-------
TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
Parameter
72 Titanium — Total 4 mg/L
73 Turbidity NTU63
75. Zinc -Total", mg/L
Methodology58
ICP/AES
Digestion " followed by:
AA direct aspiration
DCP
Nephelometric
Digestion 4 followed by:
AA furnace
ICP/AES . . .
ICP/MS
DCP or
Colorimetric (Gallic Acid)
Digestion4 followed by:
AA furnace
ICP/AES36
ICP/MS
DCP 3e or
Reference (method number or page)
EPA 35. 52
200.7, Rev. 4.4
(1994).
283.2 1 (Issued
1978).
180.1, Rev. 2.0
(1993).
200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).
289.2 ' (Issued
1978).
200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).
Standard methods
(18th, 19th)
3111 D
2130 B
3111 D
3120 B
3500-V D
3111 B or C
3120 B
3500-Zn E.
3500-Zn F
Standard methods
(20th)
2130 B
3120 B
3500-V B
3120 B
3500-Zn B
Standard methods
online
3111 D-99.
2130 B-01
3111 D-99.
3120 B-99
3500-V B-97.
3111 BorC-99
3120 B-9958
3500-Zn B-97
ASTM
D1889-94, 00
D3373-93, 03.
05673-03
D4190-94, 99
D1691-95, 02 (A
or B).
D5673-03
D4190-94, 99
USGS/AOAC/other
See footnote34
1-3860-85?
1-4471-9750
993. 143
See footnote34
974. 27 3, p. 37 9, I-
3900-85 2
(-4471-9750
993. 143
See footnote34
See footnote33
to
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o.
OJQ
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o
Z
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er
tvj
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O
03
P.
I
o
3
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 (NTIS PB 84-128677), Revised
March 1983 and 1979 where applicable.
2Fishman, 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.
3"Official Methods of Analysis of the Association of Official Analytical Chemists," Methods Manual, Sixteenth Edition, 4th Revision, 1998.
4 For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material
and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as
specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the
sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recover-
able digestion is described as Method 200.2 in Supplement I of "Methods for the Determination of Metals in Environmental Samples" EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8,
and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite fur-
nace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced
method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or the
EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes
as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the anal-
ysis after digestion procedure are reported as "total" metals.
5 Copper sulfate may be used in place of mercuric sulfate.
6 Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to re-
solve any controversies.
7Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY
10523.
8The approved method is that cited in "Methods for Determination of Inorganic Substances in Water and Fluvial Sediments", USGS TWRI, Book 5, Chapter A1 (1979).
9American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd St., New York, NY 10036.
'""Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency," Supplement to the Fifteenth Edition of Standard Methods tor the Examination of Water and Wastewater
(1981).
"The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
12Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures "total BOD." The addition of the nitrification inhibitor is not a procedural option,
but must be included to report the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a dis-
charger's permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
I3OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.
l4Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
-------
15The back titration method will be used to resolve controversy.
16Orion 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, respectively.
17The approvad method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
18National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971.
'"Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
20When using a method with block digestion, this treatment is not required.
21 Hydrogen-ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY
10523.
22lron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
"Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.
24Wershaw, R. L.,ef a/., "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 %
25Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. • •
2eJust prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
27The 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 approved methods are given on pp
576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 510C for the manual spectrometric procedure.
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.
29Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chlo-
ride 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 Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.
30The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition.
31 For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by add-
ing 4.0 mL of concentrated NH^OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the
digestate to >7 to prevent the formation ofHCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen
Book 1, Chapter D1, 1975. 2
33Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537. -
34"Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029," 1986—Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge
Parkway, Franklin, MA 02038
36Precision 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 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. "Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals", CEM Corporation S
P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation. O
37When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. "
38Only use n-hexane extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664A). Use of other extraction
solvents (e.g., those in the 18th and 19th editions) is prohibited.
39Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.
40Nitrogen, Total Kieldahl, Method PA1-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842. ^
41 Nitrogen, Total Kjejdanl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842. £•
42Method 1664, Revision A "n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated fT-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry" EPA-821-
R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161.
43USEPA. 2001. 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-821-R-02-024). 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-96-011) 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, P.O. 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. Q
46"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) o
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 (OFR) 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 Colorimetric Finish That Includes Di- _
alysis" Open File Report (OFR) 92-146. CD
""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 Absorption Spectrometry" "
Open File Report (OFR) 98-639. g
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 (OFR) 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 Fluvial Sediment," Open File Report (OFR) 93-125.
52AII EPA methods, excluding EPA Method 300.1, are published in "Methods for the Determination of Metals in Environmental Samples," Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL-CI), _cp
EPA/600/R-94/111, May 1994; and "Methods for the Determination of Inorganic Substances in Environmental Samples," NERL-CI, EPA/600/R-93/100, August, 1993. EPA Method 300.1 is available from http://
www.epa.gov/safewater/methods/pdfs/met300.pdf.
53Styrene divinyl benzene beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCal™ or equivalent) are acceptable substitutes for formazin. £2.
54Method D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte," available from Waters Corp 34 Maple
St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
55 Kelada-01, "Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate," EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information Service (NTIS), 5285
Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. The toll free telephone number is: 800-553-6847. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified
if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided
that the QC acceptance criteria are met.
56QuikChem 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" is available from Lachat
Instruments 6645 W. Mill Road, Milwaukee, Wl 53218, Telephone: 414-358-4200.
57 When using sulfide removal test procedures described in Method 335.4, reconstitute paniculate that is filtered with the sample prior to distillation.
6sUnless otherwise stated, if the language of this table specifies a sample digestion and/or distillation "followed by" analysis with a method, approved digestion and/or distillation are required prior to analysis. ..^
59Method 245.7, Rev. 2.0, "Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry," February 2005, EPA-821-R-05-001, available from the U.S. EPA Sample Control Center (operated by CSC), 6101 N5
Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100, Fax: 703-461-8056.
-------
60The use of EDTA may decrease method sensitivity in some samples. Analysts may omit EDTA provided that all method specified quality control acceptance criteria are met.
61 Samples analyzed for available cyanide using Methods OIA-1677 or D6888-04 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because
the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand ex-
change reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples.
bo
to
O3
•n
0)
EL
90
z
p
o
CL
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o
03
a-
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11227
TABLE 1C.—-LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS
Parameter '
1 . Acenaphthene
2. Acenaphthylene
3. Acrolein
4. Acrylonitrile
5 Anthracene
6. Benzene
7 Bsnzidine
8. Benzo(a)anthracene
9. Benzo(a)pyrene
10. Benzo(b)fluoranthene ..
1 1. Benzo(g,h,i) perylene ..
12. Benzo(k) fluoranthene
13. Benzyl chloride ...
14. Benzyl butyl phthalate
15. Bis(2-chloroethoxy)
methane.
