In reviewing a project under section
1424(e), the Regional Administrator
may request any additional informa-
tion from the funding Federal agency
which is pertinent to reaching a deci-
sion. If full evaluation of the ground-
water impact of a project has not been
submitted in accordance with the agen-
cy's NEPA procedures, the Regional
Administrator may specifically request
that the Federal agency submit a
groundwater impact evaluation of
whether the proposed project may con-
taminate the aquifer through its re-
charge zone so as to create a signifi-
cant hazard to public health.
§149.108 Public hearing.
If there is significant public interest,
the Regional Administrator may hold a
public hearing with respect to any
project or projects to be reviewed if he
finds that such a hearing is necessary
and would be helpful in clarifying the
issues. Public hearings held under this
section should be coordinated, if pos-
sible, with other Federal public hear-
ings held pursuant to applicable laws
and regulations. Any such hearing
shall be conducted by the Regional Ad-
ministrator or designee in an informal,
orderly and expeditious manner. Where
appropriate, limits may be placed upon
the time allowed for oral statements,
and statements may be required to be
submitted in writing. The record will
be held open for further public com-
ment for seven (7) days following the
close of the public hearing.
§ 149,109 Decision under section
1424(e).
(a) As soon as practicable after the
submission of public comments under
section 1424(e) and information re-
quested by the Environmental Protec-
tion Agency from the originating Fed-
eral agency, on the basis of such infor-
mation as is available to him, the Re-
gional Administrator shall review the
project taking all relevant factors into
account including:
(1) The extent of possible public
health hazard presented by the project;
(2) Planning, design, construction,
operation, maintenance and moni-
toring measures included in the project
which would prevent or mitigate the
possible health hazard;
(3) The extent and effectiveness of
State or local control over possible
contaminant releases to the aquifer;
(4) The cumulative and secondary im-
pacts of the proposed project; and
(5) The expected environmental bene-
fits of the proposed project.
841
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§149.110
40 CFR Ch. I (7-1-04 Edition)
(b) After reviewing the available in-
formation, the Regional Administrator
shall:
(1) Determine that the risk of con-
tamination of the aquifer through the
recharge zone so as to create a signifi-
cant hazard to public health is not suf-
ficiently great so as to prevent com-
mitment of Federal funding to the
project; or
(2) Forward the information to the
Administrator with his recommenda-
tion that the project may contaminate
the aquifer through the recharge zone
so as to create a significant hazard to
public health.
(c) After receiving the available in-
formation forwarded by the Regional
Administrator, the Administrator
shall:
(1) Determine that the risk of con-
tamination of the aquifer through the
recharge zone so as to create a signifi-
cant hazard to public health is not suf-
ficiently great so as to prevent com-
mitment of Federal funding to the
project; or
(2) Determine that the project may
contaminate the aquifer through the
recharge zone so as to create a signifi-
cant hazard to public health.
(d) Notice of any decisions by the Re-
gional Administrator under paragraph
(b)(l) of this section or by the Adminis-
trator under paragraphs (c)(l) and (2) of
this section to prevent a commitment
of Federal funding shall be published in
the FEDERAL REGISTER. Such notices
shall include a description of the
propsed project, and a statement of de-
cision with an accompanying state-
ment of facts and reasons.
§149.110 Rcsubraittal of redesigned
projects.
If a project is redesigned in response
to EPA's objections, the applicant for
Federal financial assistance or the
grantor agency may file a petition with
the Regional Administrator for with-
drawal of the determination that the
project may contaminate the aquifer
through the recharge zone so as to cre-
ate a significant hazard to public
health. Any such petition shall dem-
onstrate how the project has been rede-
signed so as to justify the withdrawal
of EPA's objections. If appropriate, the
Regional Administrator may request
public comments or hold an informal
public hearing to consider the petition.
After review of pertinent information,
the Regional Administrator shall ei-
ther deny the petition or recommend
to the Administrator that the initial
determination that a project may con-
taminate the aquifer be vacated. Upon
receipt of a recommendation from the
Regional Administrator that a deter-
mination be vacated, the Adminis-
trator shall either deny the petition or
order that the initial determination be
vacated. The final decision regarding a
petition shall be published in the FED-
ERAL REGISTER with an accompanying
statement of reasons.
§149.111
ects.
Funding to redesigned proj-
After publication of a decision that a
proposed project may contaminate a
sole or principal source aquifer in a
designated area through its recharge
zone so as to create a significant haz-
ard to public health, a commitment for
Federal financial assistance may be en-
tered into, if authorized under another
provision of law, to plan or redesign
such project to assure that it will not
so contaminate the aquifer.
842
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FINDING AIDS
A list of CFR titles, subtitles, chapters, subchapters and parts and an alphabet-
ical list of agencies publishing in the CPB are included in the OPR Index and
Finding Aids volume to the Code of Federal Regulations which is published sepa-
rately and revised annually.
Material Approved for Incorporation by Reference
Table of CFR Titles and Chapters
Alphabetical List of Agencies Appearing in the CFR
List of CFR Sections Affected
843
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-------
Material Approved for Incorporation by Reference
(Revised as of July 1, 2004)
The Director of the Federal Register has approved under 5 U.S.C. 552(a) and
1 CFR Part 51 the incorporation by reference of the following publications. This
list contains only those incorporations by reference effective as of the revision
date of this volume. Incorporations by reference found within a regulation are
effective upon the effective date of that regulation. For more information on
incorporation by reference, see the preliminary pages of this volume,
40 CFR (PARTS 136 TO 149)
ENVIRONMENTAL PROTECTION AGENCY
40 CFR
American National Standards Institute
25 West 43rd Street, Fourth floor, New York, NY 10036; Telephone:
(212) 642^900
American National Standard on Photographic Processing Effluents, 136.3(a) Table IB,
April 2,1975. Note 9
American Public Health Association
1015 Fifteenth Street NW., Washington, DC 20005; Telephone: (202)
777-APHA
Standard Methods for the Examination of Water and Wastewater,
Joint Editorial Board, American Public Health Association, Amer-
ican Waterworks Association, and Water Environment Control
Federation:
20th Edition, 1998 , 136.3, Table 1A,
Note 4. Tables IB,
1C, ID, IE
19th Edition, 1995 136,3; Table 1A,
Note 4; Tables IB,
1C, ID, IE
18th Edition, 1992 136.3, Tables IA,
Note 4; IB, 1C, ID,
IE
15th Edition, 1980 136.3(a) Table IB,
Note 30; Table ID
14th Edition, 1975 136.3(a) Table IB,
Notes 17 and 27
Selected Analytical Methods Approved and Cited by the United States 136.3(a) Table IB,
Environmental Protection Agency, Supplement to the 15th Edition Note 10; Table 1C,
of Standard Methods for the Examination of Water and Wastewater, Note 6; Table ID,
1981. Note 6
American Society for Microbiology
1752 N Street, NW, Washington, DC 20036
Brenner, et al.: New Medium for the Simultaneous Detection of Total 136.3
Coliforms and Escherichia coli in Water. Appl. Environ Mlcrobial,
59:3534-3544, 1993.
American Society for Testing and Materials
100 Barr Harbor Drive, West Conshohocken, PA 19428-2959; Tele-
phone: (610) 832-9585, FAX: (610) 832-9555
845
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Title 40—Protection of Environment
1C, ID, and IE
136,3, Tables IB, 1C,
ID, and IE
136.3
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Annual Book of ASTM Standards—Water, Section 11, Volumes 11,01 136.3(a) Tables IB,
and 11.02, 1993.
Annual Book of ASTM Standards, Water and Environmental Tech-
nology, Section 11, Volumes 11.01 and 11.02, 1994, 1996, and
1999.
Annual Book of ASTM Standards, Water and Environmental Tech-
nology, Volume 11.02, 2002 edition.
AOAC International (Association of Official Analytical Chemists)
481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland
20877-2417
Official Methods of Analysis, 16th Edition, Volume 1, Chapter 17, 138.3
Method 991.15.
Bran & Luebbe Analyzing Technologies, Inc.
Elmsford, NY 10523
Hydrogen Ion (pH) Automated Electrode Method, Industrial Method
Number 378-75WA, October 1976, Bran & Luebbe (Techicon) Auto
Analyzer II.
CEM Corporation
P.O. Box 200, Matthews, North Carolina 28106-0200
Closed Vessel Microwave Digestion of Wastewater Samples for Deter-
mination of Metals, April 16,1992.
Fisons Instruments, Inc
32 Commerce Center, Cherry Hill Drive, Danvers, MA 01923
Direct Current Plasma (DCP) Optical Emission Spectrometric Method
for Trace Elemental Analysis of Water and Wastes, Method
AES0029,1986, revised 1991.
Hach Company
100 Dayton Avenue, Ames, Iowa 50010
m-ColiBlue24® test: "Total Coliforms and E. coli," Revision 2, 1999
1, 10—Phenanthroline Method Using FerroVer Iron Reagent for Water,
Hach Method 8008, 1980.
Bicinchoninate Method for Copper, Method 8506, Hach Handbook
of Water Analysis, 1979,
Chemical Oxygen Demand, Method 8000, Hach Handbook of Water
Analysis, 1979,
Nitrogen, Nitrite—-Low Range, Diazotization Method for Water and
Wastewater, Hach Method 8507, 1979.
Periodate Oxidation Method for Manganese, Method 8034, Hach
Handbook for Water Analysis, 1979.
Zincon Method for Zinc, Method 8009, Hach Handbook for Water
Analysis, 1979.
IDEXX Laboratories, Inc.
One IDEXX Drive, Westbrook, Maine 04092
Colilert Method®, 2002
Colilert-18® Method, 2002
Enterolert® Method, 2002
Quanti-Tray® Method, 2002
Quanti-tray/2002® Method , ,
Journal of Chromatography
Available from: Elsevier/North-Holland, Inc., Journal Information
Centre, 52 Vanderbilt Avenue, New York, NY 10164
136.3(a) Table IB,
Note 21
136.3(a) Table IB,
Note 36
136.3(a) Table IB,
Note 34
136.3
136.3(a)
Note
136.3(a)
Note
136.3(a)
Note
136.3(a)
Note
136.3(a)
Note
136.3(a)
Note
Table IB,
22
Table IB,
19
Table IB,
14
Table IB,
25
Table IB,
23
Table IB,
33
136.3
136.3
136.3
136.3
136.3
846
-------
136.3(a) Table IB,
Note 18
136.3
136.3
136.3
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Direct Determination of Elemental Phosphorous by Gas-Liquid Chro- 136.3(a) Table IB,
matography, by R.F. Addison and R.G. Ackman, Journal of Chroma- Note 28
tography, Volume 47, No. 3, pp. 421^26,1970.
National Council of the Paper Industry for Air and Stream Improvements, Inc.
260 Madison Avenue, New York, NY 10016
An Investigation of Improved Procedures for Measurement of Mill
Effluent and Receiving Water Color, NCASI Technical Bulletin No,
253, December 1971.
National Technical Information Service
5285 Port Royal Road, Springfield, Virginia 22161
Method OIA-1677, "Available Cyanide by Flow Injection, Ligand
Exchange, and Amperometry," PB99-132011, August 1999,.
Method 1631, Revision E, "Mercury in Water by Oxidation, Purge
and Trap, and Cold Vapor Atomic Fluorescence Spectrometry" Sep-
tember 2002, Office of Water, US EPA, (EPA-821-R-02-019)..
EPA-821-R-Q2/012"Methods for Measuring the Acute Toxicity of
Effluents and Receiving Waters to Freahwater and Marine Orga-
nisms," Fifth Edition, October 2002.
Oceanography International Corporation
512 West Loop, P.O. Box 2980, College Station, TX 77840
OIC Chemical Oxygen Demand Method, 1978 136.3(a) Table IB,
Note 13
ORION Research Incorporated
840 Memorial Dr., Cambridge, MA 02138
ORION Research Instruction Manual, Residual Chlorine Electrode
Model 97-70, 1977.
Perstorp Analytical Corporation
1256 Stockton St., Helena, CA 94574
Nitrogen, Total Kjeldahl, Method PAl-DkOl, (Block Digestion, Steam
Distillation, Tritrimetric Detection), Revised December 22, 1994
Nitrogen, Total Kjeldahl, Method PAl-Dk02, (Block Digestion, Steam
Distillation, Colorimetric Detection), Revised December 22, 1994
Nitrogen, Total Kjeldahl, Method PAl-Dk03, (Block Digestion, Steam
Distillation, Automated FLA Gas Diffusion), Revised December 22,
1994.
Technicon Industrial Systems
Tarrytown, New York 10591
Ammonia, Automated Electrode Method, Industrial Method Number
379-75WE, dated February 19, 1976, Technicon Auto Analyzer
II.
U.S. Environmental Protection Agency, ORD publications, CERI
Cincinnati, OH 45268
Methods for Benadine, Chlorinated Organic Compounds,
Pentachlorophenol and Pesticides in Water and Wastewater, U.S.
Environmental Protection Agency, 1978.
EPA-600/4-79-020: "Methods for Chemical Analysis of Water and
Wastes," U.S. Environmental Protection Agency, March 1979, or
"Methods for Chemical Analysis of Water and Wastes," U.S. Envi-
ronmental Protection Agency, EPA-600/4-79-020, Revised March
1983.
EPA-821-R-01-025: Method 1623: "Cryptosporidium and Giardia in
Water by Filtration/IMS/FA," U.S. Environmental Protection Agen-
cy, April 2001.
136.3(a) Table IB,
Note 16
136.3(a), Table IB,
Note 39
136.3(a), Table IB,
Note 40
136.3(a), Table IB,
Note 41
136.3(a) Table IB,
Note 7
136.3(a) Table 1C,
Note 3; Table ID,
Note 3
136.3(a) Table IB,
Notes 1 and 4
136.3
847
-------
Title 40—Protection of Environment
40 CFR (PAETS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
EPA-821-R-Q1-026: Method 1622: "Cryptosporidium in Water by
Filtration/IMS/FA," U.S. Environmental Protection Agency, April
2001.
EPA-821-R-02-020: Method 1103.1: "Escherichia coli (E coli) in
Water by Membrane Filtration Using Membrane-Thermotolerant
Escherichia coli Agar (mTEC), September 2002.
EPA-821-R-02-021: Method 1106.1: "Enterococci in Water by Mem-
brane Filtration Using Membrane-Enterococcus-Esculin Iron Agar
(mE-EIA), September 2002.
EPA-821-R-02-022: Method 1600: "Enterococci in Water by Mem-
brane Filtration Using Membrane-Enterococcus-Indoxyl-p-D-Gluco-
side Agar (mEI), September 2002.
EPA-821-R-02-023: Method 1603: "Escherichia Coli (E. coli) in Water
by Membrane Filtration Using Modified Membrane-thermotolerant
Escherichia-coli Agar (Modified mTEC), September 2002,
EPA-821-R-02-024: Method 1604: Total coliforms and Escherichia
coli (E, coli) in Water by Membrane Filtration Using a Simultaneous
Detection Technique (MI Medium), September 2002.
EPA-600/1-80-031: Cabelli, V.J., "Health Effects Criteria for Marine
Recreational Waters" August 1983.
EPA-600/1-84-004: Dufour, A.P., "Health Effects Criteria for Fresh
Recreational Waters" August 1984.
Microbiological Methods for Monitoring the Environment, Water and
Wastes, U.S. Environmental Protection Agency, EPA-600/8-78-017,
1978.
Organochlorine Pesticides and PCBs in Wastewater Using Empore
TM Disk, Revised October 28, 1994.
Prescribed Procedures for Measurement of Radioactivity in Drinking
Water, U.S. Environmental Protection Agency, EPA-600/4-80-032,
1980.
U.S. Environmental Protection Agency, Office of Water Resource Center
Washington, DC 20460
Short-Term Methods for Estimating the Chronic Toxieity of Effluents 136.3
and Receiving Waters to Freshwater Organisms, Fourth Edition,
October 2002 (EPA 821/R-02/013).
Short-Term Methods for Estimating the Chronic Toxicity of Effluents 136.3
and Receiving Waters to Marine and Estuarine Organisms, Third
Edition, October 2002 (EPA 821/R-02/014).
Method 1664, Revision A, n-Hexane Extractable Material (HEM; Oil 136.3
and Grease) and Silica Gel Treated n-Hexane Extractable Material
(SGT-HEM; Non-polar material) by Extraction and Gravimetry, Feb-
ruary 1999 (EPA-821-R-98-002).
The following standard is available from: National Technical Infor-
mation Service, 5285 Port Royal Road, Springfield, VA 22161
EPA-821-B-98-016, Analytical Methods for the Determination of 136.3
Pollutants in Pharmaceutical Manufacturing Industry Wastewater,
July 1998.
EPA Method 526: Determination of Selected Semivolatile Organic 141.40
Compounds in Drinking Water by Solid Phase Extraction and Cap-
illary Column Gas Chromatography/Mass Spectrometry (CC/MS),
Revision 1.0, June 2000.
U.S. Geological Survey
Denver Federal Center, Box 25425, Denver, CO 80225
40 CFR
136.3
136.3
136.3
136.3
136.3
136.3
136.3
136.3
136.3(a) Table IA,
Note 3
136.3(b)(33)
136.3(a) Table IE,
Note 1
848
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
Methods for Collection and Analysis of Aquatic Biological and Micro-
biological Samples, edited by Britton, L.J, and P,E, Greason, Tech-
niques of Water-Resources Investigations of the U.S, Geological
Survey, Book 5, Chapter Al (1989).
Methods for Determination of Inorganic Substances in Water and
Fluvial Sediments, N.W. Skougstad and others, editors, Techniques
of Water-Resources Investigations of the U.S, Geological Survey,
Book 5, Chapter Al (1979).
Methods for Determination of Inorganic Substances in Water and
Fluvial Sediments, M.J. Fishman and Linda C. Friedman, Tech-
niques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5, Chapter Al (1989),
Methods for the Determination of Organic Substances in Water and
Fluvial Sediments, Wershaw, R.L., et al, Techniques of Water-
Resources Investigations of the U.S. Geological Survey, Book 5,
Chapter A3 (1987).
Selected Methods of the U.S. Geological Survey of Analysis of
Wastewaters, by M.J. Fishman and Eugene Brown; U.S. Geological
Survey Open File Report 76-77 (1976).
Water Temperature—Influential Factors, Field Measurement and Data
Presentation, by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot, Tech-
niques of Water-Resources Investigations of the U.S. Geological
Survey, Book 1, Chapter Dl, 1975,
Open File Report 00-170: Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory—Determination of Am-
monium Plus Organic Nitrogen by a Kjeldahl Digestion Method
and an Automated Photometric Finish that Includes Digest Cleanup
by Gas Diffusion, 2000.