16. Bis(2-chloroethyl) ether
17. Bis(2-ethylhexyl)
phthalate.
18. Bromodichloro-meth-
ane.
19. Bromoform
20. Bromomethane
21. 4-Bromophenyl phenyl
ether.
22. Carbon tetrachloride ...
23. 4-Chloro-3-methyl phe-
nol.
24. Chlorobenzene ..
25. Chloroethane ....
26. 2-Chloroethylvinyl
ether.
EPA method number2-7
GC
610
610
603
603
610
602
610
610
610
610
610
606
611
611
606
601
601
601
611
601
604
601, 602
601
601
GC/MS
625, 1625B
625, 1625B
624", 1624B.
624", 1624B.
625, 1625B
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, 1625B
624, 1624B
624 1624B
624 1624B
HPLC
610
610
610
605
610
" 610
610
610
610
Other approved methods
Standard Methods
[Edition(s)]
6440 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
6220 B
[18th,19th],
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 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].
6200 B [20th] and
6210 B [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
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
Standard Methods
Online
6410 B-00
6410 B-00
6200 B and C-97.
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6200 B and C-97.
6200 B and C-97.
6200 B and C-97.
6410 B-00
6200 C-97
64 10 B-00, 6420
B-00.
6200 B and C-97
6200 B and C-97.
6200 B and C-97.
ASTM
D4657-92 (99)
D4657-92 (99)
D4657-92 (99)
D4657-92 (99)
04657-92 (99)
D4657-92 (99)
D4657-92 (99)
D4657-92 (99)
Other
See footnote9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote 3, p.1
See footnote9, p.
27
See footnote9, p.
27
See footnote8, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130: See foot-
note6, p. S102
See footnote9, p.
27
See footnote6, p.
27
See footnote 9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130
See footnote 6, p.
27
See footnote3, p.
130
-------
11228
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
27 Chloroform
28 Chloromethane
29. 2-Chloronaph-thalene
30 2-Chlorophenol
31. 4-Chlorophenyl phenyl
ether.
32 Chrysene
33. Dibenzo(a,h)an-
thraoene.
34. Dibromochloro-meth-
ane.
35. 1,2-Dichloro-benzene ..
36. 1,3-Dichloro-benzene ..
37. 1,4-Dichloro-benzene ..
38. 3,3-Dichloro-benzidine
39. Dichlorodifluoro-meth-
ane.
40. 1,1-Dichloroethane
41. 1,2-Dichloroethane
42. 1,1-Dichloroethene
43. trans-1,2-Dichloro-
ethene.
44. 2,4-Dichlorophenol
45. 1 ,2-Dichloro-propan8 ..
46. cis-1,3-Dichloro-
propene.
EPA method number2'7
GC
601
601
612
604
611
610
610
601
601, 602
601, 602
601, 602
601
601
601
601
601
604
601
601
GC/MS
624 1624B
624 1624B ...
625 1625B
625, 1625B ....
625, 1625B ....
625, 1625B ....
625, 1625B
624 1624B
624 1625B
624 1625B
624 1625B
625, 1625B
624, 1624B
624 1624B
624, 1624B
624, 1624B
625, 1625B
624 1624B
624 1624B
HPLC
610
610
605
Other approved methods
Standard Methods
[Edition(s)]
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].
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
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 C [20th] and
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 C [20th] and
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
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], 6200 C
[20th] and 6230
B [18th, 19th].
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], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
Standard Methods
Online
6200 B and C-97
6200 B and C-97.
6410 B-00
64106(00, 6420
B-00.
6410 B-00
6410 B-00
6410 B-00
6200 B and C-97.
6200 C-97
6200 C-97
6200 C-97
64 10 B-00.
6200 C-97.
6200 B and C-97
6200 B and C-97
6200 B and C-97
6200 B and C-97
6410 B-00, 6420
B-00.
6200 B and C-97
6200 B and C-97
ASTM
D4657-92 (99)
D4657-92 (99)
Other
See footnote3, p.
130
See footnote9, p.
27
See footnote 9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote 9, p.
27
See footnote9, p.
.27
See footnote 9, p.
27
See footnote 9, p.
27
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11229
TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
47. trans-1,3-Dichloro-
propene.
48. Diethyl phthalate
49. 2,4-Dimethylphenol
50. Dimethyl phthalate
51. Di-n-butyl phthalate
52. Di-n-octyl phthalate
53. 2,3-Dinitrophenol
54. 2,4-Dinitrotoluene
55. 2,6-Dinitrotoluene
56 Epichlorohydrin
57. Ethylbenzene
58. Ruoranthene
59. Fluorene
60. 1,2,3,4,6,7,8-
Heptachloro-
dibenzofuran.
61. 1,2,3,4,7,8,9-
Heptachloro-
dibenzofuran.
62. 1,2,3,4,6,7,8-
Heptachlorodibenzo-p-
dioxin.
63. Hexachlorobenzene ....
64. Hexachloro-butadiene
65. Hexachlorocyclo-
pentadiene.
66. 1,2,3,4,7,8-
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8-
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9-
Hexachlorodibenzofuran.
69. 2,3,4,6,7,8-
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-
Hexachlorodibenzo-p-
dioxin.
71. 1,2,3,6,7,8-
Hexachlorodibenzo-p-
dioxin.
72. 1,2,3,7,8,9-
Hexachlorodibenzo-p-
dioxin 1613B10.
73. Hexachloroethane
74. ldeno(1,2,3-cd) pyrene
75. IsophoronG
76. Methylene chloride
77. 2-Methyl-4,6-
dinitrophenol.
78. Naphthalene
EPA method number2'7
GC
601
606
604
606
606
606
604
609
609
602
610
610
612
612
612
612
610
609
601
604
610
GC/MS
624, 1624B ....
625 1625B
625 1625B
625 1625B
625, 1625B
625, 1625B
625 1625B
625, 1625B
625 1625B
624, 1624B .. .
625, 1625B
625, 1625B
1613B10.
1613B10.
1613B'0.
625 1625B
625, 1625B
6256, 1625B ..
1613B10.
16138'°.
1613B1".
1613B10.
1613B10.
1613B10.
1613B'0.
625 1625B
625, 1625B
625 1625B
624, 1624B
625, 1625B
625, 1625B
HPLC
610
610
610
610
Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[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 [18th, 19th,
20th],
6410 B[18th, 19th,
20th],
6410 B, 6420 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th).
6410 B [18th, 19th,
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,
20th],
6410 B [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],
6410 B, 6420 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
Standard Methods
Online
6200 B and C-97.
6410 B-00
6410 B-00, 6420
B-00.
64' 10 B-00
6410 B-00
6410 B-00
64106-00,6420
B-00.