Open File Report 92-146: Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory—Determination of Total
Phosphorous by a Kjeldahl Digestion Method and an Automated
Colorimetric Finish that Includes Dialysis, 1992.
Open File Report 93-125: Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory—Determination of Inor-
ganic and Organic Constituents in Water and Fluvial Sediments,
1993.
Open File Report 93-449: Methods of Analysis by the U.S, Geological
Survey National Water Quality Laboratory—Determination of Chro-
mium in Water by Graphite Furnace Atomic Absorption
Spectrophotometry, 1993.
Open File Report 94-37: Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory—Determination of Tri-
azine and Other Nitrogen-Containing Compounds by Gas Chroma-
tography, 1994.
Open File Report 97-198: Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory—Determination of Mo-
lybdenum in Water by Graphite Furnace Atomic Absorption
Spectrophotometry, 1997.
Open File Report 98-165: Methods of Analysis by the U.S, Geological
Survey National Water Quality Laboratory—Determination of Ele-
ments in Whole-Water Digests Using Inductively Coupled Plasma—
Optical Emission Spectrometry and Inductively Coupled Plasma-
Mass Spectrometry, 1998.
40 CFR
136,3(a) Table LA
136.3(a) Table IB,
Note 8
136.3(a) Table IB,
Note 2
136.3(a) Table IB,
Note 24; Table ID,
Note 4
136,3(a) Table IE,
Note 2
136.3(a) Table IB,
Note 32
136.3
136,3
136.3
136.3
136.3
136.3
136.3
849
-------
Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Open File Report 98-639: Methods of Analysis by the U.S. Geological 136.3
Survey National Water Quality Laboratory—Determination of Ar-
senic and Selenium in Water and Sediment by Graphite Furnace-
Atomic Absorption Spectrometry, 1999,
40 CFR (PART 141); WATER PROGRAMS
AOAC International (Association of Official Analytical Chemists)
First Union National Bank Lockbox, P.O. Box 75198, Baltimore,
MD 21275-5198
Official Methods of Analysis of the Association of Official Analytical 141,40
Chemists, Volume 1,16th Edition, 4th Revision (1998).
American Public Health Association
1015 Fifteenth Street, NW, Washington DC 20005
Standard Methods for the Examination of Water and Waste Water, 141.21; 141.23;
18th Edition, 1992; 19th Edition, 1995; 20th Edition, 1998. 141.24; 141,25;
141,40; 141.74;
143,4
Methods 6200 B, 2130 B, 2550, 4500-CI, D, E, F, G, H, I; 4500- 141.40
CIO2D, E, 4500-H*B, and 4500-03 B, Standard Methods for the
Examination of Water and Waste Water, 20th Edition, 1998.
Method 3125, "Metals by Inductively Coupled Plasma/Mass Spectrom- 141.25
etry" as published in "Standard Methods for the Examination of
Water and Waste Water," 20th Edition, 1998.
American Society for Testing and Materials
100 Barr Harbor Drive, West Conshohocken, PA 19428-2959; Tele-
phone; (610) 832-9585, FAX: (610) 832-9555
ASTM D 5673-03 Standard Test Method for Elements in Water by 141,25
Inductively Coupled Plasma-Mass Spectrometry,
Annual Book of ASTM Standards—Water and Environment Tech- 141.24
nology—Section 11, Volume 11,02,1999,
American Water Works Association, Water Pollution Control Federation
Available from American Public Health Association, 1015 Fifteenth
Street NW,, Washington, DC 20005; Telephone: (202) 777-APHA
Selected Analytical Methods Approved and Cited by the United States
Environmental Protection Agency, Supplement to the 16th Edition
of Standards Methods for the Examination of Water and Wastewater,
1985:
Methods 908C pp. 878-880; 908D pp. 880-882; 909C pp. 896- 141.74(a)
898; 908A pp. 872-876; 908B pp. 876-878; 908D pp. 880-882;
909A pp. 887-894; 909B pp. 894-896; 907A pp. 864-866; 214A
pp. 134-136; 408C pp. 303-306; 408D pp. 306-309; 408E pp. 309-
310; 408F pp. 310-313; 410B pp. 322-323; 410C pp. 323-324;
212 pp. 126-127; 423 pp. 429-437.
Methods 908, 908A, and 908B pp. 870-878; Method 908E pp. 141.21{f)
882-886; Methods 909, 909A, and 909B pp. 886-896; Nutrient
Agar p. 874; EC Medium p. 879.
Standard Methods for the Examination of Water and Wastewater,
18th Edition Supplement, 1994:
Standard Methods for the Examination of Water and Wastewater, 141.21; 141.23;
18th Edition, 1992. 141.24; 141.40;
141.74; 143.4
Method 6610, Carbamate Pesticides Method 141,24; 141.40
850
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Standard Methods for the Examination of Water and Waste Water, 141.21; 141.23;
19th Edition, 1995. 141.24; 141.40;
141.74; 141.142;
143.4
Standard Methods for the Examination of Water and Wastewater, 141.31
19th Edition, 1995; Supplement, 1996.
Methods 6200 B, 2130 B, 2550; 4500-CI, D, E, F, G, H. I; 4500- 141.40
CIO2D, E, 4500-H+B, and 4500-O3 B, Standard Methods for the
Examination of Water and Waste Water, 20th Edition, 1998,
American Society for Testing and Materials
100 Barr Harbor Drive, West Conshohocken, PA 19428-2959; Tele-
phone; (610) 832-9585, FAX: (610) 832-9555
ASTM D 511-88 Standard Test Methods for Calcium and Magnesium 141.89
in Water.
ASTM D 515-88 Standard Test Methods for Phosphorus in Water 141.89
ASTM D 859-88 Standard Test Method for Silica in Water 141.89
ASTM D 1067-88 Standard Test Methods for Acidity or Alkalinity 141.89
of Water.
ASTM D 1125-82 Standard Test Methods for Electrical Conductivity 141.89
and Resistivity of Water.
ASTM D 1293-84 Standard Test Methods for pH of Water 141.89
ASTM D 1688-90 Standard Test Methods for Copper in Water 141,89
ASTM D 2459-75 Gamma Spectrometry in Water 141.25(a)(6)
ASTM D 2907-75 Micro-quantities of Uranium in Water by 141.25(a)(7)
Flourometry.
ASTM D 3559-85 Standard Test Methods for Lead in Water 141,89
ASTM D 4327-88 Standard Test Method for Anions in Water by 141.89
Ion Chromatography.
AnnualBookof ASTM Standards, 1993, Volume 11 141.23; 143.4
Annual Book of ASTM Standards, Water and Environmental Tech- 141.23; 141.25;
nology, Section 11, Volumes 11.01 and 11.02,1999. 143.4
Annual Book of ASTM Standards, 1994 and 1996, Volume 11.01 141.40
Annual Book of ASTM Standards, 1996 and 1998, Volume 11.02 141.40
ASTM D 1293-95, Standard Test Methods for pH of Water 141.40
ASTM D 5317-93, Standard Test Method for Determination of 141.40
Chlorinated Organic Acid Compounds in Water by Gas Chroma-
tography with an Electron Capture Detector.
ASTM D 5790-95, Standard Test Method for Measurement of 141.40
Purgeable Organic Compounds in Water by Capillary Column Gas
Chromatography-Mass Spectrometry.
ASTM D 5812-96, Standard Test Method for Determination of 141,40
Qrganochlorine Pesticides in Water by Capillary Column Gas Chro-
matography.
Annual Book of ASTM Standards 1994; Vol. 11,01, 1994 edition 141.31
and 1996 edition.
AnnualBookof ASTM Standards, 1994 and 1996, Vol. 11,01 141,23; 141.40;
143.4
Annual Book of ASTM Standards, 1994 and 1996, Vol. 11:02 141.24; 143,4
Annual Book of ASTM Standards, 1996 and 1998, Vol. 11.02 ., , 141.40
Annual Book of ASTM Standards, 1994, Vol. 11:02 141.25
American Water Works Association Research Foundation
Customer Service, 6666 West Qumey Avenue, Denver, CO 80235;
Telephone: 303-794-7711
851
-------
Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Guidance Manual for Compliance with the Filtration and Disinfection 141,142
Requirements for Public Water Systems Using Surface Water
Sources, 1991, Appendices C and O.
Methods for Chemical Analysis of Water and Wastes, EPA Environ- 141.89
mental Monitoring and Support Laboratory, Cincinnati, OH (EPA-
600/4-79-020], Revised March 1983, Procedures 239.2, 220.2,
220.1, 150.1, 150.2, 120.1, 215,2, 215.1, 310.1, 365,1, 365,3, 365.2,
and 370.1 located at pp. 239.2-1 through 239,2-2 and metals -1
through metals-19, 220.2-1 through 220.2-2 and metals-1 through
metals-19, 220,1-1 through 220.1-2 and metals-1 through metals-
19, 150.1-1 through 150.1-3, 150.2-1 through 150.2-3, 120.1-1
through 120.1-3, 215.2-1 through 215.2-3, 215.1-1 through 215.1-
2, 310.1-1 through 310.1-3, 365.1-1 through 365.1-9, 365.3-1
through 365,3-4, 365,2-1 through 365.2-6, and 370,1-1 through
370.1-5.
National Field Evaluation of a Defined Substrate Method for the 141.21(a); 141.74(a)
Simultaneous Enumeration of Total Coliforms and Escherichia coli
from Drinking Water: Comparison with the Standard Multiple Tube
Fermentation Method, Stephen C. Edberg, Martin J. Allen, Darwell
B. Smith, and the National Collaborative Study, which appears
in Applied and Environmental Microbiology, Volume 54, pages
1595-1601, June 1988, as amended under Erratum, Applied and
Environmental Microbiology, Volume 54, page 3197.
National Field Evaluation of a Defined Substrate Method for the 141.21(f)
Simultaneous Detection of Total Coliforms and Escherichia coli
from Drinking Water: Comparison with Presence-Absence Tech-
niques, Stephen C. Edberg, Martin J. Allen, Darwell B. Smith,
and the National Collaborative Study, which appears in Applied
and Environmental Microbiology, Volume 55, No. 4 pages 1003—
1008, April 1989, published by the American Society for Microbi-
ology,
New Medium for the Simultaneous Detection of Total coliforms and 141.21; 141.74
Escherichia coli in Water, Kristen P. Brenner, Clifford C. Rankin,
Yvette R, Roybal, Gerald N. Stelma, Jr., Pasquale V. Scarpino,
and Alfred P, Dufour, which appears in Applied and Environmental
Microbiology, Vol. 59, No. 11, pages 3534-3544, November 1993,
published by the American Society for Microbiology,
Standard Methods for the Examination of Water and Wastewater, 141.89
17th Edition, American Public Health Association, American Water
Works Association, Water Pollution Control Federation, 1989, Pro-
cedures 3113, 3111-B, 3120, 4500-H+, 2510, 3500-Ca-D, 3120,
2320, 4500-P-F, 4500-P-E, 4110, 4500-Si-D, 4500-Si-E, 4500-
Si-F, and 2500 located at pp. 3-32 through 3-43, 3-20 through
3-23, 3-53 through 3-63, 4-94 through 4-102, 2-57 through 2-
61, 3-85 through 3-87, 2-35 through 2-39, 4-178 through 4-181,
4-177 through 4-178, 4-2 through 4-6, 4-184 through 4-187, 4-
188 through 4-191, and 2-80 through 2-81.
Analytical Technology, Inc. Orion
529 Main St., Boston, MA 02129
Analytical Technology, Inc. Orion, Technical Bulletin 601, Standard 141.23
Method of Test for Nitrate in Drinking Water, PN 221890-001,
dated July 1994.
AOAC International (Association of Official Analytical Chemist)
First Union National Bank Lockbox, P.O. Box 75198, Baltimore,
MD 21275-5198
852
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Official Methods of Analysis of the Association of Official Analytical 141,40
Chemists, Vol. I (16th Edition, 4th Revision, 1998).
Charm Sciences, Inc.
36 Franklin Street, Maiden, MD 02148
Ecolite Test, "Presence/Absence for Colifornis and E.coli in Water" 141.21
dated December 21,1997.
CPI International, Inc.
5580 Skylane Boulevard, Santa Rosa, California 95403
"Colitag Product as a Test for Detection and Identification of Colifornis I41.21(f)(3)
and Escherichia Coli Bacteria in Drinking Water and Source Water
as Required in National Primary Drinking Water Regulations," Au-
gust 2001.
Department of Commerce
National Institute of Standard and Technology (formerly National
Bureau of Standards), Washington, DC 20234
Handbook No. 69, Permissible Body Burdens and Maximum Permis- 141.16(b); 141.66
sible Concentrations of Radionuclides in Air or Water for Occupa-
tional Exposure, August 1963.
Department of Commerce
National Technical Information Service, 5285 Port Royal Rd.,
Springfield, VA 22161; Telephone: (703) 487-4650, FAX: (703)
487-4142
Interim Radiochemical Methodology for Drinking Water, EPA 600/ 141.25
4-75-008 (revised), March 1976,
Prescribed Procedures for Measurement of Radioactivity in Drinking 141.25
Water, EPA 600/4-80-032, August 1980,
Method 200.8: "Determination of Trace Elements in Waters and 141.25
Wastes by Inductively Coupled Plasma-Mass Spectrometry" Revi-
sion 5,4, as published in "Methods for the Determination of Metals
in Environmental Samples—Supplement 1," EPA-600/R-94-111,
May 1994.
Radiochemical Analytical Procedures for Analysis of Environmental 141.25
Samples, March 1979,
Radiochemistry Procedures Manual, EPA 520/5-84-006, December 141.25
1987.
Standard Methods for the Examination of Water and Wastewater, 141.25
13th, 17th, 18th, and 19th Editions, 1971, 1989, 1992, and 1995.
Technical Notes on Drinking Water Methods, EPA-600/R-94-173, 141.40
October 1994.
Methods for the Determination of Inorganic Substances in Environ- 141.40
mental Samples, EPA-600/R-93-100, August 1993.
EPA Method 515,3: Determination of Chlorinated Acids in Drinking 141.40
Water by Liquid-Liquid Extraction, Derivatization and Gas Chroma-
tography with Electron Capture Detection, Revision 1,0, July 1996.
EPA Method 515.4: Determination of Chlorinated Acids in Drinking 141.24; 141.40
Water by Liquid-Liquid Microextraction, Derivatization and Fas
Gas Chromatography with Electron Capture Detection, Revision
1.0, April 2000, EPA 815/B-00/001.
EPA Method 528: Determination of Phenols in Drinking Water by 141.40
Solid Phase Extraction and Capillary Column Gas Chromatography/
Mass Speetrometry (GC/MS), Revision 1.0, April 2000.
EPA Method 532: Determination of Phenylurea Compounds in Drink- 141.40
ing Water by Solid Phase Extraction and High-Performance Liquid
Chromatography with UV Detection, Revision 1,0, June 2000,
853
-------
Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
EPA Method 1605: Aeromonas in Finished Water by Membrane Filtra- 141.40
tion Using Ampicillin-Dextrin Agar with Vancomvcin (ADA-V);
October 2001, EPA 821*01-034.
EPA Method 531,2: Measurement of n-Methylcarbamoyloximes and 141.24
n-Methylcarbamates in Water by Direct Aqueous Injection HPLC
with Postcolurnn Derivatization (EPA 815-B-01-002), Revision 1.0,
September 2001.
Method AG-B25: Atazine in Drinking Water by Immunoassay, Feb- 141.24
ruary 2001.
EPA-821-B-01-009, Method Kelada-01: Kelada Automated Test Meth- 141.23
ods for Total Cyanide, Acid Dissociable Cyanide, and Tblocyanate,
Revision 1.2, August 2001.
Hach Method 10133: Determination of Turbidity by Laser 141.74
Nephelonietry, Revision 2.0, January 7, 2000.
Chromocult Coliform Agar Presence/Absence Membrane Filter Test 141.21
Method for Detection and Identification of Coliform Bacteria and
Escherichla Coli in Finished Waters, Version 1.0, November 2000.
Readycult Coliforms 100 Presence/Absence Test for Detection and 141,21
Identification of Coliform Bacteria and Escherichla Coli in Finished
Waters, Version 1.0, November 2000.
IDEXX SimPlate HPC Test Method for Heterotrophs in Water, Novem- 141.74
her 29, 2000.
QuickChem Method 10-204-00-1-X: Digestion and Distillation of Total 141.24
Cyanide in Drinking and Wastewaters using MICRO DIST and Deter-
mination of Cyanide by Flow Injection Analysis, Revision 2.1,
November 30, 2000.
U.S. Environmental Protection Agency, NERL 28 W. Martin Luther King Drive,
Cincinnati Ohio 45268
Method 150.1 Electrometric (1978 and 1982) 141.40
Method 150.2 pH, Continuous Monitoring, Electrometric (December 141.40
1982).
EPA Safe Drinking Water Hotline
800-426-4791 (Hours are Monday through Friday, excluding Federal
holidays, from 9:00 am to 5:30 pm Eastern Standard Time.)
Department of Energy
Environmental Measurements Laboratory, 376 Hudson St., New
York, NY 10014-3621
EML Procedures Manual, 27th Edition, Vol. 1,1990 141.25
EML Procedures Manual, HASL-300, Volume 1: Gamma Radioassay, 141.25
28th Edition, February 1997.
EML Procedures Manual, HASL-300, Volume 1: Radium-226 in Tap 141.25
Water, Urine, and Feces, 28th Edition, February 1997,
EML Procedures Manual, HASL-300, Volume II: Strontium-89, 28th 141.25
Edition, February 1997.
EML Procedures Manual, HASL-300, Volume II: Strontium-90, 28th 141.25
Edition, February 1997.
EML Procedures Manual, HASL-300, Volume I: Isotopic Uranium 141.25
in Biological and Environmental Materials, 28th Edition, February
1997.
EML Procedures Manual, HASL-300, Volume II: Uranium in Biologi- 141.25
cal and Environmental Materials, 28th Edition, February 1997,
HASL Procedures Manual HASL—300,1978 141.25(b)(2)
854
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Environmental Protection Agency
Environmental Monitoring & Support Laboratory (EMSL), 25 W.
St. Glair St., Cincinnati, OH 45268
Interim Radiochemical Methodology for Drinking Water, EMSL, EPA- 141.25(a)
600/4-75-008,
Microbiological Methods for Monitoring the Environment, Water and 141,21(f)
Wastes, U.S. EPA, Environmental Monitoring and Support Labora-
tory (EPA-600/8-78-Q17), December 1978; Part III, Section B.2.1—
2.6, pp. 108-112; Part III, Section B.4.1—4.6.4, pp. 114-118.