6410 B-00
6410 B-00
6200 B and C-97
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6200 C— 97
6410 B-00, 6420
B-00.
6410 B-00
ASTM
D4657-92 (99)
D4657-92 (99)
D4657-92 (99)
Other
See footnote8, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 3, p.
130; See foot-
note 6, p. S102
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote8, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130
See footnote9, p.
27
See footnote °, p.
27
-------
11230
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
79 Nitrobenzene
80. 2-Nitrophenol
81 4-Nitrophenol
82. N-
Nitrosodimethylamine.
83. N-Nitrosodi-n-propyl-
amine.
84. N-
Nitrosodiphenylamine.
85.
Octachlorodibenzofuran.
86. Octachlorodibenzo-p-
dioxin.
87. 2,2'-Oxybis(2-
chloropropane) [also
known as bis(2-
ohloroisopropyl) 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 .
96. 2,3,4,7,8-Pentachloro-
dibenzofuran .
97. 1,2,3,7,8,-
Pentachlorodibenzo-p-
dioxin.
98. Pentachlorophenol
99. Phenanthrene
1 00 Phenol
101. Pyrene
102. 2,3,7,8-Tetra-
chlorodibenzofuran.
103. 2,3,7,8-Tetra-
chlorodibenzo-p-dioxin.
104. 1 , 1 ,2,2-Tetra-chloro
ethane .
105. Tetrachloroethene
106 Toluene
107. 1,2,4-Trichloro-ben-
zene.
EPA method number2.7
GC
609
604
604
607
607
607
611
608
608
608
608
608
608
608
604
610
604
610
601
601
602
612
GC/MS
625, 1625B
625 1625B
625, 1625B
6255, 1625E ...
6255, 1625B ...
6255, 1625B ...
1613B10'.
1613B10.
625, 1625B ....
625 .
625
625
625
625.
625
625
1613B<°.
1613B'0.
1613B'0.
625, 1625B
625, 1625B
625 1625B
625, 1625B
1613B10.
613, 625 5a,
161 3B10.
624 1624B
624 1624B .
624, 1624B ...
625, 1625B
HPLC
610
610
Other approved methods
Standard Methods
[Edition(s)]
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].
6410 B, 6440 B
[18th, 19th, 20th],
6410 B, 6420 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 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],
Standard Methods
Online
6410 B-00
6410 B-00, 6420
B-00.
6410 B-00, 6420
B-00.
6410 B-00
6410 B-00
6410 B-00
6410 B-00.
6410 B-00
6410 B-00
6410 B-00
6410 B-00 .
6410 B-00
6410 B-00
6410 B-00
6410 B-00
6410 B-00, 6420
B-00.
6410 B-00
6200 B and C-97
6200 B and C-97
6200 B and C-97.
6410 B-00
ASTM
D4657-92 (99)
D4657-92 (99)
D4657-92 (99)
Other
See footnote 9, p.
27
See footnote9, p.
27
See footnote8, p.
27
See footnote 9, p.
27
See footnote0, p.
27
See footnote 9, p.
27
See footnote 3, p.
43; See foot-
note a
See footnote 3, p.
43; See foot-
note8
See footnote3, p.
43; See foot-
note8
See footnote3, p.
43; See footnote
8
See footnote 3, p.
43; See footnote
8
See footnote 3, p.
43; See footnote
8
See footnote 3, p.
140; See foot-
note 9, p. 27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 3, p.
130
See footnote 3, p.
130
See footnote 3, p.
130; See foot-
note 9, p. 27
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11231
TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
108. 1,1,1-Triohloro-ethane
1 09. 1,1 ,2-Trichloro-ethane
1 10. Trichloroethene
111. Trichlorofluoro-meth-
ana.
112. 2,4,6-Triohlorophenol
1 13. Vinyl chloride
EPA method number2-7
GC
601
601
601
601
604
601
GC/MS
624, 1624B
624, 1624B
624, 1624B
624
625 1625B
624, 1624B
HPLC
6200 B [20th]
and 6210 B
[18th, 19th],
6200 C [20th]
and 6230 B
[18th, 19th]
Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B[18th, 19th].
6200 B and C-97
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].
6410 B, 6420 B
[18th, 19th, 20th].
6200 B [20th] and
6210 B [18th,
19th], £6200 C
[20th] and 6230
B[18th, 19th].
Standard Methods
Online
6200 B and C-97.
6200 B and C-97.
6200 B and C-97.
6410 B-00, 6420
B-00.
6200 B and C-97.
ASTM
See footnote3, p.
130.
Other
See footnote9, p.
27
'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).
2The 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, "Defini-
tion 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.
•* 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.
5Method 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, or Method 1625B, are preferred methods for these compounds.
5a625, screening only.
6 "Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency," Supplement to the Fifteenth Edition of Standard Meth-
ods for the Examination of Water and Wastewater (1981).
'Each 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 1625B (See Appendix 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) of all samples 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 falls outside the warning limits, the analytical results for
that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control
requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
8"Organochlorine Pesticides and PCBs in Wastewater Using Empore™ 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 Con-
stituents in Water and Fluvial Sediments," U.S. Geological Survey, Open File Report 93-125.
'"Analysts may use Fluid Management Systems, Inc. PowerPrep system in place of manual cleanup provided that the analysis meet the requirements of Method
1613B (as specified in Section 9 of the method) and permitting authorities.
TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1
Parameter
1 . Aldrin
2 Ametryn
3. Aminocarb
4. Atraton
5 Atrazine
6. Azinphos methyl
7. Barban
8. a-BHC . . ..
9. p-BHC
Method
GC
GC/MS
GC
TLC ...
GC .
GC
GC
TLC
GC
GC/MS
GC
GC/MS
EPAs.'
608
625
608
625 5
608
625 6
Standard Methods
18th, 19th, 20th Ed.
6630 B & C
6410 B ..
6630 B & C
6410 B
6630 C
6410 B
Standard Methods
Online
6410 B-00
6410 B-00
64 10 B-00.
ASTM
D3086-90
D5812-96 (2002) '..
D3086-90
05812-96(02)
D3086-90
05812-96(02)
Other
27; See footnote 8
pS68
See footnote3 p 94' See footnote6
p. S16
See footnote3 p 831 See footnote6
p. S68
See footnote3 p 83' See footnote6
p. S68; See footnote6
See footnote3 p 25' See footnote6,
p. S51
See footnote 3 p 1 04' See footnote 6
p. S64
See footnote3 p 7' See footnote8
See footnote 8
-------
11232
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued
Parameter
10 5-BHC
1 1 y-BHC (Lindane)
1 3 Carbaryl
1 5 Chlordane
17 2 4-D
18 4 4'-DDD
19 4 4'-DDE
20 4 4'-DDT
21 DemQton-O
22 Demeton-S
23 Oi37innn
24 Dicamba
27 Dioofol
28 Dieldrin
30 Disulfoton
33 Endosulfan II
35 Endrin
37 Ethion
38 Fenuron
43 Linuron
Method
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
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
EPA"
608
625 5
608
625
608
625
608
625
608
625
608
625
603
625
603
625 5
603
625 5
603
625
603
625 5
603
625
603
625
603
625
Standard Methods
18th, 19th, 20th Ed.