Office of Solid Waste and Emergency Response, Waste Characteriza-
tion Branch, Washington, DC 20460
The above standards are also available at the Office of Drinking
Water, Criteria and Standards Division, Environmental Protection
Agency, 401 M St., SW., Washington, DC 20460
NERL, 26 W. Martin Luther King Drive, Cincinnati, OH 45268
Method 150.1 Electrometric (1978 and 1982 141.40
Method 151.2pH, Continuous Monitoring, Electrometric (December 141.40
1982).
Method 549.2, Determination of Disquat and Paraquat in Drinking 141.24
Water by Liquid-Solid Extraction and High Performance Liquid
Chromatography with Ultraviolet Detection, Revision 1.0, EPA/815/
B-99/002, June 1997.
Method 515.3, Determination of Chlorinated Acids in Drinking Water 141.24
by Liquid-Liquid Extraction, Derivatization and Gas Chroma-
tography with Electron Capture Detection, Revision 1,0, EPA 815/
B-99-001, July 1996.
Available from; National Technical Information Service, 5285 Port
Royal Road, Springfield, VA 22161
Method 300.1 Determination of Inorganic Anions in Drinking Water 141.31
by Ion Chromatography, Revision 1.0, 1997 (EPA/600/R-98/118).
Methods for the Determination of Organic Compounds in Drinking 141.31
Water, Supp. II, August 1992 (EPA 600/R-92-129).
Methods for the Determination of Organic Compounds in Drinking 141.31
Water, Supp. Ill, August 1995 (EPA 600/R-95-131).
Methods for Determination of Inorganic Substances in Environmental 141.31; 141.40;
Samples, August 1993 (EPA 600/R-93-100). 141.74; 143.4
Technical Notes on Drinking Water Methods, EPA-600/R-94-173, 141.40
October 1994.
Method 314.0, Determination of Perchlorate in Drinking Water Using 141.40
Ion Chromatography, EPA 815-B-99-003, Revision 1,0, November
1999.
Environmental Protection Agency, National Exposure Research Lab-
oratory (NERL) 26 West Martin Luther King Drive Cincinnati, Ohio
45268
Determination of Ozone in Water by the Indigo Method; A Submitted 141.74(a)
Standard Method, H. Bader and J. Hoigne; Ozone Science and
Engineering, Volume 4, pp. 169-176, 1982.
Great Lakes Instruments, Inc.
8855 North 55th Street, Milwaukee, WI 53223
GLI Method 2, Turbidity, dated November 2, 1992 141.40; 141,74
Hatch Company
100 Dayton Avenue, Ames, IA 50010
Method No. 10029, m-ColiBlue24 Broth, Total Coliforma and E.coli 141,21
Membrane Filteration Method, Revision 2, dated August 17, 1999.
855
203-160 D-28
-------
Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Millipore Corporation
Technical Services Department, 80 Ashby Road, Bedford, MA 01730
Millipore Corporation, Method AN208, Colisure Presence/Absence 141.21
Test for Detection and Identification of Coliform Bacteria and Esch-
erichla colt in Drinking Water, dated February 28,1994.
Palintest, LTD
21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018
Method 1001, Lead in Drinking Water by Differential Pulse Anodic 141.23
Stripping Voltammetry, August 1999.
Radiological Sciences Institute Center for Laboratories and Research, New York State
Department of Health
Empire State Plaza, Albany, NY 12201
Determination of Ra-226 and Ra-228 (Ra-02), January, 1980 141.25
State of New Jersey Department of Environmental Protection, Division of Environmental
Quality, Bureau of Radiation and Inorganic Analytical Services
9 Ewing Street, Trenton, NJ 08625
Determination of Radium 228 in Drinking Water, August 1980 141.25
Technicon Industrial Systems, do Bran & Luebbe
1025 Busch Parkway, Buffalo Grove, IL 60089
Technicon Industrial Systems, Industrial Method No. 129-71W, Fluo- 141.23
ride In Water and Wastewater dated December 1972, and Method
No. 380-75WE, Fluoride in Water and Wastewater, dated February
1976.
U.S. Geological Survey, Department of the Interior
Books and Open-File Reports Section, Federal Center, Box 25425,
Denver, CO 80225
Methods for Determination of Inorganic Substances in Water and 141.89
Fluvial Sediments, 3rd edition, U.S. Department of Interior, U.S.
Geological Survey, 1989, Procedures 1-1030-85,1-1601-85,1-2601-
85, 1-2598-85, 1-1700-85, and 1-2700-85 located at pp. 55-56,
381-382, 383-385, 387-388, 415-416, and 417-419.
U.S. Geological Survey, Department of the Interior
USGL Information Services, Box 25286, Federal Center, Denver,
CO 80225-0425
Methods for Determination of Radioactive Substances in Water and 141.25
Fluvial Sediments, Chapter A5 in Book 5 of Techniques of Water-
Resources Investigations of the United States Geological Survey,
1977.
Techniques of Water Resources Investigation of the U.S. Geological 141.23
Survey, Book 5, Chapter A-I, 3rd edtion, Methods 1-1030-85; I-
1601-85; 1-2598-85; 1-1700-85; 1-2700-85; 1-3300-85.
Techniques of Water Resources Investigation of the U.S. Geological 143.4
Survey, Book 5, Chapter A-I, 3rd edition, Method 1-3720-85.
State Statutes and Regulations (PART 147): STATE UNDERGROUND INJECTOR
CONTROL PROGRAMS
Alabama; (1) Code of Alabama, section 9-17-1 through 9-17-109 147.50(a)
(Cumm, Supp, 1989); (2) State Oil and Gas Board of Alabama
Administrative Code, Oil and Gas Report 1 (supplemented through
May 1989), Rules and Regulations Governing the Conservation of
Oil and Gas in Alabama, and Oil and Gas Statutes of Alabama
with Oil and Gas in Alabama, and Oil and Gas Statutes of Alabama
with Oil and Gas Board Forms, 400-1-2, and 400-1-5-.04.
856
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
Alabama; (1) Alabama Water Pollution Control Act, Code of Alabama
1975, §§22-22-1 through 22-22-14 (1980 and Supp, 1983); (2)
Regulations, Policies and Procedures of the Alabama Water Im-
provement Commission, Title I (Regulations) (Rev, December 1980),
as amended May 17, 1982, to add Chapter 9, Underground Injection
Control Regulations (effective June 10, 1982), as amended April
6, 1983 (effective May 11, 1983).
Alabama: (1) Rule 400-4-1-.02, Definitions; Rule 400-4-5-.04, Pro-
tection of Underground Sources of Drinking Water during the Hy-
draulic Fracturing of Coal Beds.
Alaska: (1) Alaska Statutes, Alaska Oil and Gas Conservation Act,
Title 31, Sections 31.05,005 through 31.30.010 (1979 and Cumin,
Supp, 1984); (2) Alaska Statutes, Administrative Procedures Act,
Title 44, Sections 44.62,010 through 44,62,850 (1984); (3) Alaska
Administrative Code, Alaska Oil and Gas Conservation Commission,
20 AAC 25,005 through 20 AAC 25,570 (Supp. 1986).
Indiana: (1) Indiana Code, title 4, article 21.5, chapters 1 through
6 (1988); (2) West's Annotated Indiana Code, title 13, article 8,
chapters 1 through 15 (1990 and Cumm. Supp. 1990); (3) Indiana
Administrative Code, title 310, article 7, rules 1 through 3 (Cumm.
Supp, 1991),
Arkansas: (1) Arkansas Water and Air Pollution Control Act, Act
472 of 1949 as amended, Arkansas Statutes Annotated §§82-1901
through 82-1943 (1976); (2) Act 105 of 1939, Arkansas Statutes
Annotated §§53-101 through 53-130 (1971 and Supp. 1981); Act
937 of 1979, Arkansas Statutes Annotated §§53-1301 through 53-
1320 (Supp, 1981); Act 523 of 1981; (3) Arkansas Underground
Injection Control Code, Department of Pollution Control and Ecol-
ogy, promulgated January 22, 1982; (4) General Rule and Regula-
tions, Arkansas Oil and Gas Commission (Order No. 2-39, revised
July 1972); (5) Arkansas Hazardous Waste Management Code, De-
partment of Pollution Control and Ecology, promulgated August
21, 1981.
California: (1) California Public Resources Code, California Laws for
Conservation of Petroleum and Gas, Div. 3, Chapt. 1, sections
3000-3359 (1989); (2) California Administrative Code, Title 14,
section 1710 through 1724.10 (May 28, 1988).
Colorado: (1) Colorado Revised Statutes, 1989 replacement volume,
Section 34-60-101 through 34-60-123; (2) Colorado Revised Stat-
utes, 1989 replacement volume, Section 25-8-101 through 25-
8-612; (3) Rules and Regulations, Rules of Practice and Procedure,
and Oil and Gas Conservation Act (as amended), Department of
Natural Resources, Oil and Gas Conservation Commission of the
State of Colorado (revised July 1989); (4) Oil and Gas Conservation
Commission Revised Rules and Regulations in the 300, 400, 500,
and 600 series, effective March 20,1989.
Connecticut: (1) Connecticut General Statutes Annotated, Title 22a
(Environmental Protection), Chapter 439, Sections 22a-l through
22a-27 (1985 and Cumm. Supp. 1990); (2) Connecticut General
Statutes Annotated, Title 22a (Environmental Protection), Chapter
446K (1985 and Cumm. Supp. 1990).
40 CFR
147.51(a)
147,52(a)
147.100(a)
147.750
147.200(a)
147.250(a)
147.300(a)
147,350(a)
857
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Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Delaware: (1) Delaware Environmental Protection Act (Environmental 147.4QO(a)
Control), 7 Delaware Code Annotated, Chapter 60, Sections 6001
through 6060 (Revised 1974 and Cumm, Supp. 1988); (2) State
of Delaware Regulations Governing Underground Injection Control,
Parts 122, 124, and 146 (Department of Natural Resources and
Environmental Control), effective August 15,1983.
Florida: (1) Florida Air and Water Pollution Control Act, Florida 147.500(a)
Statutes Annotated §§403.011^03,90 (1973 and Supp. 1983); (2)
Florida Administrative Code, Chapter 17-28, Underground Injection
Control (April 27,1989).
Georgia: (1) Oil and Gas Deep Drilling Act of 1975, Official Code 147.550(a)
of Georgia Annotated (O.C.G.A.), sections 12^1—JO through 12-
4-53 (1988); (2) Ground Water Use Act of 1972, O.C.G.A., sections
15-2-90 through 12-5-107 (1988); (3) Water Well Standards Act
of 1985, O.C.G.A., sections 12-5-120 through 12-5-138 (1988);
(4) Georgia Administrative Procedure Act, O.C.G.A., sections 50-
13-1 through 50-13-22 (Reprinted from the O.C.G.A and 1988
Cumm. Supp.); (5) Georgia Water Quality Control Act, O.C.G.A,,
sections 12-5-20 through 12-5-53 (1988); (6) Georgia Hazardous
Waste Management Act, O.C.G.A., sections 12-8-60 through 12-
8-83 (1988); (7) Georgia Safe Drinking Water Act of 1977, O.C.G.A.,
sections 12-5-170 through 12-5-193 (1988); (8) Rules of the Georgia
Department of Natural Resources, Environmental Protection Divi-
sion, Water Quality Control, GA. COMP. R. & REGS., Chapter 391-
3-6-13 (Revised July 28,1988).
Idaho: (1) Public Writings, Title 9, Chapter 3, Idaho Code, §§9- 147.650(a)
301 through 9-302 (Bobbs-Merrill 1979); (2) Crimes and Punish-
ments, Title 18, Chapter 1, Idaho Code, §§ 18-113 through 18-
114 (Bobbs-Merrill 1979 and Supp. 1984); (3) Department of Health
and Welfare, Title 39, Chapter 1, Idaho Code, Chapter 39-108
(Bobbs-Merrill 1977); (4) Drainage-Water Rights and Reclamation,
Title 42, Chapter 2, Idaho Code, §42-237(e); §42-238 (Bobbs-
Merrill 1977 and Supp. 1984); Department of Water Resources-
Water Resources Board, Title 42, Chapter 17, Idaho Code, §§42-
1701, 42-1703, 42-1735 (Bobbs-Merrill 1977), §42-1701A (Supp.
1984); (6) Director of Department of Water Resources, Title 42,
Chapter 18, Idaho Code, §§ 42-1801 through 42-1805 (Bobbs-Merrill
1977); (7) Waste Disposal and Injection Wells, Title 42, Chapter
39, Idaho Code, §§42-3901 through 42-3914 (Bobbs-Merrill 1977),
§§42-3915 through 42-3919 (Supp. 1984); (8) Idaho Trade Secrets
Act, Title 48, Chapter 8, Idaho Code, §§48-801 through 48-807
(Bobbs-Merrill 1977 and Supp. 1984); (9) Administrative Procedure,
Title 67, Chapter 52, Idaho Code, §§67-5201 through 67-5218
(Bobbs-Merrill 1980 and Supp, 1984); (10) Idaho Radiation Control
regulations (IRCR) §1-9002.70; §§1-9100 through 1-9110, Depart-
ment of Health and Welfare (May 1981); (11) Rules and Regulations:
Construction and Use of Injection Wells, Idaho Department of Water
Resources, Rules 1 through 14 (August 1984); (12) Rules and Regula-
tions: Practice and Procedures, Idaho Department of Water Re-
sources, Rules 1 through 14 (October 1983),
858
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149J—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Illinois: (1) Illinois Environmental Protection Act, Illinois ch. lil\l/ 147.700(8)
2\, §§1001-1051 (Smith-Kurd 1977 Revised Statutes and Supp.
1983), as amended by Public Act No. 83-431, 1983 Illinois Legisla-
tive Service, pages 2910-2916 (West); (2) Illinois Pollution Control
Board Rules and Regulations at Title 35, Illinois Administrative
Code, Chapter I, Part 700, Outline of Waste Disposal Regulations;
Part 702, RCRA and UIC Permit Programs; Part 704, UIC Permit
Program; Part 705, Procedures for Permit Issuance and Part 730,
Underground Injection Control Operating Requirements as amended
by IPCB Order No. R-83039 on December 15,1983.
Illinois: (1) Conservation of Oil and Gas, etc., Illinois Revised Statutes 147.701(a)
ch. 96\l/2\, §§5401-5457 (Smith-Kurd 1979 and Supp. 1983),
as amended by Public Act No. 83-1074 1983 Illinois Legislative
Service pages 7183-7185 (West); (2) Illinois Environmental Protec-
tion Act, Illinois Revised Statutes ch. lll\l/2\, §§1001-1051
(Smith-Kurd 1977 and Supp, 1983), as amended by Public Act
No. 83-431, 1983 Illinois Legislative Services pages 2910-2916
(West); (3) Illinois Revised Statutes ch. 100\l/2\, §§26 (Smith-
Kurd Supp. 1983); (4) Illinois Department of Mines and Minerals
Regulations for the Oil and Gas Division, Rules I, II, IIA, III, V,
VII, and IX. (1981),
Indiana; (1) Indiana Code, title 4, article 21.5, chapters 1 through 147.750
6 (1988); (2) West's Annotated Indiana Code,.title 13, article 8,
chapters 1 through 15 (1990 and Cumm. Supp. 1990); (3) Indiana
Administrative Code, title 310, article 7, rules 1 through 3 (Cumm.
Supp. 1991).
Kansas; (1) Kansas Administrative Regulations, Chapter 28, Article 147.850(a)
46, Underground Injection Control Regulations, Kansas Administra-
tive Regulations, sections 28^16-1 through 28^6-42 (1986 and
Supp. 1987); (2) Kansas Administrative Regulations, Chapter 28,,
Article 43, Construction, Operation, Monitoring and Abandonment
of Salt Solution Mining Wells, sections 28-43-1 through 28-43-
10 (1986); (3) Kansas Statutes Annotated, sections 65-161, 65-
164 through 65-166a, 65-17ld (1980 and Cumm. Supp. 1989).
859
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Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
Louisiana: (1) Louisiana Revised Statutes Annotated §§30:1-30:24
(1975 and Supp. 1982); (2) Underground Injection Control Program
Regulations for Class I, III, IV, and V Wells, Statewide Order No,
29-N-l (February 20, 1982), as amended June 1, 1985, and January
1986; (3)(i) Statewide Order Governing the Drilling for and Pro-
ducing of Oil and Gas in the State of Louisiana, Statewide Order
No. 29-B (August 26, 1974) (Composite Order Incorporating
Amendments through March 1, 1974); (ii) Amendments to State-
wide Order No. 29-B (Off-site Disposal of Drilling Mud and Salt
Water Generated from Drilling and Production of Oil and Gas
Wells) (effective July 20, 1980); (iii) Amendment to Statewide Order
No. 29-B (Amendment concerning the use of Tables 5A and 8A,
etc.) (December 15, 1980, effective January 1, 1981); (iv) Amend-
ment to Statewide Order No. 29-B (amendment concerning the
underground injection control of saltwater disposal wells, enhanced
recovery injection wells, and liquid hydrocarbon storage wells),
(effective February 20, 1982); (v) Amendment to Statewide Order
No. 29-B (amendment concerning the offsite disposal of drilling
mud and saltwater) (effective May 20, 1983; (vi) Amendment to
Statewide Order No. 29-B (amendment concerning disposal of non-
hazardous oilfields waste) (March 20,1984, effective May 20, 1984);
(vii) Amendment to Statewide Order No. 29-B (amendment con-
cerning the adminstrative approval of injectivity tests and pilot
projects in order to determine the feasibility of proposed enhanced
recovery projects) (June 20, 1985, effective July 1, 1985).
Maine: (1) Maine Revised Statutes Annotated title 38, §§361-A, 363-
B, 413, 414, 414-A, 420, and 1317-A (1978); (2) Rules to Control
the Subsurface Discharge of Pollutants by Well Injection, Rules
of the Department of Environmental Protection, Chapter 543 (adopt-
ed June 22, 1983, effective July 4, 1983),
Maryland: (1) Code of Maryland Regulations, Title 26, Subtitle 08,
Chapter 07, promulgated and effective as of March 1, 1989; (2)
Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 01,
promulgated and effective as of March 1,1989; (3) Code of Maryland
Regulations, Title 26, Subtitle 08, Chapter 02, promulgated and
effective as of March 1, 1989; (4) Code of Maryland Regulations,
Title 26, Subtitle 08, Chapter 03, promulgated and effective as
of March 1, 1989; (5) Code of Maryland Regulations, Title 26,
Subtitle 08, Chapter 04, promulgated and effective as of March
1, 1989; (6) Code of Maryland Regulations, Title 26, Subtitle 13,
Chapter 05, section ,19, promulgated and effective as of August
1, 1989; (7) Code of Maryland Regulations, Title 26, Subtitle 01,
Chapter 02, promulgated and effective as of March 1, 1989; (8)
Code of Maryland Regulations, Title 26, Subtitle 01, Chapter 04,
promulgated and effective as of March 1, 1989.
Massachusetts; (1) Massachusetts General Laws Annotated ch, 21,
§§27, 43, and 44 (West 1981); (2) Code of Massachusetts Regula-
tions, title 310, §§ 23,01-23.11 as amended April 26,1982.
40 CFR
147,950(a)
147.100
147.1050(a)
147.1100(a)
860
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Mississippi: (1) Mississippi Air and Water Pollution Control Law, 147.1250(a)
Mississippi Code Annotated §§49-17-1 through 49-17-29 (1972)
and Supp, 1983); (2) Mississippi Department of Natural Resources,
Bureau of Pollution Control, Underground Injection Control Pro-
gram Regulations (adopted February 11, 1982); (3) Mississippi De-
partment of Natural Resources, Bureau of Pollution Control, State
of Mississippi Wastewater Permit Regulations for National Pollutant
Discharge Elimination System (NPDES), Underground Injection
Control (UIC), and State Operating Permits (adopted May 1, 1974;
amended February 11, 1982).
Mississippi: (1) (i) Mississippi Code Annotated (MCA), Section 5- 147.1251(a)
9-9 (Supp. 1988); (ii) MCA, Sections 53-1-1 through 53-1-17,
inclusive and Sections 53-1-71 through 53-1-77, inclusive (1972
and Supp, 1988); (iii) MCA, Sections 53-3-1 through 53-3-165,
inclusive (1972 and Supp, 1988); (2) State Oil and Gas Board
Statewide Rules and Regulations, Rules 1 through 65, inclusive
(Aug. 1,1987, as amended, Sept. 17, 1987).
Missouri: (1) Revised Statutes of the State of Missouri, Volume 2, 147.1300(a)
sections 204.016, 204.026, 204.051, 204.056 and Volume V, section
577,155 (1978 and Cumm, Supp. 1984); (2) Missouri Code of State
Regulations, Title 10, division 50, chapters 1 and 2 (June 1984);
(3) Vernon's Annotated Missouri Statutes, chapter 204, sections
204.006 through 204.470 (1983 and Cumm. Supp. 1990).
Montana: (1) Montana Statutory Requirements Applicable to the Un- 147.1350(a)
derground Injection Control Program, August 1996; (2) Montana
Regulatory Requirements Applicable to the Underground Injection
Control Program, August 1996.
Nebraska: (1) Rules and Regulations of the Nebraska Oil and Gas 147.1400(a)
Conservation Commission, Rules 1-6 (as published by the Commis-
sion, May 1981); (2) Revised Statutes of Nebraska, sections 57-
903 and 57-906 (Reissue 1988).
Nebraska: (1) Revised Statutes of Nebraska, Nebraska Environmental 147.1401(a)
Protection Act, sections 81-1502, 81-1506, 81-1519, and 81-1520
(Reissue 1987); (2) Nebraska Department of Environmental Control,
Title 122—Rules and Regulations for Underground Injection and
Mineral Production Wells, Effective Date: February 16, 1982,
Amended Dates: November 12, 1983, March 22, 1984; as amended
by amendment approved by the Governor on January 2,1989.
Nevada: (1) (i) Nevada Revised Statutes (NRS) VOlume 25, Chapter 147.1450(a)
445.131 through 445.354, inclusive, 1987; (ii) NRS Volume 29,
Chapter 534A.010 through 534A.090, inclusive. 1987; (iii) NRS
Volume 28, Chapter 522.010 through 522.190, inclusive. 1987; (2)
(i) Nevada Administrative Code (NAG) Underground Injection Con-
trol Regulations, Sections 1 through 96.1, inclusive. July 22, 1987,
revised September 3, 1987 (amending NAG Chapter 445); (ii) NAG
Regulations and Rules of Practice and Procedure adopted pursuant
to NRS 534A, Sections 1 through 69, inclusive. November 12,
1985 (amending NAG Chapter 534A); (iii) NAG Regulations and
Rules of Practice and Procedure adopted pursuant to NRS 522.010
through 522.625, inclusive. July 22, 1987 (amending NAG Chapter
522).
New Hampshire: (1) New Hampshire Revised Statutes Annotated 147.1500(a)
§ 149:8 III(a) (1978); (2) New Hampshire Code of Administrative
Rules, Part We 410 (Protection of Groundwaters of the State, §§ Ws
410.1 through Ws 410,16) (Issue Ws 3-82).
861
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Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
New Jersey: (1) New Jersey Statutes Annotated, Water Pollution Con-
trol Act, sections 58:10A-1 through 58:10A-20 (West 1982 and
Supp, 1990); (2) New Jersey Administrative Code sections 7:14A-
1.1 through 1.9 (subchapter 1), 7:14A-2.1 through 2.15 (subchapter
2), 7:14A-5.1 through 5.17 (subchapter 5) (amended March 1988).
New Mexico; (1) Oil and Gas Act, New Mexico Statutes Annotated
§§70-2-1 through -36 (1978); (2) State of New Mexico Energy
and Mineral Department, OH Conservation Division—Rules and
Regulations (dated 10-1-78), §§B-3, 1-701 through 1-708, M-1100
through M-1121.
New Mexico: (1) New Mexico Water Quality Control Commission
Regulations (WQCC 82-1) §§ 1-100 through 5-300 (September 20,
1982).
North Carolina: (1) Administrative Procedure Act, N.C. GEN. STAT.
sections 150B-1 through 150B-64 (1987 and Cumm. Supp. 1989);
(2) North Carolina Well Construction Act, N.C. GEN. STAT. sections
87-83 through 87-99 (1989 and Cumm, Supp. 1989); (3) Water
and Air Resources, N.C. GEN. STAT. sections 143-211 through
143-215.10 (1987 and Cumm. Supp. 1989); (4) Solid Waste Manage-
ment, N.C. GEN. STAT. sections 130A-290 through 130A-309.03
(1989); (5) North Carolina Drinking Water Act, N.C, GEN. STAT.
sections 130A-311 through 130A-332 (1989); (6) Sanitary Sewage
Systems, N.C. GEN. STAT. sections 130A-333 through 130A-335
(1989).
North Dakota: (1) North Dakota Century Code, Chapter 38-08 (Control
of Gas and Oil Resources, 1987 and Supp. 1989); (2) North Dakota
Administrative Code, Chapter 43-02-05 (Underground Injection
Control, as published in Statutes and Rules for the Conservation
of Oil and Gas, North Dakota Industrial Commission, revised effec-
tive November 1, 1987); (3) North Dakota Administrative Code,
Chapter 43-Q2-O3 (General Rules, as published in Statutes and
Rules for the Conservation of Oil and Gas, North Dakota Industrial
Commission, revised effective November 1,1987).,
North Dakota; (1) North Dakota Century Code sections 38-12-01,
39-12-03 (1980); sections 61-28-02, 61-28-06 (Supp. 1980); (2)
North Dakota Century Code, sections 61-28-02 and 61-28-06
(1989); (3) sections 43-02-02-01, 43-02-02-12, 43-02-02-16
through 43-02-02-26, 43-02-02-29, 43-02-02-31, 43-02-02-35
(1978); (4) North Dakota Administrative Code, Chapter 43-02-02
(Subsurface Mineral Mineral Exploration and Development) (August
1986), and Chapter 43-02-02.1 (Underground Injection Control. Pro-
gram) (March 1,1984).
Ohio: (1) Ohio Revised Code Annotated, §§1509.01, 1509.03,
1509.221 (Supp. 1983); (2) Rules of the Division of Oil and Gas,
Ohio Administrative Code, §§1501:9-7-01 through 7-14 (1984);
(3) Ohio Revised Code Annotated, §§6111.04, 6111.043, 6111.044
(Supp. 1983); (4) Rules of the Ohio Environmental Protection Agen-
cy, Ohio Administrative Code §§ 3745-34-01, through 34-41; 3745-
9-01 through 9-11 (Director Ohio EPA Order, June 18,1984).
Oklahoma: (1) Oklahoma Statutes title 63 §§1-901, 1-903 (1981);
(2) Oklahoma Controlled Industrial Waste Disposal Act, Oklahoma
Statute Annotated title 63 §§1-2002, 1-2014 (West Supp. 1983-
1984).
40 CFR
147.1550(a)
147.1600(a)
147.1601(a)
147.1700(a)
147.1750(a)
147.1751(a)
147.1801(a)
147.1850(a)
862
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY^Continued
40 CFR
147.1900(a)
Oregon: (1) Oregon Revised Statutes, Title 16, Ch, 164, sections
164.785; Title 36, Ch. 468, sections 468,005, 468.065 to 468,070,
468.700 to 468.815; (2) Oregon Administrative Rules, Chapter 340,
Division 44, sections 340-^14-005 through 340-44-055 (October
1983); Chapter 340, Division 45, sections 340-45-005 through 340-
45-075 (January 1990); Chapter 632, Division 10, sections 632-
10-002 through 632-10-235 (May 1986); Chapter 632, Division
20, sections 632-20-005 through 632-20-180 (May 1984).
Rhode Island; (1) Rhode Island Gen. Laws §§46-12-1, 46-12-5, and 147.2000(a)
46-12-28 (Supp. 1983); (2) "Underground Injection Control Program
Rules and Regulations." State of Rhode Island and Providence Plan-
tations Department of Environmental Management, Division of
Water Resources (as received by the Secretary of State, May 21,
1984),
South Carolina:(l) Pollution Control Act, S.C. Code Ann §§48-1- 147,2050(a)
10, 48-1-90, 48-1-100, 48-1-110 (Law. Co-op. 1976 and Supp.
1983); (2) South Carolina Department of Health and Environmental
Control, Ground-Water Protection Division, Underground Injection
Control Regulations, R-61-87, Effective Date: June 24, 1983.
South Dakota: (1) South Dakota Codified Laws, §§45-9-2, 45-9- 147.2100(a)
4, 45-9-11, 45-9-13, 45-9-14, 5-9-15 (1983). (2) Administrative
Rules of South Dakota, sections 74:10:02 through 74:10:07, 74:10:09,
and 74:10:11 published by the South Dakota Code Commission,
as revised through October 4, 1987,
Texas: "Texas Statutory and Regulatory Requirements Applicable to 147,2200
the Underground Injection Control Program for Class I, III, IV and
V, except Class III, Brine Mining Wells,".
Texas: "Texas Statutory and Regulatory Requirements Applicable to 147.2200
the Underground Injection Control Program for Class III Brine Min-
ing Wells,".
Utah: (1) Utah Code Annotated, Utah Water Pollution Control Act, 147.2250(a)
Title 26, Chapter 11, Sections 2, 8, and 10 (1989); (2) Utah Adminis-
trative Code, Underground Injection Control Regulations, section
R448-7 (effective as of January 2, 1990); (3) Underground Injection
Control Program (adopted January 20, 1990 and revised effective
July 20, 1990) (officially submitted to EPA by the Executive Sec-
retary of Utah Water Pollution Control Committee on August 16,
1990).
Utah; (1) Utah Code Annotated, 1953, section 40-6-1 through 40- 147,2251(a)
6-18, as amended 1988 and Cumm, Supp. 1990; (2) The Oil and
Gas Conservation General Rules, adopted under the authority of
the Oil and Gas Conservation Act, 40-6-1 et seq, Utah Code Anno-
tated, as amended 1988 (revised March 1989), rules R615-1 through
R615-4, and R815-8 through R615-10.
Vermont: (1) Vt. Stat. Ann. tit. 10, sections 1251, 1259, 1263 (1973 147.2300(a)
and Supp. 1981), Effective date: July 1, 1982; (2) Vermont Depart-
ment of Water Resources and Environmental Engineering, Chapter
13 Water Pollution Control Regulations, Subchapter 13.UIC—Under-
ground Injection Control, Discharges to Injection Wells, Effective
Date: June 21, 1984.
863
-------
Title 40—Protection of Environment
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Washington: (1) Revised Code of Washington §§90.48.020, -.080, 147.240Q(a)
-.160, and -.162 (Bureau of National Affairs, 1983 Laws); (2) Wash-
ington Administrative Code §§173-218-010 to 173-218-110 (Bu-
reau of National Affairs 2/29/84); (3) Washington Administrative
Code §§344-12-001 to 344-12-262 (Bureau of National Affairs,
1983); (4) Washington Administrative Code, Chapter 173-160 (re-
printed May 1988).
Wisconsin: (1) Wisconsin Statutes Annotated, sections 147.015, 147.2500(a)
147.02 and 147.04 (West 1974 and Supp. 1983); (2) Wisconsin
Administrative Code, Chapter NR 112, Well Construction and Pump
Installation, sections NR 112.03 and 112,20 (October 1981), as
amended by Natural Resources Board Order No. WQ-25-82, ap-
proved by the Natural Resources Board on August 25, 1982; (3)
Wisconsin Administrative Code, Chapter NR 113, Servicing Septic
Tanks, Seepage Pits, Grease Traps or Privies, sections NR 113.07
through 113.08 (1979), as amended by Natural Resources Board
Order No. WQ-25—82, approved by the Natural Resources Board
on August 25, 1982; (4) Wisconsin Administrative Code, Chapter
NR 181, Hazardous Waste Management, sections NR 181.04 through
181.415 (1981), as amended June 1985; (5) Wisconsin Administra-
tive Code, Chapter NR 210, Sewage Treatment Works, Natural Re-
sources Board Order No. WQ-25-82, section NR 210.05, approved
by the Natural Resources Board on August 25, 1982; (6) Wisconsin
Administrative Code, Chapter NR 214, Land Application and Dis-
posal of Liquid Industrial Wastes and By-products, sections NR
214.03 and 214.08 (1983),
Wyoming: (1) Wyoming Environmental Quality Act, Wyoming Stat- 147.2550(a)
utes, sections 35-11-101 through 35-11-115, and 35-11-301
through 35-11-305 (1977 Republished Edition and 1989 Cumm.
Supp.); (2) Water Quality Rules and Regulations, Wyoming Depart-
ment of Environmental Quality, Chapter III; Regulations for Permit
to Construct, Install or Modify Public Facilities Capable or, (sic)
Causing or Contributing to Pollution (certified copy, signed Decem-
ber 21, 1983); (3) Water Quality Rules and Regulations, Wyoming
Department of Environmental Quality, Chapter VIII; Quality Stand-
ards for Groundwaters of Wyoming (certified copy, signed April
9,1980); (4) Water Quality Rules and Regulations, Wyoming Depart-
ment of Environmental Quality, Chapter IX: Wyoming Groundwater
Pollution Control Permit (certified copy, signed April 9, 1980);
(5) Water Quality Rules and Regulations, Wyoming Department
of Environmental Quality, Chapter XIII: Prohibitions of Permits
for New Hazardous Waste Injection Wells (certified copy, signed
August 25, 1989); (6) Land Quality Rules and Regulations, Wyoming
Department of Environmental Quality, Chapter XXI: In Situ Mining
(effective March 26,1981),
Wyoming: (1) Rules and Regulations of the Wyoming Oil and Gas 147.2551(a)
Conservation Commission, Including Rules of Practice and Proce-
dure, as published by the Wyoming Oil and Gas Conservation
Commission, August 7, 1990; (2) Wyoming Statutes, Title 30, Chap-
ter 5, sections 30-5-101 through 30-5-126, (June 1983 and Wyo-
ming Statutes Annotated, 1990 Supp).
864
-------
Material Approved for Incorporation by Reference
40 CFR (PARTS 136 TO 149)—Continued
ENVIRONMENTAL PROTECTION AGENCY—Continued
40 CFR
Guam: (1) Water Resources Conservation Act, Government Code of 147,2600(a)
Guam §§57021-57025, Pub, L. 9-31 (March 9, 1967), as amended
by Pub. L. 9-76 (July 29, 1967), as amended by Pub. L. 12-191
(December 30, 1974); (2) Water Pollution Control Act, Government
Code of Guam §§57042 and 57045, Pub. L, 9-76 (July 29, 1967),
as amended by Pub. L, 9-212 (August 5, 1968), as amended by
Pub. L, 10-31 (March 10, 1969), as amended by Pub. L. 12-191
(December 30, 1974); (3) Guam Environmental Protection Agency,
Underground Injection Control Regulations, Chapters 1—9, as re-
vised by amendments adopted September 24, 1982; (4) Guam Envi-
ronmental Protection Agency, Water Quality Standards, Section
I—IV (approved September 25, 1981, effective November 16, 1981).
Commonwealth of the Northern Mariana Islands: (1) CNMI Environ- 147.2800(a)
mental Protection Act, 2 CMC sections 3101, et seq. (1984); (2)
CNMI Coastal Resources Management Act, 2 CMC sections 1501,
et seq. (1984); (3) CNMI Drinking Water Regulations, Common-
wealth Register, Volume 4, Number 4 (August 15, 1982); (4) CNMI
Underground Injection Control Regulations, Commonwealth Reg-
ister, Volume 8, Number 5 (May 15, 1984, amended November
15, 1984, January 15, 1985); (5) CNMI Coastal Resources Manage-
ment Regulations, Commonwealth Register, Volume fi. Number 12,
December 17, 1984.
Commonwealth of Puerto Rico: (1) Underground Injection Control 147.2650
Regulations of the Commonwealth of Puerto Rico, Parts I through
V and appendices A and B, adopted September 14, 1983 (Amended
July 20, 1988); (2) Puerto Rico Public Policy Environmental Act
(PRPPE), Title 12 Laws of Puerto Rico Annotated (LPRA) Chapters
121 and 131, 1977 edition, as amended 1988 edition, and Chapter
122,1988 edition.