6630 C
6410 B
6630 B & C
6410 B
6630 B
6630 B& C
6410 B
6640 B
6630 B & C
6410 B ... .
6630 B & C
6410 B
6630 B & C
6410 B
6630 B & C
6630 B & C
6410 B
6630 B & C
6410 B
6630 B & C
6410 B
6630 C
6410 B
6630 B & C
6410 B
6630 B& C
6410 B
6630 B&C
6410 B
6630 C ... .
Standard Methods
Online
6410 B-00,
6410 B-00
64 10 B-00.
6410 B-00
6410 B-00.
6410 B-00.
6410 B-00
"
6410 B-00.
6410 B-00
6410 B-00.
6410 B-OO.
6410 B-00
6410 B-00
ASTM
D3086-90
05812-96(02)
D3086-90
05812-96(02)
D3086-90
05812-96(02)
03086-90 .. .
05812-96(02)
D3086-90
05812-96(02)
03086-90
05812-96(02)
03086-90
05812-96(02)
03086-90,
05812-96(02).
03086-90
05812-96(02)
03086-90
05812-96(02)
D3086-90
05812-96(02)
D3086-90
05812-96(02) .. .
03086-90 .
05812- 96(02)
Other
See footnote 8
See footnote3 p 7' See footnote4 p
27; See footnote8
See footnote 3 p 7
See footnote 3 p 94 See footnote 6
p. S60
See footnote4 p 271 See footnote6
p. S73
See footnote3 p 7' See footnote4 p
27; See footnote8
See footnote 3 p 1 04' See footnote 6
p. S64.
See footnote 3 p 115' See footnote 4
p. 40
See footnote3 p 7' See footnote4 p
27; See footnote 8
See footnote3 p 7' See footnote4 p
27; See footnote a
See footnote3 p 7~ See footnote4 p
27; See footnote8
See footnote3 p 25- See footnote6
p. S51
See footnote3 p 25' See footnote6
p. S51
See footnote3, p. 25; See footnote4,
p. 27; See footnote6, p. S51
See footnote3, p. 115
See footnote4 p 27' See footnote6
p. S73
See footnote3 p 7
See footnote3 p 7- See footnote4 p
27; See footnote8
See footnote4 p 27- See footnote6
p. S73
See footnote3, p. 25; See footnote6
p. S51
See footnote3, p. 1041 See footnote6
p. S64
See footnote 3 p 7' See footnote 4 p
27; See footnote8
See footnote3 p 7' See footnote8
See footnote8
See footnote3 p 71 See footnote4 p
27; See footnote8
See footnote8
See footnote4, p 27' See footnote6
p. S73
See footnote3, p. 104; See footnote6,
p. S64
See footnote 3 p 1 04J See footnote 6
p. S64
See footnote3, p. 7; See footnote4, p.
27; See footnote 8
See footnote3 p 71 See footnote4 p
27; See footnote6, p S73; See
footnote8
See footnote4, p. 27; See footnote6,
p. S73
See footnote3, p. 104; See footnote6,
p. S64
See footnote3, p. 25; See footnote4,
p. 27; See footnote6, p. S51
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11233
TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued
Parameter
45 Methiocarb
46 Methoxy-chlor
47 Mexacar-batG
48 Mirex
49 Monuron
50 Monuron-TCA
51 Nuburon
52. Parathion methyl
53, Parathion ethyl .. . .
54. PCNB
55 Perthane
56 Prometon
57 Prometryn
F,R Prnpa7Jr|A
59 Propham
60 Propoxur
61 Secbumeton
62 Siduron
63. Simazine
64 Strobane
65. Swep
66 245-T
67 2 4 5-TP (Silvex)
68. Terbuthylazine
69 Toxaphene
70 Trifluratin
Method
TLC
GC
TLC
GC
TLC
TLC
TLC
GC .
GC
GC . ..
GC
GC
GC
GC
TLC
TLC
TLC
TLC
GC
GC
TLC
GC
GC
GC
GC
GC/MS
GC
EPA 2.'
608
625
Standard Methods
18th, 19th, 20th Ed.
6630 B & C
6630 B & C
6630 C
6630 C
6630 B & C
6630 B & C
6640 B
6640 B
6630 B & C
6410 B
6630 B
Standard Methods
Online
6410 B-00.
ASTM
D3086-90
05812-96(02).
D3086-90
05812-96(02).
03086-90
05812-96(02).
Other
See footnote3, p. 94; See footnote6,
p. S60
See footnote3 p 7' See footnote4, p.
27; See footnote 8
See footnote3 p 941 See footnote6
p.S60
See footnote3 p 7' See footnote4 p.
27
See footnote3 p 104' See footnote6
p. S64
See footnote 3 p 1 04" See footnote 6
p. S64
See footnote 3 p 1 04" See footnote 6,
p. S64
See footnote3, p. 25; See footnote4,
p. 27
See footnote3, p. 25; See footnote4,
p. 27
See footnote3, p. 7
See footnote 4 p 27
See footnote3 p 83' See footnote6
p. S68; See footnote9
See footnote 3 p 83' See footnote 6
p. S68; See footnote9
See footnote3 p 83' See footnote6
p. S68; See footnote9
See footnote 3 p 1 04' See footnote e,
p. S64
See footnote3 p 94' See footnote6
p. S60
See footnote3 p 83' See footnote6
p. S68
See footnote 3 p 1 04' See footnote 6
p. S64
See footnote3, p. 83; See footnote6,
p. S68; See footnote9
See footnote 3 p 7
See footnote3, p. 104; See footnote6,
p. S64
See footnote3 p 1 15' See footnote4
p. 40
See footnote3 p 1 15' See footnote4
p. 40
See footnote3 p 83' See footnote6
p. S68
See footnote 3 p 7' See footnote 4 p
27; See footnote8
See footnote3 p 7' See footnote9
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.
2The full text of Methods 608 and 625 are given at Appendix A, 'Test Procedures for 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 tor Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesti
EPA publication includes thin-layer chromatography (TLC) methods.
sticides in Water and Wastewater," U.S. Environmental Protection Agency, September 1978. This
""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).
5The method may be extended to include cc-BHC. y-BHC. endosulfan I, endosutfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.
6 "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).
'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 falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to dem-
onstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
8"Organochlorine Pesticides and PCBs in Wastewater Using Empore™ Disk", 3M Corporation. Revised 10/28/94.
9USGS 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 wrth Nitrogen Phosphorus Detectors" U.S. Geological Survey Open File Report 94-37.
TABLE IE.—LIST OF APPROVED RADIOLOGIC TEST TEST PROCEDURES
Parameter and units
1 . Alpha-Total, pCi per
liter.
2. Alpha-Counting
error, pCi per liter.
3. Beta-Total, pCi per
liter.
Method
Proportional or scin-
tillation counter.
Proportional or scin-
tillation counter.
Proportional counter
Reference (method number or page)
EPA1
900 0
Appendix B ..
900.0
Standard Meth-
ods 18th, 19th,
20th Ed.
7110 B
7110 B
7110 B
Standard Meth-
ods Online
7110 B-00
7110 B-00
71 1 0 B-00
ASTM
D1943-90, 96 ....
D1 943-90, 96 ....
D1890-90, 96 ....
USGS2
pp. 75 and 78 3
p. 79
pp. 75 and 78 3
-------
11234
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE IE.—LIST OF APPROVED RADIOLOGIC TEST TEST PROCEDURES—Continued
Parameter and units
4. Beta-Counting error,
pCi.
5. (a) Radium Total
pCi per liter.
(b) Ra, pCi per liter ....
Method
Proportional counter ...
Proportional counter
Scintillation counter ....
Reference (method number or page)
EPA1
Appendix B ..
9030
903.1 ;
Standard Meth-
ods 18th, 19th,
20th Ed.
7110 B
7500-Ra B
7500-Ra C
Standard Meth-
ods Online
7110 B-00
7500-Ra B-01 ....
7500-Ra C-01 ....
ASTM
D1 890-90, 96
D2460-90, 97
D3454-91. 97
USGS2
p. 79
D. 81
1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agen-
cy, August 1980.
2Fishman, M. J. and Brown, Eugene, "Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters," U.S. Geological Survey,
Open-File Report 76-177 (1976).
3The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore,
the two results must be added to obtain the "total."
TABLE IG.—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS
EPA Survey
Code
8
12
16
17
22
25
26
27
30
31
35
39
41
45
52
53
54
55
58
60
62
68
69
69
70
73
75
76
80
82
84
86
90
103
107
1 10
1 12
1 13
1 18
1 19
123
124
125
126
127
132
133
138
140
144
148
150
154
156
Pesticide name
Triadimefon
2 4-D1 2 4— D Salts and Esters [2 4— Dichloro-phenoxyacetic acid]
2 4— DB1 2 4— DB Salts and EstGrs [2 4— Dichlorophenoxybutyric acid]
Mevinphos .
MCPA- MCPA Salts and Esters [2-Methyl-4-chlorophenoxyacetic acid]
Dichlorprop; Dichlorprop Salts and Esters [2-(2,4-Dichlorophenoxy) propionic acid]
MCPP; MCPP Salts and Esters [2-(2-Methyl-4-chlorophenoxy) propionic acid]
TCMTB [2-(Thiocyanomethylthio) benzo-thiazole]
Metribuzin
Acephate
Ametryn
Captafol
Chlorothalonil . .
DCPA [Dimethyl 2 3 5 6-tetrachloro-terephthalate]
Dinoseb ... .
Dioxathion
Nabonate [Disodium cyanodithio-imidocarbonate] . .
Endothall .. . .
Ethalfluralin
Glyphosate [N(Phosphonomethyl) glycine]
Heptachlor
Methomvl
CAS No.
43121-43-3
62-73-7
94-75-7
94-82-6
7786-34-7
21725-46-2
1918-16-7
94-74-6
120-36-5
93-65-2
21564-17-O
23950-58-5
709-98-8
21087-64-9
30560-19-1
50594-66-6
15972-60-8
116-06-3
834-12-8
1912-24-9
17804-35-2
314-40-9
1 689-84-5
1689-99-2
23184-66-9
2425-06-1
63-25-2
1 563-66-2
2675-77-6
1 897-45-6
961-11-5
2921-88-2
51630-58-1
333-41-5
298-00-0
1861-32-1
88-85-7
78-34-2
138-93-2
330-54-1
145-73-3
72-20-8
55283-68-6
563-12-2
13194-48-4
60168-88-9
55-38-9
1071-83-6
76-44-8
33820-53-0
330-55-2
121-75-5
10265-92-6
16752-77-5
EPA Analytical Method No.(s)
507/633/525 'l/1 656
1657/507/622/525 1
1658/515 1/615/5152/555
1658/515 1/615/5152/555
1657/507/622/525 1
629/507
1656/508/608 1/525 1
1658/615/555
1658/515.1/615/515 2/555
1658/615/555
637
525 1/507/633 1
632 1/1656
507/633/5251/1656
1656/1657
515 1/515 2/555
505/507/645/525 1/1656
531 1
507/619/525.1
505/507/619/525 1/1656
631
507/633/525 1/1656
1625/1661
1656
507/645/525 1/1656
1656
531 1/632/553
531.1/632
1656/508/608 1/525 1
508/6082/525 1/1656
1657/507/622/525 1
1657/508/622
1660
1657/507/614/622/525 1
1657/614/622
508/6082/525 1/515.1/515.2/1656
1658/515.1/615/5152/555
1657/614.1
630.1
632/553
548/548.1
1656/505/508/608/617/525 1
1 1656/627 See footnote 1
1657/614/614 1
1657/507/622/525 1
507/633 1/525 1/1656
1657/622
547
1 656/505/508/608/6 1 7/525. 1
1 656/627
553/632
1657/614
1657
531.1/632
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Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11235
TABLE IG.—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS—Continued
EPA Survey
Coda
158
172
1 73 ...
175
178
182
183
185
186
192
197
203
204
205
206
208
212
218
219
220
223
224
226
230 ...
232
236
239
241
243
252
254
255
256 . .
257
259
262
263
264
268
Pesticide name
Methoxychlor •
Nabam
Naled . .
Nortlurazon ..
Benfluralin
FGhsulfothion .
Disulfoton
Phosmet
Azinphos Methyl
Organo-tin pesticides
Bolstar
Parathion ....
Pendimethalin
Pentachloronitrobenzene
Pentachlorophenol
Permethrin
Phorate
Busan 85 [Potassium dimethyldithiocarbamate] ....
Busan 40 [Potassium N-hydroxymethyl-N-methyldithiocarbamate]
KN Methyl [Potassium N-methyl-dithiocarbamate]
Prometon , , . .... ...
Prometryn
Propazins . , .
Pyrethrin 1 ... . .,
Pyrethrin II
DEF [S S S-Tributyl phosphorotrithioate] ...