Copies of these materials are available at the addreses provided in the regulations cited
in this table
865
-------
-------
Table of CFR Titles and Chapters
(Revised as of July 1, 2004)
Title 1—General Provisions
I Administrative Committee of the Federal Register (Parts 1—49)
II Office of the Federal Register (Parts 50—299)
IV Miscellaneous Agencies (Parts 400—500)
Title 2—Grants and Agreements
SUBTITLE A—OFFICE OF MANAGEMENT AND BUDGET GUIDANCE FOR
GRANTS AND AGREEMENTS
I [Reserved]
II Office of Management and Budget Circulars and Guidance [Re-
served]
SUBTITLE B—FEDERAL AGENCY REGULATIONS FOR GRANTS AND
AGREEMENTS [RESERVED]
Title 3—The President
I Executive Office of the President (Parts 100—199)
Title 4—Accounts
I General Accounting Office (Parts 1—99)
Title 5—Administrative Personnel
I Office of Personnel Management (Parts 1—1199)
II Merit Systems Protection Board (Parts 1200—1299)
III Office of Management and Budget (Parts 1300—1399)
V The International Organizations Employees Loyalty Board
(Parts 1500—1599)
VI Federal Retirement Thrift Investment Board (Parts 1600—1699)
VIII Office of Special Counsel (Parts 1800—1899)
IX Appalachian Regional Commission (Parts 1900—1999)
XI Armed Forces Retirement Home (Part 2100)
XIV Federal Labor Relations Authority, General Counsel of the Fed-
eral Labor Relations Authority and Federal Service Impasses
Panel (Parts 2400—2499)
867
203-160 D-29
-------
Title 5—Administrative Personnel—Continued
Chap.
XV Office of Administration, Executive Office of the President
(Parts 2500—2599)
XVI Office of Government Ethics (Parts 2600—2699)
XXI Department of the Treasury (Parts 3100—3199)
XXII Federal Deposit Insurance Corporation (Part 3201)
XXIII Department of Energy (Part 3301)
XXIV Federal Energy Regulatory Commission (Part 3401)
XXV Department of the Interior (Part 3501)
XXVI Department of Defense (Part 3601)
XXVHI Department of Justice (Part 3801)
XXIX Federal Communications Commission (Parts 3900—3999)
XXX Farm Credit System Insurance Corporation (Parts 4000—4099)
XXXI Farm Credit Administration (Parts 4100—4199)
XXXIII Overseas Private Investment Corporation (Part 4301)
XXXV Office of Personnel Management (Part 4501)
XL Interstate Commerce Commission (Part 5001)
XLI Commodity Futures Trading Commission (Part 5101)
XLII Department of Labor (Part 5201)
XLIII National Science Foundation (Part 5301)
XLV Department of Health and Human Services (Part 5501)
XLVI Postal Bate Commission (Part 5601)
XLVII Federal Trade Commission (Part 5701)
XLVIII Nuclear Regulatory Commission (Part 5801)
L Department of Transportation (Part 6001)
LII Export-Import Bank of the United States (Part 6201)
LIII Department of Education (Parts 6300—6399)
LIV Environmental Protection Agency (Part 6401)
LV National Endowment for the Arts (Part 6501)
LVI National Endowment for the Humanities (Part 6601)
LVII General Services Administration (Part 6701)
LVIII Board of Governors of the Federal Reserve System (Part 6801)
LIX National Aeronautics and Space Administration (Part 6901)
LX United States Postal Service (Part 7001)
LXI National Labor Relations Board (Part 7101)
LXII Equal Employment Opportunity Commission (Part 7201)
LXIII Inter-American Foundation (Part 7301)
LXV Department of Housing and Urban Development (Part 7501)
LXVI National Archives and Records Administration (Part 7601)
LXVH Institute of Museum and Library Services (Part 7701)
LXIX Tennessee Valley Authority (Part 7901)
LXXI Consumer Product Safety Commission (Part 8101)
LXXIII Department of Agriculture (Part 8301)
LXXTV Federal Mine Safety and Health Review Commission (Part 8401)
868
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Title 5—Administrative Personnel—Continued
Chap.
LXXVI Federal Retirement Thrift Investment Board (Part 8601)
LXXVII Office of Management and Budget (Part 87011
Title 6—Homeland Security
I Department of Homeland Security, Office of the Secretary
(Parts 0—99)
Title 7—Agriculture
SUBTITLE A—OFFICE OF THE SECRETARY OF AGRICULTURE (PARTS
0—26)
SUBTITLE B—REGULATIONS OP THE DEPARTMENT OF AGRICULTURE
I Agricultural Marketing Service (Standards, Inspections, Mar-
keting Practices), Department of Agriculture (Parts 27—209)
II Pood and Nutrition Service, Department of Agriculture (Parts
210—299)
III Animal and Plant Health Inspection Service, Department of Ag-
riculture (Parts 300—399)
IV Federal Crop Insurance Corporation, Department of Agriculture
(Parts 400—499)
V Agricultural Research Service, Department of Agriculture
(Parts 500—599)
VI Natural Resources Conservation Service, Department of Agri-
culture (Parts 600—699)
VII Farm Service Agency. Department of Agriculture (Parts 700—
799)
VIII Grain Inspection, Packers and Stockyards Administration (Fed-
eral Grain Inspection Service), Department of Agriculture
(Parts 800—899)
IX Agricultural Marketing Service (Marketing Agreements and Or-
ders; Fruits, Vegetables, Nuts), Department of Agriculture
(Parts 900—999)
X Agricultural Marketing Service (Marketing Agreements and Or-
ders; Milk), Department of Agriculture (Parts 1000—1199)
XI Agricultural Marketing Service (Marketing Agreements and Or-
ders: Miscellaneous Commodities), Department of Agriculture
(Parts 1200—1299)
XIV Commodity Credit Corporation. Department of Agriculture
(Parts 1400—1499)
XV Foreign Agricultural Service, Department of Agriculture (Parts
1500—1599)
XVI Rural Telephone Bank, Department of Agriculture (Parts 1600—
1699)
XVII Rural Utilities Service, Department of Agriculture (Parts 1700—
1799)
XVIII Rural Housing Service, Rural Business-Cooperative Service,
Rural Utilities Service, and Farm Service Agency, Depart-
ment of Agriculture (Parts 1800—2099)
XX Local Television Loan Guarantee Board (Parts 2200—2299)
869
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Title 7—Agriculture—Continued
Chap.
XXVI Office of Inspector General, Department of Agriculture (Parts
2600—2699)
XXVII Office of Information Resources Management, Department of
Agriculture (Parts 2700—2799)
XXVIII Office of Operations, Department of Agriculture (Parts 2800—
2899)
XXIX Office of Energy, Department of Agriculture (Parts 2900—2999)
XXX Office of the Chief Financial Officer, Department of Agriculture
(Parts 3000—3099)
XXXI Office of Environmental Quality, Department of Agriculture
(Parts 3100—3199)
XXXII Office of Procurement and Property Management, Department
of Agriculture (Parts 3200—3299)
XXXIII Office of Transportation, Department of Agriculture (Parts
3300—3399)
XXXIV Cooperative State Research, Education, and Extension Service,
Department of Agriculture (Parts 3400—3499)
XXXV Rural Housing Service, Department of Agriculture (Parts 3500—
3599)
XXXVI National Agricultural Statistics Service, Department of Agri-
culture (Parts 3600—3699)
XXXVII Economic Research Service, Department of Agriculture (Parts
3700—3799)
XXXVIII World Agricultural Outlook Board, Department of Agriculture
(Parts 3800—3899)
XLI [Reserved]
XLII Rural Business-Cooperative Service and Rural Utilities Service,
Department of Agriculture (Parts 4200—4299)
Title 8—Aliens and Nationality
I Department of Homeland Security (Immigration and Naturaliza-
tion) (Parts 1—499)
V Executive Office for Immigration Review, Department of Justice
(Parts 1000—1399)
Title 9—Animals and Animal Products
I Animal and Plant Health Inspection Service, Department of Ag-
riculture (Parts 1—199)
II Grain Inspection, Packers and Stockyards Administration
(Packers and Stockyards Programs), Department of Agri-
culture (Parts 200—299)
III Pood Safety and Inspection Service, Department of Agriculture
(Parts 300—599)
Title 10—Energy
I Nuclear Regulatory Commission (Parts 0—199)
II Department of Energy (Parts 200—699)
870
-------
Title 10—Energy—Continued
Chap.
Ill Department of Energy (Parts 700—999)
X Department of Energy (General Provisions) (Parts 1000—1099)
XVII Defense Nuclear Facilities Safety Board (Parts 1700—1799)
XVIII Northeast Interstate Low-Level Radioactive Waste Commission
(Part 1800)
Title 11 —Federal Elections
I Federal Election Commission (Parts 1—9099)
Title 12—Banks and Banking
I Comptroller of the Currency, Department of the Treasury (Parts
1—199)
II Federal Reserve System (Parts 200—299)
III Federal Deposit Insurance Corporation (Parts 300—399)
IV Export-Import Bank of the United States (Parts 400—499)
V Office of Thrift Supervision, Department of the Treasury (Parts
500—599)
VI Farm Credit Administration (Parts 600—699)
VII National Credit Union Administration (Parts 700—799)
VIII Federal Financing Bank (Parts 800—899)
IX Federal Housing Finance Board (Parts 900—999)
XI Federal Financial Institutions Examination Council (Parts
1100—1199)
XIV Farm Credit System Insurance Corporation (Parts 1400—1499)
XV Department of the Treasury (Parts 1500—1599)
XVII Office of Federal Housing Enterprise Oversight, Department of
Housing and Urban Development (Parts 1700—1799)
XVIII Community Development Financial Institutions Fund, Depart-
ment of the Treasury (Parts 1800—1899)
Title 13—Business Credit and Assistance
I Small Business Administration (Parts 1—199)
III Economic Development Administration, Department of Com-
merce (Parts 300—399)
IV Emergency Steel Guarantee Loan Board, Department of Com-
merce (Parts 400—499)
V Emergency Oil and Gas Guaranteed Loan Board, Department of
Commerce (Parts 500—599)
Title 14—Aeronautics and Space
I Federal Aviation Administration, Department of Transportation
(Parts 1—199)
II Office of the Secretary, Department of Transportation (Aviation
Proceedings) (Parts 200—399)
871
-------
Title 14—Aeronautics and Space—Continued
Chap.
Ill Commercial Space Transportation, Federal Aviation Adminis-
tration, Department of Transportation (Parts 400—499)
V National Aeronautics and Space Administration (Parts 1200—
1299)
VI Air Transportation System Stabilization (Parts 1300—1399)
Title 15—Commerce and Foreign Trade
SUBTITLE A—OFFICE OP THE SECRETARY OF COMMERCE (PARTS 0—
29)
SUBTITLE B—REGULATIONS RELATING TO COMMERCE AND FOREIGN
TRADE
I Bureau of the Census, Department of Commerce (Parts 30—199)
II National Institute of Standards and Technology, Department of
Commerce (Parts 200—299)
III International Trade Administration, Department of Commerce
(Pf»,rts 300—399)
IV Foreign-Trade Zones Board, Department of Commerce (Parts
400-499)
VII Bureau of Industry and Security, Department of Commerce
(Parts 700—799)
VIII Bureau of Economic Analysis, Department of Commerce (Parts
800—899)
IX National Oceanic and Atmospheric Administration, Department
of Commerce (Parts 900—999)
XI Technology Administration, Department of Commerce (Parts
1100—1199)
XIII Bast-West Foreign Trade Board (Parts 1300—1399)
XIV Minority Business Development Agency (Parts 1400—1499)
SUBTITLE C—REGULATIONS RELATING TO FOREIGN TRADE AGREE-
MENTS
XX Office of the United States Trade Representative (Parts 2000—
2099)
SUBTITLE D—REGULATIONS RELATING TO TELECOMMUNICATIONS
AND INFORMATION
XXIII National Telecommunications and Information Administration,
Department of Commerce (Parts 2300—2399)
Title 16—Commercial Practices
I Federal Trade Commission (Parts 0—999)
II Consumer Product Safety Commission (Parts 1000—1799)
Title 17—Commodity and Securities Exchanges
I Commodity Futures Trading Commission (Parts 1—199)
II Securities and Exchange Commission (Parts 200—399)
IV Department of the Treasury (Parts 400—499)
872
-------
Title 18—Conservation of Power and Water Resources
Chap.
I Federal Energy Regulatory Commission, Department of Energy
(Parts 1—399)
III Delaware River Basin Commission (Parts 400—499)
VI Water Resources Council (Parts 700—799)
VIII Susquehanna River Basin Commission (Parts 800—899)
XIII Tennessee Valley Authority (Parts 1300—1399)
Title 19—Customs Duties
I Bureau of Customs and Border Protection, Department of Home-
land Security; Department of the Treasury (Parts 0—199)
II United States International Trade Commission (Parts 200—299)
III International Trade Administration, Department of Commerce
(Parts 300—399)
IV Bureau of Immigration and Customs Enforcement, Department
of Homeland Security (Parts 400—599)
Title 20—Employees' Benefits
I Office of Workers' Compensation Programs, Department of
Labor (Parts 1—199)
II Railroad Retirement Board (Parts 200—399)
III Social Security Administration (Parts 400—499)
IV Employees Compensation Appeals Board, Department of Labor
(Parts 500—599)
V Employment and Training Administration, Department of Labor
(Parts 600—699)
VI Employment Standards Administration, Department of Labor
(Parts 700—799)
VII Benefits Review Board, Department of Labor (Parts 800—899)
VIII Joint Board for the Enrollment of Actuaries (Parts 900—999)
IX Office of the Assistant Secretary for Veterans' Employment and
Training, Department of Labor (Parts 1000—1099)
Title 21—Food and Drugs
I Pood and Drug Administration, Department of Health and
Human Services (Parts 1—1299)
II Drug Enforcement Administration, Department of Justice (Parts
1300—1399)
III Office of National Drug Control Policy (Parts 1400—1499)
Title 22—Foreign Relations
I Department of State (Parts 1—199)
II Agency for International Development (Parts 200—299)
III Peace Corps (Parts 300—399)
873
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Title 22—Foreign Relations—Continued
Chap.
IV International Joint Commission, United States and Canada
(Parts 400—499)
V Broadcasting Board of Governors (Parts 500—599)
VII Overseas Private Investment Corporation (Parts 700—789)
IX Foreign Service Grievance Board Regulations (Parts 900—999)
X Inter-American Foundation (Parts 1000—1099)
XI International Boundary and Water Commission, United States
and Mexico, United States Section (Parts 1100—1199)
XII United States International Development Cooperation Agency
(Parts 1200—1299)
XIV Foreign Service Labor Relations Board; Federal Labor Relations
Authority; General Counsel of the Federal Labor Relations
Authority; and the Foreign Service Impasse Disputes Panel
(Parts 1400—1499)
XV African Development Foundation (Parts 1500—1599)
XVI Japan-United States Friendship Commission (Parts 1600—1699)
XVII United States Institute of Peace (Parts 1700—1799)
Title 23—Highways
I Federal Highway Administration, Department of Transportation
(Parts 1—999)
II National Highway Traffic Safety Administration and Federal
Highway Administration, Department of Transportation
(Parts 1200—1299)
III National Highway Traffic Safety Administration, Department of
Transportation (Parts 1300—1399)
Title 24—Housing and Urban Development
SUBTITLE A—OFFICE OF THE SECRETARY, DEPARTMENT OF HOUSING
AND URBAN DEVELOPMENT (PARTS 0—99)
SUBTITLE B—REGULATIONS RELATING TO HOUSING AND URBAN DE-
VELOPMENT
I Office of Assistant Secretary for Equal Opportunity, Department
of Housing and Urban Development (Parts 100—199)
II Office of Assistant Secretary for Housing-Federal Housing Com-
missioner, Department of Housing and Urban Development
(Parts 200—299)
III Government National Mortgage Association, Department of
Housing and Urban Development (Parts 300—399)
IV Office of Housing and Office of Multifamlly Housing Assistance
Restructuring, Department of Housing and Urban Develop-
ment (Parts 400—499)
V Office of Assistant Secretary for Community Planning and De-
velopment, Department of Housing and Urban Development
(Parts 500—599)
VI Office of Assistant Secretary for Community Planning and De-
velopment, Department of Housing and Urban Development
(Parts 600—699) [Reserved]
874
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Title 24—Housing and Urban Development—Continued
Chap.
VII Office of the Secretary, Department of Housing and Urban Devel-
opment (Housing Assistance Programs and Public and Indian
Housing Programs) (Parts 700—799)
VIII Office of the Assistant Secretary for Housing—Federal Housing
Commissioner, Department of Housing and Urban Develop-
ment (Section 8 Housing Assistance Programs, Section 202 Di-
rect Loan Program, Section 202 Supportive Housing for the El-
derly Program and Section 811 Supportive Housing for Persons
With Disabilities Program) (Parts 800—899)
IX Office of Assistant Secretary for Public and Indian Housing, De-
partment of Housing and Urban Development (Parts 900—1699)
X Office of Assistant Secretary for Housing—Federal Housing
Commissioner, Department of Housing and Urban Develop-
ment (Interstate Land Sales Registration Proarram) (Parts
1700—1799)
XII Office of Inspector General, Department of Housing and Urban
Development (Parts 2000—2099)
XX Office of Assistant Secretary for Housing—Federal Housing
Commissioner, Department of Housing and Urban Develop-
ment (Parts 3200—3899)
XXV Neighborhood Reinvestment Corporation (Parts 4100—4199)
Title 25—Indians
I Bureau of Indian Affairs, Department of the Interior (Parts 1—
299)
II Indian Arts and Crafts Board, Department of the Interior (Parts
300—399)
III National Indian Gaming Commission, Department of the Inte-
rior (Parts 500—599)
IV Office of Navajo and Hopi Indian Relocation (Parts 700—799)
V Bureau of Indian Affairs, Department oi the Interior, and Indian
Health Service, Department of Health and Human Services
(Part 900)
VI Office of the Assistant Secretary-Indian Affairs, Department of
the Interior (Parts 1000—1199)
VII Office of the Special Trustee for American Indians, Department
of the Interior (Part 1200)
Title 26—Internal Revenue
I Internal Revenue Service, Department of the Treasury (Parts 1—
899)
Title 27—Alcohol, Tobacco Products and Firearms
I Alcohol and Tobacco Tax and Trade Bureau, Department of the
Treasury (Parts 1—399)
II Bureau of Alcohol, Tobacco, Firearms, and Explosives, Depart-
ment of Justice (Parts 400—699)
875
-------
Title 28—Judicial Administration
Chap.