Simazine
Carbam-S [Sodium dimethyldithiocarbanate]
Vapam [Sodium methyldithiocarbamate]
Tebuthiuron
Terbacil
Terbufos . ...
Terbuthylazine
Dazomet
Toxaphene
Merphos [Tributyl phosphorotrithioate]
Trifluralin
Ziram [Zinc dimethvldithiocarbarnatel
CAS No.
72-43-5
142-59-6
300-76-5
27314-13-2
1861-40-1
115-90-2
298-04-4
732-11-6
86-50-0
12379-54-3
35400-43-2
56-38-2
40487-42-1
82-68-8
87_86-5
52645-53-1
298-02-2
128-03-0
51026-28-9
137-41-7
1610-18-0
7287-19-6
1 39-4Q-2
121-21-1
121-29-9
78-48-8
122-34-9
128-04-1
137-42-8
34014-18-1
5902-51-2
13071-79-9
5915-41-3
886-50-0
533-74-4
8001-35-2
150-50-5
1 582-09-8
137-30-4
EPA Analytical Method No.(s)
1656/505/508/608.2/617/525 1
630/630. 1
1657/622
507/645/525.1/1656
11656/1627
1657/622
1657/507/614/622/525 1
1657/622 1
1657/614/622
lnd-01/200 7/200 9
1657/622
1657/614
1656
1656/608 1/617
625/1625/515 2/555/515 1/ 525 1
6082/508/525 1/1656/1660
1657/622
630/630 1
630/630 1
630/630 1
507/619/525 1
507/619/525 1
507/619/525 1/1656
1660
1660
1657
505/507/6 1 9/525. 1 / 1 656
630/630. 1
630/630 1
507/525 1
507/633/525 1/1656
1657/507/614 1/525 1
619/1656
507/619/525 1
630/630 1/1659
1656/505/508/608/617/525 1
1657/507/525.1/622
1656/508/617/627/525 1
630/630.1
1 Monitor and report as total Trifluralin.
(b)***
References, Sources, Costs, and Table
Citations
*****
(6) American Public Health
Association. 1992,1995, and 1998.
Standard Methods for the Examination
of Water and Wastewater. 18th, 19th,
and 20th Edition (respectively).
Available from: American Public Health
Association, 1015 15th Street, NW.,
Washington, DC 20005. Standard
Methods Online are available through
the Standard Methods Web site (http://
www.standardmethods.org). Tables IA,
IB, 1C, ID, IE.
* * * * *
(10) ASTM International. Annual
Book of ASTM Standards, Water, and
Environmental Technology, Section 11,
Volumes 11.01 and 11.02, 1994, 1996,
1999, Volume 11.02, 2000, and
individual standards published after
2000. Available from: ASTM
International, 100 Barr Harbor Drive,
P.O. Box C700, West Conshohocken, PA
19428-2959, or http://www.astm.org.
Tables IA, IB, 1C, ID, and IE.
(17) AOAC-International. Official
Methods of Analysis of AOAC-
International, 16th Edition, (1995).
Available from: AOAC-International,
481 North Frederick Avenue, Suite 500,
Gaithersburg, MD 20877. Table IB, See
footnote 3.
*****
(63) Waters Corporation. Method
D6508, Rev. 2, "Test Method for
Determination of Dissolved Inorganic
Anions in Aqueous Matrices Using
Capillary Ion Electrophoresis and
Chromate Electrolyte," available from
Waters Corp, 34 Maple Street, Milford,
MA 01757, Telephone: 508/482-2131,
Fax: 508/482-3625, Table IB, See
footnote 54.
(64) Kelada-01, "Kelada Automated
Test Methods for Total Cyanide, Acid
Dissociable Cyanide, and Thiocyanate,"
EPA 821-B-01-009 Revision 1.2,
August 2001 is available from National
Technical Information Service (NTIS),
5285 Port Royal Road, Springfield, VA
22161 [Order Number PB 2001-108275].
Telephone: 800-553-6847. Table IB, See
footnote 55.
(65) 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 2.2, March 2005 is available
from Lachat Instruments 6645 W. Mill
Road, Milwaukee, WI 53218, Telephone:
414-358-4200. Table IB, See footnote
56.
(66) "Methods for the Determination
of Metals in Environmental Samples,"
Supplement I, National Exposure Risk
Laboratory-Cincinnati (NERL-CI), EPA/
600/R-94/111, May 1994; and "Methods
for the Determination of Inorganic
Substances in Environmental Samples,"
NERL-CI, EPA/600/R-93/100, August,
1993 are available from National
Technical Information Service (NTIS),
5285 Port Royal Road, Springfield, VA
22161. Telephone: 800-553-6847. Table
IB.
(67) "Determination of Inorganic Ions
in Drinking Water by Ion
Chromatography," Rev. 1.0,1997 is
available from from http://www.epa.gov/
safetwater/methods/metSOO.pdf. Table
IB.
(68) Table IG Methods are available in
"Methods For The Determination of
Nonconventional Pesticides In
-------
11236
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
Municipal and Industrial Wastewater,
Volume I," EPA 821-R-93-010A,
August 1993 Revision I, and "Methods
For The Determination of
Nonconventional Pesticides In
Municipal and Industrial Wastewater,
Volume II," EPA 821-R-93-010B
(August 1993) are available from
National Technical Information Service
(NTIS), 5285 Port Royal Road,
Springfield, VA 22161. Telephone: 800-
553-6847.
(69) Method 245.7, Rev. 2.0, "Mercury
in Water by Cold Vapor Atomic
Fluorescence Spectrometry," February
2005, EPA-821-R-05-001, available
from the U.S. EPA Sample Control
Center (operated by CSC), 6101
Stevenson Avenue, Alexandria, VA
22304, Telephone: 703-461-8056. Table
IB, See footnote 59.
(c) Under certain circumstances, the
Regional Administrator or the Director
in the Region or State where the
discharge will occur may determine for
a particular discharge that additional
parameters or pollutants must be
reported. Under such circumstances,
additional test procedures for analysis
of pollutants may be specified by the
Regional Administrator, or the Director
upon recommendation of the Alternate
Test Procedure Program Coordinator,
Washington, DC.
(d) Under certain circumstances, the
Administrator may approve additional
alternate test procedures for nationwide
use, upon recommendation by the
Alternate Test Procedure Program
Coordinator, Washington, DC.
(e) Sample preservation procedures,
container materials, and maximum
allowable holding times for parameters
are cited in Tables I A, IB, 1C, ID, IE, IF,
and IG are prescribed in Table II.