I Department of Justice (Parts 0—299)
III Federal Prison Industries, Inc., Department of Justice (Parts
300—399)
V Bureau of Prisons, Department of Justice (Parts 500—599)
VI Offices of Independent Counsel, Department of Justice (Parts
600—699)
VII Office of Independent Counsel (Parts 700—799)
VIII Court Services and Offender Supervision Agency for the District
of Columbia (Parts 800—899)
IX National Crime Prevention and Privacy Compact Council (Parts
900—999)
XI Department of Justice and Department of State (Parts 1100—
1199)
Title 29—Labor
SUBTITLE A—OFFICE OF THE SECRETARY OF LABOE (PARTS 0—99)
SUBTITLE B—REGULATIONS RELATING TO LABOR
I National Labor Relations Board (Parts 100—199)
II Office of Labor-Manag-ement Standards, Department of Labor
(Parts 200—299)
III National Railroad Adjustment Board (Parts 300—399)
IV Office of Labor-Manag-ement Standards, Department of Labor
(Parts 400—499)
V Wage and Hour Division, Department of Labor (Parts 500—899)
IX Construction Industry Collective Bargaining' Commission (Parts
900—999)
X National Mediation Board (Parts 1200—1299)
XII Federal Mediation and Conciliation Service (Parts 1400—1499)
XIV Equal Employment Opportunity Commission (Parts 1600—1699)
XVII Occupational Safety and Health Administration, Department of
Labor (Parts 1900—1999)
XX Occupational Safety and Health Review Commission (Parts
2200—2499)
XXV Employee Benefits Security Administration, Department of
Labor (Parts 2500—2599)
XXVII Federal Mine Safety and Health Review Commission (Parts
2700—2799)
XL Pension Benefit Guaranty Corporation (Parts 4000—4999)
Title 30—Mineral Resources
I Mine Safety and Health Administration, Department of Labor
(Parts 1—199)
II Minerals Management Service, Department of the Interior
(Parts 200—299)
III Board of Surface Mining and Reclamation Appeals, Department
of the Interior (Parts 300—399)
876
-------
Chap.
IV
VII
I
II
IV
V
VI
VII
VIII
IX
XII
XVI
XVIII
XIX
XX
XXI
XXIV
XX VII
XXVIII
Title 30—Mineral Resources—Continued
Geological Survey, Department of the Interior (Parts 400—499)
Office of Surface Mining Reclamation and Enforcement, Depart-
ment of the Interior (Parts 700—999)
Title 31—Money and Finance: Treasury
SUBTITLE A—OFFICE OF THE SECRETARY OF THE TREASURY (PARTS
0—50)
SUBTITLE B—REGULATIONS RELATING TO MONEY AND FINANCE
Monetary Offices, Department of the Treasury (Parts 51—199)
Fiscal Service, Department of the Treasury (Parts 200—399)
Secret Service, Department of the Treasury (Parts 400—499)
Office of Foreign Assets Control, Department of the Treasury
(Parts 500—599)
Bureau of Engraving and Printing. Department of the Treasury
(Parts 600—699)
Federal Law Enforcement Training Center, Department of the
Treasury (Parts 700—799)
Office of International Investment. Department of the Treasury
(Parts 800—899)
Federal Claims Collection Standards (Department of the Treas-
ury—Department of Justice) (Parts 900—999)
Title 32—National Defense
SUBTITLE A—DEPARTMENT op DEFENSE
Office of the Secretary of Defense (Parts 1—399)
Department of the Army (Parts 400—699)
Department of the Navy (Parts 700—799)
Department of the Air Force (Parts 800—1099)
SUBTITLE B—OTHER REGULATIONS RELATING TO NATIONAL DE-
FENSE
Defense Logistics Agency (Parts 1200—1299)
Selective Service System (Parts 1600—1699)
National Counter-intelligence Center (Parts 1800—1899)
Central Intelligence Agency (Parts 1900—1999)
Information Security Oversight Office, National Archives and
Records Administration (Parts 2000—2099)
National Security Council (Parts 2100—2199)
Office of Science and Technology Policy (Parts 2400—2499)
Office for Micronesian Status Negotiations (Parts 2700—2799)
Office of the Vice President of the United States (Parts 2800—
2899)
Title 33—Navigation and Navigable Waters
I Coast Guard, Department of Homeland Security (Parts 1—199)
II Corps of Engineers, Department of the Army (Parts 200—399)
I
V
VI
VII
877
-------
Title 33—Navigation and Navigable Waters—Continued
Chap.
IV Saint Lawrence Seaway Development Corporation, Department
of Transportation (Parts 400—499)
Title 34—Education
SUBTITLE A—OFFICE OF THE SECRETARY, DEPARTMENT OF EDU-
CATION (PARTS 1—99)
SUBTITLE B—REGULATIONS OF THE OFFICES OF THE DEPARTMENT
OF EDUCATION
I Office for Civil Rights, Department of Education (Parts 100—199)
II Office of Elementary and Secondary Education, Department of
Education (Parts 200—299)
III Office of Special Education and Rehabilitative Services, Depart-
ment of Education (Parts 300—399)
IV Office of Vocational and Adult Education, Department of Edu-
cation (Parts 400—499)
V Office of Bilingual Education and Minority Languages Affairs,
Department of Education (Parts 500—599)
VI Office of Postsecondary Education, Department of Education
(Parts 600—699)
XI National Institute for Literacy (Parts 1100—1199)
SUBTITLE c—REGULATIONS RELATING TO EDUCATION
XII National Council on Disability (Parts 1200—1299)
Title 35—Panama Canal
I Panama Canal Regulations (Parts 1—299)
Title 36—Parks, Forests, and Public Property
I National Park Service, Department of the Interior (Parts 1—199)
II Forest Service, Department of Agriculture (Parts 200—299)
III Corps of Engineers, Department of the Army (Parts 300—399)
IV American Battle Monuments Commission (Parts 400—499)
V Smithsonian Institution (Parts 500—599)
VII Library of Congress (Parts 700—799)
VIII Advisory Council on Historic Preservation (Parts 800—899)
IX Pennsylvania Avenue Development Corporation (Parts 900—999)
X Presidio Trust (Parts 1000—1099)
XI Architectural and Transportation Barriers Compliance Board
(Parts 1100—1199)
XII National Archives and Records Administration (Parts 1200—1299)
XV Oklahoma City National Memorial Trust (Part 1501)
XVI Morris K. Udall Scholarship and Excellence in National Environ-
mental Policy Foundation (Parts 1600—1699)
878
-------
Title 37—Patents, Trademarks, and Copyrights
Chap.
I United States Patent and Trademark Office, Department of
Commerce (Parts 1—199)
II Copyright Office, Library of Congress (Parts 200—299)
IV Assistant Secretary for Technology Policy, Department of Com-
merce (Parts 400—499)
V Under Secretary for Technology, Department of Commerce
(Parts 500—599)
Title 38—Pensions, Bonuses, and Veterans' Relief
I Department of Veterans Affairs (Parts 0—99)
Title 39—Postal Service
I United States Postal Service (Parts 1—999)
III Postal Rate Commission (Parts 3000—3099)
Title 40—Protection of Environment
I Environmental Protection Agency (Parts 1—1099)
IV Environmental Protection Agency and Department of Justice
(Parts 1400—1499)
V Council on Environmental Quality (Parts 1500—1599)
VI Chemical Safety and Hazard Investigation Board (Parts 1600—
1699)
VII Environmental Protection Agency and Department of Defense;
Uniform National Discharge Standards for Vessels of the
Armed Forces (Parts 1700—1799)
Title 41 —Public Contracts and Property Management
SUBTITLE B—OTHER PROVISIONS RELATING TO PUBLIC CONTRACTS
50 Public Contracts, Department of Labor (Parts 50-1—50-999)
51 Committee for Purchase From People Who Are Blind or Severely
Disabled (Parts 51-1—51-99)
60 Office of Federal Contract Compliance Programs, Equal Employ-
ment Opportunity, Department of Labor (Parts 60-1—60-999)
61 Office of the Assistant Secretary for Veterans' Employment and
Training Service, Department of Labor (Parts 61-1—61-999)
SUBTITLE C—FEDERAL PROPERTY MANAGEMENT REGULATIONS
SYSTEM
101 Federal Property Management Regulations (Parts 101-1—101-99)
102 Federal Management Regulation (Parts 102-1—102-299)
105 General Services Administration (Parts 105-1—105-999)
109 Department of Energy Property Management Regulations (Parts
109-1—109-99)
114 Department of the Interior (Parts 114-1—114-99)
115 Environmental Protection Agency (Parts 115-1—115-99)
879
-------
Title 41—Public Contracts and Property Management—Continued
Chap,
128 Department of Justice (Parts 128-1—128-99)
SUBTITLE D—OTHER PROVISIONS RELATING TO PROPERTY MANAGE-
MENT [RESERVED]
SUBTITLE E—FEDERAL INFORMATION RESOURCES MANAGEMENT
REGULATIONS SYSTEM
201 Federal Information Resources Management Regulation (Parts
201-1—201-99) [Reserved]
SUBTITLE P—FEDERAL TRAVEL REGULATION SYSTEM
300 General (Parts 300-1—300-99)
301 Temporary Duty (TOY) Travel Allowances (Parts 301-1—301-99)
302 Relocation Allowances (Parts 302-1—302-99)
303 Payment of Expenses Connected with the Death of Certain Em-
ployees (Part 303-70)
304 Payment of Travel Expenses from a Non-Federal Source (Parts
304-1—304-99)
Title 42—Public Health
I Public Health Service, Department of Health and Human Serv-
ices (Parts 1—199)
IV Centers for Medicare & Medicaid Services, Department of Health
and Human Services (Parts 400—499)
V Office of Inspector General-Health Care, Department of Health
and Human Services (Parts 1000—1999)
Title 43—Public Lands: Interior
SUBTITLE A—OFFICE OF THE SECRETARY OF THE INTERIOR (PARTS
1—199)
SUBTITLE B—REGULATIONS RELATING TO PUBLIC LANDS
I Bureau of Reclamation, Department of the Interior (Parts 200—
499)
II Bureau of Land Management, Department of the Interior (Parts
1000—99§9)
III Utah Reclamation Mitigation and Conservation Commission
(Parts 10000—10010)
Title 44—Emergency Management and Assistance
I Federal Emergency Management Agency, Department of Home-
land Security (Parts 0—399)
IV Department of Commerce and Department of Transportation
(Parts 400—499)
Title 45—Public Welfare
SUBTITLE A—DEPARTMENT OP HEALTH AND HUMAN SERVICES
(PARTS 1—199)
SUBTITLE B—REGULATIONS RELATING TO PUBLIC WELFARE
880
-------
Title 45—Public Welfare—Continued
Chap.
II Office of Family Assistance (Assistance Programs), Administra-
tion for Children and Families, Department of Health, and
Human Services (Parts 200—299)
III Office of Child Support Enforcement (Child Support Enforce-
ment Program), Administration for Children and Families,
Department of Health and Human Services (Parts 300—399)
IV Office of Refugee Resettlement, Administration for Children and
Families, Department of Health and Human Services (Parts
400—499)
V Foreign Claims Settlement Commission of the United States,
Department of Justice (Parts 500—599)
VI National Science Foundation (Parts 600—699)
VII Commission on Civil Bights (Parts 700—799)
VIII Office of Personnel Management (Parts 800—899)
X Office of Community Services, Administration for Children and
Families, Department of Health and Human Services (Parts
1000—1099)
XI National Foundation on the Arts and the Humanities (Parts
1100—1199)
XII Corporation for National and Community Service (Parts 1200—
1299)
XIII Office of Human Development Services, Department of Health
and Human Services (Parts 1300—1399)
XVI Legal Services Corporation (Parts 1600—1699)
XVII National Commission on Libraries and Information Science
(Parts 1700—1799)
XVIII Harry S. Truman Scholarship Foundation (Parts 1800—1899)
XXI Commission on Fine Arts (Parts 2100—2199)
XXIII Arctic Research Commission (Part 2301)
XXIV James Madison Memorial Fellowship Foundation (Parts 2400—
2499)
XXV Corporation for National and Community Service (Parts 2500—
2599)
Title 46—Shipping
I Coast Guard, Department of Homeland Security (Parts 1—199)
II Maritime Administration, Department of Transportation (Parts
200—399)
HI Coast Guard (Great Lakes Pilotage), Department of Homeland
Security (Parts 400—499)
IV Federal Maritime Commission (Parts 500—599)
Title 47—Telecommunication
I Federal Communications Commission (Parts 0—199)
II Office of Science and Technology Policy and National Security
Council (Parts 200—299)
881
-------
Title 47—Telecommunication—Continued
Chap,
III National Telecommunications and Information Administration,
Department of Commerce (Parts 300—399)
Title 48—Federal Acquisition Regulations System
1 Federal Acquisition Regulation (Parts 1—99)
2 Department of Defense (Parts 200—299)
3 Department of Health and Human Services (Parts 300—399)
4 Department of Agriculture (Parts 400—499)
5 General Services Administration (Parts 500—599)
6 Department of State (Parts 600—699)
7 United States Agency for International Development (Parts
700—799)
8 Department of Veterans Affairs (Parts 800—899)
9 Department of Energy (Parts 900—999)
10 Department of the Treasury (Parts 1000-1099)
12 Department of Transportation (Parts 1200—1299)
13 Department of Commerce (Parts 1300—1399)
14 Department of the Interior (Parts 1400—1499)
15 Environmental Protection Agency (Parts 1500—1599)
16 Office of Personnel Management, Federal Employees Health
Benefits Acquisition Regulation (Parts 1600—1699)
17 Office of Personnel Management (Parts 1700—1799)
18 National Aeronautics and Space Administration (Parts 1800—
1899)
19 Broadcasting Board of Governors (Parts 1900—1999)
20 Nuclear Regulatory Commission (Parts 2000—2099)
21 Office of Personnel Management, Federal Employees Group Life
Insurance Federal Acquisition Regulation (Parts 2100—2199)
23 Social Security Administration (Parts 2300—2399)
24 Department of Housing and Urban Development (Parts 2400—
249i)
25 National Science Foundation (Parts 2500—2599)
28 Department of Justice (Parts 2800—2899)
29 Department of Labor (Parts 2900—2999)
30 Department of Homeland Security, Homeland Security Acquisi-
tion Regulation (HSAR) (Parts 3000—3099)
34 Department of Education Acquisition Regulation (Parts 3400—
3499)
35 Panama Canal Commission (Parts 3500—3599)
44 Federal Emergency Management Agency (Parts 4400—4499)
51 Department of the Army Acquisition Regulations (Parts 5100—
5199)
52 Department of the Navy Acquisition Regulations (Parts 5200—
5299)
53 Department of the Air Force Federal Acquisition Regulation
Supplement (Parts 5300—5399)
882
-------
Title 48—Federal Acquisition Regulations System—Continued
Chap.
54 Defense Logistics Agency, Department of Defense (Parts 5400—
5499)
57 African Development Foundation (Parts 5700—5799)
61 General Services Administration Board of Contract Appeals
(Parts 6100—6199)
63 Department of Transportation Board of Contract Appeals (Parts
6300—6399)
99 Cost Accounting Standards Board, Office of Federal Procure-
ment Policy, Office of Management and Budget (Parts 9900—
9999)
Title 49—Transportation
SUBTITLE A—OFFICE OP THE SECRETARY OF TRANSPORTATION
(PARTS 1—99)
SUBTITLE B—OTHER REGULATIONS RELATING TO TRANSPORTATION
I Research and Special Programs Administration, Department of
Transportation (Parts 100—199)
II Federal Railroad Administration, Department of Transportation
(Parts 200—299)
III Federal Motor Carrier Safety Administration, Department of
Transportation (Parts 300—399)
IV Coast Guard, Department of Homeland Security (Parts 400—499)
V National Highway Traffic Safety Administration, Department of
Transportation (Parts 500—599)
VI Federal Transit Administration, Department of Transportation
(Parts 600—699)
VII National Railroad Passenger Corporation (AMTRAK) (Parts
700—799)
VIII National Transportation Safety Board (Parts 800—999)
X Surface Transportation Board, Department of Transportation
(Parts 1000—1399)
XI Bureau of Transportation Statistics, Department of Transpor-
tation (Parts 1400—1499)
XII Transportation Security Administration, Department of Home-
land Security (Parts 1500—1599)
Title 50—Wildlife and Fisheries
I United States Fish and Wildlife Service, Department of the Inte-
rior (Parts 1—199)
II National Marine Fisheries Service, National Oceanic and Atmos-
pheric Administration, Department of Commerce (Parts 200—
299)
III International Fishing and Related Activities (Parts 300—399)
IV Joint Regulations (United States Fish and Wildlife Service, De-
partment of the Interior and National Marine Fisheries Serv-
ice, National Oceanic and Atmospheric Administration, De-
partment of Commerce); Endangered Species Committee Reg-
ulations (Parts 400—499)
883
-------
Title 50—Wildlife and Fisheries—Continued
Chap.
V Marine Mammal Commission (Parts 500—599)
VI Fishery Conservation and Management, National Oceanic and
Atmospheric Administration, Department of Commerce (Parts
600—699)
CFR Index and Finding Aids
Subject/Agency Index
List of Agency Prepared Indexes
Parallel Tables of Statutory Authorities and Rules
List of CPB Titles, Chapters, Subchapters, and Parts
Alphabetical List of Agencies Appearing" in the CFB
884
-------
Alphabetical List of Agencies Appearing in the CFR
(Revised as of July 1, 2004)
Agency
Administrative Committee of the Federal Register
Advanced Research Projects Agency
Advisory Council on Historic Preservation
African Development Foundation
Federal Acquisition Regulation
Agency for International Development, United States
Federal Acquisition Regulation
Agricultural Marketing Service
Agricultural Research Service
Agriculture Department
Agricultural Marketing Service
Agricultural Research Service
Animal and Plant Health Inspection Service
Chief Financial Officer, Office of
Commodity Credit Corporation
Cooperative State Research, Education, and Extension
Service
Economic Research Service
Energy, Office of
Environmental Quality, Office of
Farm Service Agency
Federal Acquisition Regulation
Federal Crop Insurance Corporation
Food and Nutrition Service
Food Safety and Inspection Service
Foreign Agricultural Service
Forest Service
Grain Inspection, Packers and Stockyards Administration
Information Resources Management, Office of
Inspector General, Office of
National Agricultural Library
National Agricultural Statistics Service
Natural Resources Conservation Service
Operations, Office of
Procurement and Property Management, Office of
Rural Business-Cooperative Service
Rural Development Administration
Rural Housing Service
Rural Telephone Bank
Rural Utilities Service
Secretary of Agriculture, Office of
Transportation, Office of
World Agricultural Outlook Board
Air Force Department
Federal Acquisition Regulation Supplement
Air Transportation Stabilization Board
Alcohol and Tobacco Tax and Trade Bureau
Alcohol, Tobacco, Firearms, and Explosives, Bureau of
AMTRAK
American Battle Monuments Commission
American Indians, Office of the Special Trustee
Animal and Plant Health Inspection Service
Appalachian Regional Commission
CFR Title, Subtitle or
Chapter
1,1
32, I
36, VIII
22, XV
48, 57
22, II
48, 7
7,1, IX, X, XI
7. V
5, LXXIII
7. I, IX, X, XI
7, V
7, III; 9, I
7, XXX
7, XIV
7, XXXIV
7, XXXVII
7, XXIX
7, XXXI
7, VII, XVIII
48, 4
7, IV
7. II
9. Ill
7, XV
36, II
7, VIII: 9. II
7, XXVII
7. XXVI
7, XLI
7. XXXVI
7, VI
7, XXVIII
7, XXXII
7. XVIII, XLII
7, XLII
7, XVIII, XXXV
7, XVI
7, XVII. XVIII, XLII
7, Subtitle A
7, XXXIII
7, XXXVIII
32, VII
48, 53
14, VI
27, I
27, II
19, VII
36, IV
25, VII
7, III; 9, I
5. IX
885
-------
Agency
Architectural and Transportation Barriers Compliance Board
Arctic Research Commission
Armed Forces Retirement Home
Army Department
Engineers, Corps of
Federal Acquisition Regulation
Benefits Review Board
Bilingual Education and Minority Languages Affairs, Office of
Blind or Severely Disabled, Committee for Purchase From
People Who Are
Broadcasting Board of Governors
Federal Acquisition Regulation-.
Census Bureau
Centers for Medicare & Medlcaid Services
Central Intelligence Agency
Chief Financial Officer, Office of
Child Support Enforcement, Office of
Children and Families, Administration for
Civil Rights, Commission on
Civil Rights, Office for
Coast Guard
Coast Guard (Great Lakes Pilotage)
Commerce Department
Census Bureau
Economic Affairs, Under Secretary
Economic Analysis, Bureau of
Economic Development Administration
Emergency Management and Assistance
Federal Acquisition Regulation
Fishery Conservation and Management
Foreign-Trade Zones Board
Industry and Security, Bureau of
International Trade Administration
National Institute of Standards and Technology
National Marine Fisheries Service
National Oceanic and Atmospheric Administration
National Telecommunications and Information
Administration
National Weather Service
Patent and Trademark Office, United States
Productivity, Technology and Innovation. Assistant
Secretary for
Secretary of Commerce, Office of
Technology, Under Secretary for
Technology Administration
Technology Policy, Assistant Secretary for
Commercial Space Transportation
Commodity Credit Corporation
Commodity Futures Trading Commission
Community Planning and Development, Office of Assistant
Secretary for
Community Services, Office of
Comptroller of the Currency
Construction Industry Collective Bargaining Commission
Consumer Product Safety Commission
Cooperative State Research, Education, and Extension
Service
Copyright Office
Corporation for National and Community Service
Cost Accounting Standards Board
Council on Environmental Quality
Court Services and Offender Supervision Agency for the
District of Columbia
Customs and Border Protection Bureau
Defense Contract Audit Agency
Defense Department
CFE Title, Subtitle or
Chapter
36, XI
45, XXIII
5, XI
32, V
33, II; 36, III
48, 51
20, VII
34, V
41, 51
22, V
48, 19
15,1
42, IV
32, XIX
7, XXX
45, III
45, II, III, IV, X
45, VII
34, I
33,1; 46,1; 49, IV
46, III
44, IV
15,1
37, V
15, VIII
13, III
44, IV
48, 13
50, VI
15, IV
15, VII
15, III; 19, III
15, II
50, II, IV, VI
15, IX; 50, II. Ill, IV. VI
15, XXIII; 47, in
15, IX
37,1
37,1V
15, Subtitle A
37, V
15, XI
37, IV
14, III
7, XIV
5, XLI: 17,1
24, V, VI
45, X
12.1
29, IX
5, LXXI; 16. II
7, XXXIV
37, II
45. XII. XXV
48.99
40, V
28, VIII
19, I
32, I
5, XXVI; 32, Subtitle A;
40, VII
886
-------
Agency
Advanced Research Projects Agency
Air Force Department
Army Department
Defense Intelligence Agency
Defense Logistics Agency
Engineers, Corps of
Federal Acquisition Regulation
National Imagery and Mapping Agency
Navy Department
Secretary of Defense, Office of
Defense Contract Audit Agency
Defense Intelligence Agency
Defense Logistics Agency
Defense Nuclear Facilities Safety Board
Delaware River Basin Commission
District of Columbia, Court Services and Offender Supervision
Agency for the
Drug Enforcement Administration
Bast-West Foreign Trade Board
Economic Affairs. Under Secretary
Economic Analysis, Bureau of
Economic Development Administration
Economic Research Service
Education, Department of
Bilingrual Education and Minority Languages Affairs, Office
of
Civil Rights, Office for
Educational Research and Improvement, Office of
Elementary and Secondary Education, Office of
Federal Acquisition Regulation
Postsecondary Education. Office of
Secretary of Education, Office of
Special Education and Rehabilitative Services, Office of
Vocational and Adult Education, Office of
Educational Research and Improvement, Office of
Elementary and Secondary Education, Office of
Emergency Oil and Gas Guaranteed Loan Board
Emergency Steel Guarantee Loan Board
Employee Benefits Security Administration
Employees' Compensation Appeals Board
Employees Loyalty Board
Employment and Training" Administration
Employment Standards Administration
Endangered Species Committee
Energy, Department of
Federal Acquisition Regulation
Federal Energy Regulatory Commission
Property Management Regulations
Energy, Office of
Engineers, Corps of
Engraving and Printing, Bureau of
Environmental Protection Agency
Federal Acquisition Regulation
Property Management Regulations
Environmental Quality, Office of
Equal Employment Opportunity Commission
Equal Opportunity, Office of Assistant Secretary for
Executive Office of the President
Administration, Office of
Environmental Quality, Council on
Management and Budget, Office of
National Drug Control Policy, Office of
National Security Council
Presidential Documents
Science and Technology Policy, Office of
CFR Title, Subtitle or
Chapter
32, I
32, ¥11
32, V; 33, II; 36, III, 48,
51
32,1
32.1, XII; 48, 54
33, II; 36, III
48, 2
32,1
32, VI; 48, 52
32,1
32, I
32,1
32, XII; 48, 54
10, XVII
18, III
28, VIII
21, II
15, XIII
37, V
15, VIII
13, III
7. XXXVII
5, LIII
34, V
34, I
34, VII
34.11
48, 34
34, VI
34, Subtitle A
34, III
34, IV
34, VII
34,11
13. V
13. IV
29. XXV
20,1V
5, V
20, V
20, VI
50, IV
5, XXIII; 10, II, III, X
48,9
5, XXIV; 18, I
41, 109
7, XXIX
33, II; 36, III
31, VI
5, LIV; 40. I, IV, VII
48. IS
41, 115
7, XXXI
5, LXII; 29, XIV
24,1
3, I
5, XV
40, V
5, III, LXXVII: 14, VI;
48, 99
21, III
32, XXI: 47. 2
3
32, XXIV; 47, II
887
-------
Agency
Trade Representative, Office of the United States
Export-Import Bank of the United States
Family Assistance, Office of
Farm Credit Administration
Farm Credit System Insurance Corporation
Farm Service Agency
Federal Acquisition Regulation
Federal Aviation Administration
Commercial Space Transportation
Federal Claims Collection Standards
Federal Communications Commission
Federal Contract Compliance Programs, Office of
Federal Crop Insurance Corporation
Federal Deposit Insurance Corporation
Federal Election Commission
Federal Emergency Management Agency
Federal Acquisition Regulation
Federal Employees Group Life Insurance Federal Acquisition
Regulation
Federal Employees Health Benefits Acquisition Regulation
Federal Energy Regulatory Commission
Federal Financial Institutions Examination Council
Federal Financing Bank
Federal Highway Administration
Federal Home Loan Mortgage Corporation
Federal Housing Enterprise Oversight Office
Federal Housing Finance Board
Federal Labor Relations Authority, and General Counsel of
the Federal Labor Relations Authority
Federal Law Enforcement Training Center
Federal Management Regulation
Federal Maritime Commission
Federal Mediation and Conciliation Service
Federal Mine Safety and Health Review "Commission
Federal Motor Carrier Safety Administration
Federal Prison Industries, Inc.
Federal Procurement Policy Office
Federal Property Management Regulations
Federal Railroad Administration
Federal Register, Administrative Committee of
Federal Register, Office of
Federal Reserve System
Board of Governors
Federal Retirement Thrift Investment Board
Federal Service Impasses Panel
Federal Trade Commission
Federal Transit Administration
Federal Travel Regulation System
Fine Arts, Commission on
Fiscal Service
Fish and Wildlife Service, United States
Fishery Conservation and Management
Food and Drug Administration
Food and Nutrition Service
Food Safety and Inspection Service
Foreign Agricultural Service
Foreign Assets Control, Office of
Foreign Claims Settlement Commission of the United States
Foreign Service Grievance Board
Foreign Service Impasse Disputes Panel
Foreign Service Labor Relations Board
Foreign-Trade Zones Board
Forest Service
General Accounting Office
General Services Administration
Contract Appeals, Board of
Federal Acquisition Regulation
CFR Title, Subtitle or
Chapter
15, XX
5, LII: 12, IV
45.11
5, XXXI; 12, VI
5, XXX; 12, XIV
7, VII, XVIII
48, 1
14,1
14, III
31, IX
5, XXIX; 47,1
41,60
7, IV
5, XXII; 12, III
11,1
44,1
48, 44
48, 21
48, 16
5, XXIV; 18,1
12, XI
12, VIII
23, I, II
1,1V
12, XVII
12, IX
5, XIV; 22, XIV
31, VII
41, 102
46,1V
29, XII
5, LXXIV; 29, XXVII
49,111
28, III
48, 99
41, 101
49,11
1,1
1,11
12, II
5, LVIII
5, VI, LXXVI
5, XIV
5, XLVII; 16,1
49, VI
41, Subtitle F
45, XXI
31,11
50, I. IV
50, VI
21,1
7,11
9,111
7. XV
31, V
45, V
22, IX
22, XIV
22, XIV
15, IV
36,11
4,1
5, LVII; 41. 105
48, 61
48, 5
888
-------
Agency
Federal Management Regulation
Federal Property Management Regulations
Federal Travel Regulation System
General
Payment From a Non-Federal Source for Travel Expenses
Payment of Expenses Connected With the Death of Certain
Employees
Relocation Allowances
Temporary Duty (TOY) Travel Allowances
Geological Survey
Government Ethics, Office of
Government National Mortgage Association
Grain Inspection, Packers and Stockyards Administration
Harry S, Truman Scholarship Foundation
Health and Human Services, Department of
Centers for Medicare & Medicaid Services
Child Support Enforcement, Office of
Children and Families, Administration for
Community Services, Office of
Family Assistance, Office of
Federal Acquisition Regulation
Food and Drug Administration
Human Development Services, Office of
Indian Health Service
Inspector General (Health Care), Office of
Public Health Service
Refugee Resettlement, Office of
Homeland Security, Department of
Coast Guard
Coast Guard (Great Lakes Pilotage)
Customs and Border Protection Bureau
Federal Emergency Management Agency
Immigration and Customs Enforcement Bureau
Immigration and Naturalization
Transportation Security Administration
Housing and Urban Development, Department of
Community Planning and Development, Office of Assistant
Secretary for
Equal Opportunity, Office of Assistant Secretary for
Federal Acquisition Regulation
Federal Housing Enterprise Oversight, Office of
Government National Mortgage Association
Housing—Federal Housing Commissioner, Office of
Assistant Secretary for
Housing, Office of, and Multifamily Housing Assistance
Restructuring, Office of
Inspector General, Office of
Public and Indian Housing, Office of Assistant Secretary for
Secretary, Office of
Housing—Federal Housing Commissioner, Office of Assistant
Secretary for
Housing, Office of, and Multifamily Housing Assistance
Restructuring, Office of
Human Development Services, Office of
Immigration and Customs Enforcement Bureau
Immigration and Naturalization
Immigration Review, Executive Office for
Independent Counsel, Office of
Indian Affairs, Bureau of
Indian Affairs, Office of the Assistant Secretary
Indian Arts and Crafts Board
Indian Health Service
Industry and Security, Bureau of
Information Resources Management, Office of
Information Security Oversight Office, National Archives and
Records Administration
Inspector General
CFR Title, Subtitle or
Chapter
41, 102
41. 101
41, Subtitle F
41, 300
41, 304
41, 303
41, 302
41, 301
30, IV
5, XVI
24, III
7, VIII; 9, II
45, XVHI
5, XLV; 45, Subtitle A
42, IV
48, III
45, II, III, IV, X
45, X
45, II
48, 3
21,1
45, XIII
25, V; 42,1
42, V
42,1
45, IV
6,1
33. I; 46, I: 49. IV
46, III
19, I
44, I
19, IV
8, I
49, XII
5, LXV; 24, Subtitle B
24, V, VI
24.1
48, 24
12, XVII
24, III
24, II. VIII, X, XX
24, IV
24, XII
24, IX
24, Subtitle A, VII
24, II, VIII, X, XX
24, IV
45, XIII
19, IV
8, I
8, V
28, VII
25, I. V
25, VI
25, II
25, V; 42, I
15, VII
7, XXVII
32, XX
889
-------
Agency
Agriculture Department
Health and Human Services Department
Housing and Urban Development Department
Institute of Peace, United States
Inter-American Foundation
Interior Department
American Indians, Office of the Special Trustee
Endangered Species Committee
Federal Acquisition Regulation
Federal Property Management Regulations System
Fish and Wildlife Service, United States
Geological Survey
Indian Affairs, Bureau of
Indian Affairs, Office of the Assistant Secretary
Indian Arts and Crafts Board
Land Management, Bureau of
Minerals Management Service
National Indian G-aming Commission
National Park Service
Reclamation. Bureau of
Secretary of the Interior, Office of
Surface Mining and Reclamation Appeals, Board of
Surface Mining Reclamation and Enforcement, Office of
Internal Revenue Service
International Boundary and Water Commission, United States
and Mexico, United States Section
International Development, United States Agency for
Federal Acquisition Regulation
International Development Cooperation Agency, United
States
International Fishing and Related Activities
International Investment, Office of
International Joint Commission, United States and Canada
International Organizations Employees Loyalty Board
International Trade Administration
International Trade Commission, United States
Interstate Commeue Commission
James Madison Memorial Fellowship Foundation
Japan-United States Friendship Commission
Joint Board for the Enrollment of Actuaries
Justice Department
Alcohol, Tobacco, Firearms, and Explosives, Bureau of
Drug Enforcement Administration
Federal Acquisition Regulation
Federal Claims Collection Standards
Federal Prison Industries, Inc.