Information in the table takes
precedence over information in specific
methods or elsewhere. Any person may
apply for a variance from the prescribed
preservation techniques, container
materials, and maximum holding 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 provided to
assure such variance does not adversely
affect the integrity of the sample. Such
data will be forwarded by the Regional
Administrator, to the Alternate Test
Procedure Program Coordinator,
Washington, DC, for technical review
and recommendations for action on the
variance application. Upon receipt of
the recommendations from the Alternate
Test Procedure Program Coordinator,
the Regional Administrator may grant a
variance applicable to the specific
discharge 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 number/name
Table IA— Bacterial Tests:
1-5. Coliform, total, fecal, and E. coli
6 Fecal streptococci
7 Enterococci
Table lA — Protozoan Tests:
9 Giardia
Table IA — Aquatic Toxicity Tests:
Table IB — Inorganic Tests:
1 . Acidity
4. Ammonia
9 Biochemical oxygen demand
14 Biochemical oxygen demand carbonaceous
17 Chlorine total residual
21. Color
23-24 Cyanide total or available (or CATC)
25 Fluoride :
28 Hydrogen ion (pH) ....
31 43 Kjeldah! and organic N
Table IB—Metals: 7
35. Mercurv (CVAA1
Container1
PA, G
PA, G
PA, G
LDPE' field filtration
LDPE; field filtration ...
P FP G
P, FP, G
P, FP, G
P, FP, G
P, FP, G
P FP or Quartz
p FP G
P FP G
P FP G
P FP G
P, G
P, FP, G
P FP G
P
p FP G
P, FP, G
P, FP, G
P FP G
P, FP, G
Preservation2-3
Cool, <10°C,
0.0008%
Na2S2035.
Cool, <10°C
0.0008%
Na:.S203<>.
Cool, <10 °C,
0.0008%
Na2S2O35.
0-8 °C
0-8 °C
Cool £6 °C 1e
Cool, 56 °C18 ..
Cool, S6 °C18 .
Cool, 56 °C18,
H2SO4 to
pH<2.
Cool S6 °C 18
HNOi to pH<2
Cool S6 °C 1S
Cool £6 °C18
H2SO4 to
pH<2.
None required
Cool, 56 °C18 ..
Cool, £6 °C'8
NaOH to
pH>126, re-
ducing
agent5.
None required
HNOi or
H2SO4 to
pH<2.
None required
Cool, £6°C18,
H2SO4 to
pH<2.
Cool <6 °C 18
pH = 9.3-
9.7 ».
HNOri to pH<2
Maximum holding time4
6 hours
6 hours
6 hours
96 hours21
96 hours21
36 hours
14 days
1 4 days
28 days
48 hours
6 months
28 days
48 hours
28 days
28 days
Analyze within 15 minutes
48 hours
14 days
28 days
6 months
Analyze within 15 minutes.
28 days
28 days
28 days
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11237
TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Parameter number/name
35 Mercury (CVAFS)
3, 5-8, 12, 13, 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 mercury.
38. Nitrate
39. Nitrate-nitrite
40. Nitrite
41 Oi! and grease
42. Organic Carbon
44. Orthophosphate
46. Oxygen, Dissolved Probe
47. Winkler
48. Phenols
49 Phosphorous (elemental)
50 Phosphorous total . .
53 Residue, total
54, Residue, Filterable
55 Residue Nonfilterable (TSS)
56 Residue Settleable
57. Residue, Volatile
61. Silica
64 Specific conductance . ..
65. Sulfate
66. Sulfide
67. Sulfite
68. Surfactants
69. Temperature
73. Turbidity
Table 1C — Organic Tests8
13, 18-20, 22, 24-28, 34-37, 39-43
Purgeable Halocarbons.
6, 57, 106. Purgeable aromatic hydroca
3 4. Acrolein and acrylonitrile
23, 30, 44, 49, 53, 77, 80, 81, 98, 100,
7 38 Benzidines" 12 . ..
14, 17, 48, 50-52. Phthalate esters"
82-84. Nitrosamines" 14 ....
88-94 PCBs"
54, 55, 75, 79. Nitroaromatics and isop
45-47, 56, 76, 104, 105, 108-111, 113.
rbons
112. Phenols"
"torone "
Container1
FP, G; and FP-lined
cap 17.
P FP G .
P, FP, G
P, FP, G ....
P, FP, G
G
P, FP, G
P, FP, G
G, Bottle and top
G, Bottle and top
G
G
P FP G
P FP G
P, FP, G ....
P, FP, G
P FP G
P, FP, G ....
P or Quartz
P FP G
P, FP, G
P, FP, G
P, FP, G
P, FP, G
P FP G
P, FP, G ....
G, FP-lined septum ...
G, FP-lined septum ...
G, FP-lined septum ...
G, FP-lined cap
G, FP-lined cap
G, FP-lined cap
G, FP-lined cap
G, FP-lined cap
G, FP-lined cap
Preservation2.3
5 mLA 12N
HCI or 5 mL7
L BrCI '7.
HNO3 to pH<2,
or at least 24
hours prior to
analysis 19.
Cool, 56 °C18 ..
Cool, 56°C18,
H2SO4 to
pH<2.
Cool, £6°C'8 ..
Cool to ..
Cool, 56 °C18,
add zinc ace-
tate plus so-
dium hydrox-
ide to pH>9.
None required
Cool, 56 °C18 ..
None required
Cool, 56 °C18
Cool, 56°C'e,
0.008%
Na2S2O35.
Cool, 56 °C 18,
0.008%
Na2S2035,
HCI to pH 29.
Cool, 56 °C'»,
0.008%
Na2S2O35,
pH to 4-5 '°.
Cool, 56 °C<8,
0.008%
Na2S2O3s.
Cool, 56 °C18,
0.008%
Na2S2O35.
Cool, 56 °C'8 ..
Cool, 56 °C 18,
store in dark,
0.008%
Cool, 56 "C18 ..
Cool, 56 °C'S,
store in dark,
0.008%
Na2S2O35.
Maximum holding time4
90 days '7
6 months
48 hours
28 days
48 hours
28 days
28 days
Filter within 15 minutes; Ana-
lyze within 48 hours
Analyze within 15 minutes
8 hours
28 days
48 hours
28 days
7 days
7 days
7 days
48 hours
7 days
28 days
28 days
28 days
7 days
Analyze within 15 minutes
48 hours
Analyze
48 hours
14 days
14 days9
14 days10
7 days until extraction, 40 days
after extraction
7 days until extraction 13
7 days until extraction, 40 days
after extraction
7 days until extraction, 40 days
after extraction
1 year until extraction, 1 year
after extraction
7 days until extraction, 40 days
after extraction
-------
11238
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Parameter number/name
1, 2, 5, 8-12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons11
15 16 21 31 87 Haloethers11
29 35-37 63-65 107. Chlorinated hydrocarbons11
60-62, 66-72, 85, 86, 95-97, 102, 103. CDDs/CDFs".
Aqueous Samples' Field and Lab Preservation .