Foreign Claims Settlement Commission of the United
States
Immigration Review, Executive Office for
Offices of Independent Counsel
Prisons, Bureau of
Property Management Regulations
Labor Department
Benefits Review Board
Employee Benefits Security Administration
Employees' Compensation Appeals Board
Employment and Training Administration
Employment Standards Administration
Federal Acquisition Regulation
Federal Contract Compliance Programs, Office of
Federal Procurement Regulations System
Labor-Management Standards, Office of
Mine Safety and Health Administration
Occupational Safety and Health Administration
Public Contracts
Secretary of Labor, Office of
CPE Title, Subtitle or
Chapter
7, XXVI
42, V
24, XII
22, XVII
5, LXIII: 22, X
25. VII
50. IV
48. 14
41. 114
50,1, IV
30, IV
25, I. V
25. VT
25, II
43,11
30, II
25. Ill
36, I
43,1
43, Subtitle A
30, III
30, VII
26,1
22, XI
22,11
48, 7
22, XII
50, III
31, VIII
22, IV
5, V
15, III; 19, III
19, II
5, XL
45, XXIV
22, XVI
20, VIII
5, XXVIII; 28, I, XI; 40,
IV
27, II
21, II
48,28
31, IX
28, ni
45, V
8, V
28, VI
28, V
41, 128
5, XLII
20, VII
29, XXV
20, IV
20, V
20, VI
48,29
41, 60
41, 50
29, II. IV
30,1
29, XVII
41,50
29, Subtitle A
890
-------
Agency
Veterans' Employment and Training Service, Office of the
Assistant Secretary for
Wage and Hour Division
Workers' Compensation Programs, Office of
Labor-Management Standards, Office of
Land Management, Bureau of
Legal Services Corporation
Library of Congress
Copyright Office
Local Television Loan Guarantee Board
Management and Budget, Office of
Marine Mammal Commission
Maritime Administration
Merit Systems Protection Board
Micronesian Status Negotiations, Office for
Mine Safety and Health Administration
Minerals Management Service
Minority Business Development Agency
Miscellaneous Agencies
Monetary Offices
Morris K. Udall Scholarship and Excellence in National
Environmental Policy Foundation
National Aeronautics and Space Administration
Federal Acquisition Regulation
National Agricultural Library
National Agricultural Statistics Service
National and Community Service, Corporation for
National Archives and Records Administration
Information Security Oversight Office
National Bureau of Standards
National Capital Planning Commission
National Commission for Employment Policy
National Commission on Libraries and Information Science
National Council on Disability
National Counterintelligence Center
National Credit Union Administration
National Crime Prevention and Privacy Compact Council
National Drug Control Policy, Office of
National Foundation on the Arts and the Humanities
National Highway Traffic Safety Administration
National Imagery and Mapping Agency
National Indian Gaming Commission
National Institute for Literacy
National Institute of Standards and Technology
National Labor Relations Board
National Marine Fisheries Service
National Mediation Board
National Oceanic and Atmospheric Administration
National Park Service
National Railroad Adjustment Board
National Railroad Passenger Corporation (AMTRAK)
National Science Foundation
Federal Acquisition Regulation
National Security Council
National Security Council and Office of Science and
Technology Policy
National Telecommunications and Information
Administration
National Transportation Safety Board
National Weather Service
Natural Resources Conservation Service
Navajo and Hopi Indian Relocation, Office of
Navy Department
Federal Acquisition Regulation
Neighborhood Reinvestment Corporation
Northeast Interstate Low-Level Radioactive Waste
Commission
CFR Title, Subtitle or
Chapter
41, 61; 20, IX
29, V
20, I
29, II, IV
43, II
45, XVI
36, VII
37, II
7, XX
5, III, LXXVII; 14, VI;
48. 99
50, V
46, II
5, II
32, XXVII
30, I
30, II
15, XIV
1, IV
31, I
36, XVI
5, LIX; 14, V
48, 18
7, XLI
7, XXXVI
46, XII, XXV
5, LXVI; 36. XII
32. XX
15, II
1, IV
1,1V
45, XVII
34, XII
32, XVIII
12, VII
28, IX
21, III
45, XI
23, II, III; 49, V
32, I
25, III
34, XI
15,11
5, LXI; 29, I
50, II, IV, VI
29, X
15, IX; 50, II, III. IV. VI
36, I
29, III
49, VII
5, XLIII; 45, VI
48, 25
32, XXI
47, II
15, XXIII; 47, III
49. VIII
15, IX
7, VI
25, IV
32, VI
48, 52
24. XXV
10, XVIII
891
-------
Agency
Nuclear Regulatory Commission
Federal Acquisition Regulation
Occupational Safety and Health Administration
Occupational Safety and Health Review Commission
Offices of Independent Counsel
Oklahoma City National Memorial Trust
Operations Office
Overseas Private Investment Corporation
Panama Canal Commission
Panama Canal Regulations
Patent and Trademark Office, United States
Payment From a Non-Federal Source for Travel Expenses
Payment of Expenses Connected With -the Death of Certain
Employees
Peace Corps
Pennsylvania Avenue Development Corporation
Pension Benefit Guaranty Corporation
Personnel Management, Office of
Federal Acquisition Regulation
Federal Employees Group Life Insurance Federal
Acquisition Regulation
Federal Employees Health Benefits Acquisition Regulation
Postal Bate Commission
Postal Service, United States
Postseoondary Education, Office of
President's Commission on White House Fellowships
Presidential Documents
Presidio Trust
Prisons, Bureau of
Procurement and Property Management, Office of
Productivity, Technology and Innovation, Assistant
Secretary
Public Contracts, Department of Labor
Public and Indian Housing, Office of Assistant Secretary for
Public Health Service
Railroad Retirement Board
Reclamation, Bureau of
Refugee Resettlement, Office of
Regional Action Planning Commissions
Relocation Allowances
Research and Special Programs Administration
Rural Business-Cooperative Service
Rural Development Administration
Rural Housing Service
Rural Telephone Bank
Rural Utilities Service
Saint Lawrence Seaway Development Corporation
Science and Technology Policy, Office of
Science and Technology Policy, Office of, and National
Security Council
Secret Service
Securities and Exchange Commission
Selective Service System
Small Business Administration
Smithsonian Institution
Social Security Administration
Soldiers' and Airmen's Home, United States
Special Counsel, Office of
Special Education and Rehabilitative Services, Office of
State Department
Federal Acquisition Regulation
Surface Mining and Reclamation Appeals, Board of
Surface Mining- Reclamation and Enforcement, Office of
Surface Transportation Board
Susqaehanna River Basin Commission
Technology Administration
Technology Policy, Assistant Secretary for
CFR Title, Subtitle or
Chapter
5, XLVIII; 10, I
48, 20
29, XVII
29, XX
28, VI
36, XV
7, XXVIII
5, XXXIII; 22, VII
48, 35
35,1
37,1
41,304
41, 303
22,111
36, IX
29, XL
5, I, XXXV; 45, TOI
48, 17
48, 21
48, 16
5, XLVI; 39, III
5, LX; 39, I
34, VI
1, IV
3
36, X
28, V
7, XXXII
37,1V
41, 50
24, IX
42,1
20,11
43, I
45,1V
13, V
41, 302
49,1
7, XVIH, XLII
7, XLII
7, xvni, xxxv
7, XVI
7, XVII, XVIII, XLII
33,1V
32, XXIV
47, II
31, IV
17,11
32, XVI
13,1
36, V
20, IH; 48, 23
5, XI
5, VIII
34, in
22,1; 28, XI
48,6
30,111
30, VII
49, X
is, vni
15, XI
37, IV
892
-------
Agency
Technology, Under Secretary for
Tennessee Valley Authority
Thrift Supervision Office, Department of the Treasury
Trade Representative, United States, Office of
Transportation, Department of
Commercial Space Transportation
Contract Appeals, Board of
Emergency Management and Assistance
Federal Acquisition Regulation
Federal Aviation Administration
Federal Highway Administration
Federal Motor Carrier Safety Administration
Federal Railroad Administration
Federal Transit Administration
Maritime Administration
National Highway Traffic Safety Administration
Research and Special Programs Administration
Saint Lawrence Seaway Development Corporation
Secretary of Transportation, Office of
Surface Transportation Board
Transportation Statistics Bureau-
Transportation, Office of
Transportation Security Administration
Transportation Statistics Bureau
Travel Allowances, Temporary Duty (TOY)
Treasury Department
Alcohol and Tobacco Tax and Trade Bureau
Community Development Financial Institutions Fund
Comptroller of the Currency
Customs and Border Protection Bureau
Engraving and Printing, Bureau of
Federal Acquisition Regulation
Federal Law Enforcement Training Center
Fiscal Service
Foreign Assets Control, Office of
Internal Revenue Service
International Investment, Office of
Monetary Offices
Secret Service
Secretary of the Treasury, Office of
Thrift Supervision, Office of
Truman, Harry S. Scholarship Foundation
United States and Canada, International Joint Commission
United States and Mexico, International Boundary and Water
Commission, United States Section
Utah Reclamation Mitigation and Conservation Commission
Veterans Affairs Department.
Federal Acquisition Regulation
Veterans' Employment and Training Service. Office of the
Assistant Secretary for
Vice President of the United States, Office of
Vocational and Adult Education, Office of
Wage and Hour Division
Water Resources Council
Workers' Compensation Programs, Office of
World Agricultural Outlook Board
CFE Title, Subtitle or
Chapter
37, V
5. LXIX; 18, XIII
12, V
15, XX
5, L
14, III
48, 63
44, IV
48, 12
14, I
23, I, II
49, III
49, II
49, VI
46, II
23, II, III; 49, V
49, I
33. IV
14, II; 49, Subtitle A
49.X
49, XI
7, XXXIII
49, XII
49, XI
41, 301
5. XXI; 12, XV; 17, IV;
31, IX
27, I
12, XVIII
12, I
19, I
31, VI
48, 10
31, VII
31, II
31, V
26,1
31, VIII
31, I
31, IV
31. Subtitle A
12, V
45, XVIII
22, IV
22, XI
43, III
38, I
48. 8
41, 61; 20, IX
32, XXVIII
34, IV
29, V
18, VI
20, I
7, XXXVIII
893
-------
-------
List of CFR Sections Affected
All changes in this volume of the Code of Federal Regulations which
were made by documents published in the FEDERAL REGISTER since Jan-
uary 1, 2001, are enumerated in the following list. Entries indicate the
nature of the changes effected. Page numbers refer to FEDERAL REGISTER
pages. The user should consult the entries for chapters and parts as well
as sections for revisions.
Title 40 was established at 36 FR 12213, June 29, 1971. For the period be-
fore January 1, 2001, see the "List of CFR Sections Affected, 1964-1972,
1973-1985, and 1986-2000," published in ten separate volumes.
2001
40 CFR
66 FR
Pagre
Chapter I
Chapter I Nomenclature
change 34375,34376
136,3 (a) and (b) amended 3474
Regulation at 66 FR 3474 with-
drawn 26795
(b)(40) in part and (41) redesig-
nated as new (b)(41) and (42);
new (b)(41) revised; eff. 7-18-01
32776
141.2 Amended 7061
Regulation at 66 FR 7061 eff. date
delayed 16134
Regulation at 66 FR 7061 eff. date
delayed to 2-22-02 28350
141.6 (a) and (c) revised; (j) and (t)
added 7061
Regulation at 66 FR 7061 eff. date
delayed; (j)amended.. 16134
Regulation at 66 FR 7061 eff. date
delayed to 2-22-02; (j) amended
28350
141.11 (a) amended; (b) revised 7061
Regulation at 66 FR 7061 eff. date
delayed 16134
Regulation at 66 FR 7061 eff. date
delayed to 2-22-02 .....28350
141.12 Amended 3776
141.21 (f)(3) table amended 3493
Regulation at 66 FR 3493 with-
drawn 26795
141.23 (k)(l) table revised 3493
40 CFR—Continued
86 FR
Page
Chapter I—Continued
(a)(4)(i) table, (k)(l) table, (2)
table, (3) introductory text and
(ii) table amended; (a)(5), (c) in-
troductory text. (f)(l), (i)(l), (2)
and (k)(2) introductory text re-
vised; (c)(9) and (i)(4) added; eff.
in part 1-22-04 7061
Regulation at 66 FR 7061 eff. date
delayed in part 16134
Regulation at 66 FR 3493 with-
drawn 26795
Regulation at 66 FR 7061 eff. date
delayed in part to 2-22-02 28350
141.24 (eXl)amended 3495
(f)(15) introductory text and
(h)(ll) introductory text
amended; (f)(15)(i), (ii),
(h)(ll)(i) and (ii) revised;
(f)(15)(iii), (iv), (v), (22),
(hXllXiii), (iv), (v) and (20)
added; eff. in part 1-22-04 7063
Regulation at 66 FR 7063 eff. date
delayed in part... 16134
Regulation at 66 FR 3495 with-
drawn 26795
Regulation at 66 FR 7061 eff. date
delayed in part to 2-22-02 28350
141.25 (a) table revised 3495
Regulation at 66 FR 3495 with-
drawn 26795
141.30 (e) and (h) amended 3778
141.35 (c), (d), (e) and (f) re-
vised 2300
(d) Table 1 corrected 27215
(c) amended 46225
895
-------
40 CFR (7-1-04 Edition)
40 CFR—Continued
66 FB
Page
40 CFR— Continued
Chapter I—Continued
141.40 (a)(l)(iii) Introductory
text, (v) introductory text, (3)
Table 1, (4)(i) Table 2, (5)(ii)(B),
(C), (G), (7)(i), (ii), (iii) and
(b)(l)(ix) revised; Appendix A
amended 2302
(a)(3) Table 1 corrected 27215
(a)(5)(ii)(G)(J) amended 46225
141,51 (b) table amended 7063
Regulation at 66 PR 7063 eff. date
delayed 16134
Regulation at 66 FR 7063 eff. date
delayed to 2-22-02 28350
141.60 (b)(4)added 7063
Regulation at 66 B'R 7063 eff. date
delayed 16134
Regulation at 66 PR 7063 eff. date
delayed to 2-22-02 28350
141.62 (b) introductory text, table
and (c) table amended; (d)
added 7063
Regulation at 66 FR 7063 eff. date
delayed 16134
Regulation at 66 PR 7063 eff. date
delayed to 2-22-02 28350
141.64 (b)(l) and (2) amended 3776
141.65 (b)(l) and (2) amended 3776
141.71 (b)(6)amended 3776
141.73 (a)(3) and (d) amended 3776
141.74 (a)(l) table and (2) amend-
ed 3496
Regulation at 66 PR 3496 with-
drawn 26795
141.76 Added; eff. 8-7-01 31103
141.130 (b)(l)and(2)amended..... 3776
141.131 (b)(2) amended; (b)(3)
added 3776
141.132 (a)(2), (b)fl) table, (iii) and
(c)(l)(i) amended; (b)(l)(i) re-
vised; (b)(l)(iv) redesignated as
(b)(l)(v); new (b)(l)(iv)
added 3776
141.133 (a)(l), (b)(l)(i), (c)(l)(i),
(2)(i), (ii) and (d) amended;
(b)(l)(ii) and (iii) revised;
(b)(l)(iv) added 3777
141.134 (b) table and (c) table re-
vised; (d) table amended 3778
(d) table corrected 990
141.135 (a)(2)(iii), (b)(4) and (c)(l)
amended; (b)(2) table, (4) intro-
ductory text and (c)(l) table re-
vised .....3779
141.154 (b) revised; (f) added 7064
Regulation at 66 FR 7064 eff. date
delayed 16134
Page
Chapter I — Continued
Regulation at 66 FR 7064 eff. date
delayed to 2-22-02..... ................. 28350
141.151—141.155 (Subpart O) Ap-
pendix A amended ...................... 7064
Regulation at 66 FR 7064 eff. date
delayed ..................................... 16134
Regulation at 66 FR 7064 eff. date
delayed to 2-22-02. ..................... 28350
141.170 (a) introductory text
amended .................................... 3779
141.172 (a)(2)(iii)(A), (5), (b)(2) in-
troductory text, (3)(i) and
(4)(ii) amended ........................... 3779
141.173 Introductory text amend-
ed ............................................... 3779
141.175 Introductory text amend-
ed; (c) added ................................ 3779
141.201—141.210 (Subpart Q) Ap-
pendices A and B amended .......... 7065
Regulation at 66 PR 7065 eff.
date delayed .............................. 16134
Regulation at 66 PR 7065 eff. date
delayed to 2-22-02 ...................... 28350
Appendices A and B amended:
eff. 8-7-01 ......... ...... . .................. 31104
142.12 (b)(3)(i) revised; (d)(2)
amended ........................... . ........ 3780
142.14 (a)(4)(ii)(A)(7) amended;
(a)(4)(ii)(A)(5) revised;
(a)(4)(ii)(A)(9) added; eff. 8-7-
01 ........................................... ...31105
142.15 (c)(5)amended ...................... 3780
142.16 (e) introductory text re-
vised; (j) and (k) added; eff. 01-
22-04 ........................................... 7066
(i) added; eff. 8-7-01* .......... . ............ 31105
142.62 (b) table amended ................. 7066
Regulation at 66 FR 7066 eff. date
delayed ..................................... 16134
Regulation at 66 FR 7066 eff. date
delayed to 2-22-02 ...................... 28350
143.4 (b) table revised ...................... 3496
Regulation at 66 PR 3496 with-
drawn ................................ . ...... 26795
(b) amended ................................. 34376
148.18 (k) revised; (1) added ............ 58297
2002
40 CFR
67 FR
Page
Chapter I
136.3 (a) introductory text and
Tables IA through IB revised;
(b) amended 65226
(a) Table IB and (e) Table II
amended; (b)(41) revised 65886
896
-------
List of CFR Sections Affected
40 CFR—Continued STFR
Page
Chapter I—Continued
(a) Table IA and (b) amended 69971
140,4 (b)(l)(ii)added 35743
141.2 Amended 1835
141.35 (c) amended 11046
141.21 (f)(3) table, (f)(5) and (8)
amended; (f)(6)(i) and (ii) re-
vised 65246
(f)(3) table revised; (f)(6)(viii) and
(ix)added 65896
141.23 (k)(l) table revised 65246
(a)(4)(i) table and (k)(l) table
amended 65897
(a)(4)(i) table corrected 68911
141.24 (e)(l) amended ...65250
(e)(l) introductory text and table
revised 65898
141.25 (a) table revised 65250
141.40 (a)(3) Table 1 amended 65900
141.70 (e) added 1836
141.73 (a)(4) added; (d)revised 1836
141.74 (a)(l) table and (2) amend-
ed 65252
(a)(l) table revised 65901
141.153 (d)(4)(v)(C) amended 1836
141.151—141.155 (Subpart O) Ap-
pendix A amended 70855
Appendix A corrected 73011
141.170—141.175 (Subpart P) Head-
ing revised 1836
141.170 (d)added 1836
141.202 Table 1 amended 1836
141.203 (b)(3)(ii) revised 1836
141.201—141.210 (Subpart Q) Ap-
pendix A amended 1836
Appendix B amended 1838,70857
141.500—141.571 (Subpart T)
Added 1839
142.3 (b)(3) removed 70858
142.14 (a)(3), (4){i), (ii) introduc-
tory text and (7) revised 1843
142.16 (g) introductory text re-
vised; (j) added 1844
143.4 (b) table revised 65252
144 Policy decision 38403
144.1 (g) introductory text re-
vised 39592
144.13 (c)revised 39593
144.26 Introductory text revised;
(d) introductory text re-
moved 39593
144.81 (16) revised 39593
146 Policy decision 38403
147.2555 Table amended 47726
148 Determination 16262
2003
40 CFR
68 FR
Page
Chapter I
136.3 (a) Table IA revised; (b) and
(e) Table II amended 43278
(a) Table IA, (b) and (e) Table II
corrected 54934
141.23 (a)(4)(i) table and (k)(l)
table amended 14506
141.62 (b) table amended 14506
141.154 (b) introductory text and
(f) revised 14506
141.151—141.155 (Subpart O) Ap-
pendix A amended 14506
141.201—141.210 (Subpart Q) Ap-
pendix B amended 14507
2004
(Regulations published from January 1,
2004 through July 1, 2004)
40 CFR 69 FR
Page
Chapter I
136.3 Nomenclature change 18803
141 Nomenclature change 18803
Meeting-s 21958
141.21 (f)(3) table revised; (f)(6)(x)
added 7160
141.25 (a) table amended; eff, 8-31-
04 31012
(c)(l) Table B amended; eff. 7-29-
04 38855
141.26 (b)(2)(iv) and (5) revised;
(b)(6) amended; eff. 7-29-04 38855
141.62 (c) table amended; eff. 7-29-
04 38855
141.71 (a)(2) introductory text and
(c )(2)(i) amended; eff. 7-29-04 38855
141.72 (a)(3), (4)(i). (ii), (b)(2), (3)(i)
and (ii) amended; eff. 7-29-04 38855
141.73 (a)(l), (2), (4), (b)(l), (2),
(c)(l) and (2) amended; eff. 7-29-
04 38855
141.74 (b)(4)(ii), (6)(ii), (c)(3)(i) and
(ii) amended; eff. 7-29-04 38856
141.75 (a)(2)(viii)(G) and
(b)(2)(iii)(G) amended; eff. 7-29-
04 38856
141.85 (c)(2)(iii)(A) through (G)
added 38856
141.132 (a)(5) amended: eff. 7-29-
04 38856
141.133 (a)(3) revised; eff. 7-29-
04 38856
141.170 (d) amended; eff. 7-29-04 38856
897
-------
40 CFR (7-1-04 Edition)
40 CFR—Continued
69 FR
Page
Chapter I—Continued
141,201—141.209 (Subpart Q) Ap-
pendixes A and B amended;
eff. 7-29-04 38858
141.502 Revised; eff. 7-29-04 38856
141.530 Amended; eff. 7-29-04 38856
141.531 Amended; eff. 7-29-04 38856
141.534 Introductory text revised;
(a)(2) amended; eff. 7-29-04 38856
141.551 (a)(2) and (b)(2) amended;
eff. 7-29-04 38858
141.563 (b) and (c) amended; eff. 7-
29-04 38856
141.570 (b)(2) revised eff. 7-29-04 38857
142 Meetings 21958
40 CFR—Continued <*> m
Page
Chapter I—Continued
142.14 (d)(12)(iv) and (13) amended;
eff. 7-29-04 38857
142.16 (j) redesignated as (p); (1)(2)
and new (p)(2)(ii) amended; eff.
7-29-04 38857
142.62 (g-)(2) amended; eff. 7-29-
04 , ,.38857
143 Meetings , ..21958
143.4 Nomenclature change 18803
147 Comment request 18478
Nomenclature change 18803
147.2200 Revised 8568
Introductory text amended;
(a)(2), (b)(2), (c)(2), (d)(2) and
(e)(2) added 8828
n
898
------- |