Solids and Mixed-Phase Samples' Field Preservation
Tissue Samples: Field Preservation .. .
Solids Mixed-Phase and Tissue Samples1 Lab Preservation
Table ID— Pesticides Tests:
1 70 Pesticides ' 1
Table IE— Radiological Tests:
1—5 Alpha beta and radium
Container1
G, FP-lined cap
G FP-lined cap
G, FP-lined cap
G
G
G
G
G, FP-lined cap
P FP, G
Preservation2'3
Cool, S6 °C 12 with sodium hydroxide solution (e.g.. 5 % w/v), refrigerate as specified, and analyze within 48 hours. Otherwise, to extend the holding time to
14 days and mitigate interferences, treat the sample immediately using any or all of the following techniques, as necessary, followed by adjustment of the sample pH to >12 and refrigeration
as specified. There may be interferences that are not mitigated by approved procedures. Any procedure for removal or suppression of an interference may be employed, provided the labora-
tory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g., ferric ferrocyanide) or a strong cyanide complex (e.g., cobalt cyanide) are more accurately measured if
the laboratory holds the sample at room temperature and pH >12 for a minimum of 4 hours prior to analysis, and performs UV digestion or dissolution under alkaline (pH-12) conditions, if
necessary.
(1) Sulfur: To remove elemental sulfur (S8), fitter the sample immediately. If the filtration time will exceed 15 minutes, use a larger filter or a method that requires a smaller sample volume
(e.g. EPA Method 335.4 or Lachat Method 01). Adjust the pH of the filtrate to >12 with NaOH, refrigerate the filter and filtrate, and ship or transport to the laboratory. In the laboratory, ex-
tract the filter with 100 mL of 5% NaOH solution for a minimum of Z hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower trra
pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate
from the solids, test the sample with and without the solids procedure if a tow detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is ob-
tained w|thout it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in ug or mg), and divide by the original sample volume to obtain
the cyanide concentration.
(2) Sulfide: If the sample contains sulfide as determined by lead acetate paper, or if sulfide is known or suspected to be present, immediately conduct one of the volatilization treatments or
the precipitation treatment as follows: Volatilization—Headspace expelling. In a fume hood or well-ventilated area, transfer 075 Itter of'sample to a 4.4-L collapsible container (e.g.,
Cubitainer™). Acidify with concentrated hydrochloric acid to pH <2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel the headspace into the fume hood or
open area by collapsing the container without expelling the sample. Refill the headspace by expanding the container. Repeat expelling a total of five headspace volumes. Adjust the pH to
>12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio. A larger volume of air will result in too
great a loss of cyanide (> 10%). Dynamic stripping: In a fume hood or well-ventilated area, transfer 0.75 liter of sample to a container of the material specified and acidify wrth concentrated
hydrochloric acid to pH <2. Using a calibrated air sampling pump or flowmeter. purge the acidified sample into the fume hood or open area through a fritted glass aerator at a flow rate of
2.25 L/min for 4 minutes. Adjust the pH to >12. refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio.
A larger volume of air will result in too great a toss of cyanide (>10%). Precipitation: If the sample contains paniculate matter that would be removed by filtration, filter the sample prior to
treatment to assure that cyanide associated with the paniculate matter is included in the measurement. Ship or transport the filter to the laboratory. In the laboratory, extract the filter with 100
mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12
with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the
sample with and without the solids procedure if a tow detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alter-
natively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in ug or mg), and divide by the original sample volume to obtain the cyanide concentra-
tion. For removal of sulfide by precipitation, raise the pH of the sample to >12 with NaOH solution, then add approximately 1 mg of powdered cadmium chloride for each mL of sample. For
example, add approximately 500 mg to a 500-mL sample. Cap and shake the container to mix. Allow the precipitate to settle and test the sample with lead acetate paper. If necessary, add
cadmium chloride but avoid adding an excess. Finally, filter through 0.45 micron filter. Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the labora-
tory, extract the filter with 100 mL of 5% NaOH solution tor a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate,
lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate form the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure If a higher cyanide concentra-
tion is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in (g or mg), and divide by the original sample volume to
obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM D6888), it may be necessary to increase the ligand-exchange reagent to offset any excess of cadmium
chloride.
(3) Sulfite, thiosulfate, or thiocyanate: If sulfite, thiosulfate, or thiocyanate is known or suspected to be present, use UV digestion with a glass coil (Method Kelada-01) or ligand exchange
(Method OIA-1677) to preclude cyanide loss or positive interference.
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Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11239
(4) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be present, treat the sample with 20 ml of 3.5% ethylenediamine solution per liter
of sample.
(5) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the distillation flask, a reduction in the pH of the absorber solution, and incomplete cya-
nide spike recovery. When significant carbonate is present, adjust the pH to > 12 using calcium hydroxide instead of sodium hydroxide. Allow the precipitate to settle and decant or filter the
sample prior to analysis (also see Standard Method 4500-CN B 3 d)
(6) Chlorine, hypochlonte, or other oxidant: Treat a sample known or suspected to contain chlorine, hypochlorite, or other oxidant as directed in footnote 5.
'For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives. For a composite sample collected with an automated sampler (e.g., using a 24-
hour composite sampler; see 40 CFR 122.21 (g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of collection and before adding preservatives. If it
is known or suspected that dissolved sample integrity will be compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between
dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically.
'Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
* If the sample is not adjusted to pH 2. then the sample must be analyzed within seven days of sampling.
10The 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.
11 When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed tor optimum safeguard of
sample integrity (i.e., use all necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two or more chemical categories, the sample may be pre-
served by cooling to <6 °C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for
seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
thiosulfate reduction), and footnotes 12. 13 (regarding the analysis of benzidine).
12 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.
13 Extracts may be stored up to 30 days at <0 °C.
"For the analysis of diphenylnitrosamine. add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours of sampling.
15The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add
0.008% Na2S2p3.
16Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still present when the samples 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 preservation temperature maximum has not been exceeded. In the iso-
lated cases where it can be documented that this holding temperature cannot 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.
"Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be collected in tightly-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 '
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11240
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
criteria of the approved method at this
part.
(5) Method-defined Analyte means an
analyte defined solely by the method
used to determine the analyte. Such an
analyte may be a physical parameter, a
parameter that is not a specific
chemical, or a parameter that may be
comprised of a number of substances.
Examples of such analytes include
temperature, oil and grease, total
suspended solids, total phenolics,
turbidity, chemical oxygen demand, and
biochemical oxygen demand.
(6) QC means "quality control."
(b) Method Modifications.
(1) Allowable Changes. Except as set
forth in paragraph (b)(3) of this section,
an analyst may modify an approved test
procedure (analytical method) provided
that the chemistry of the method or the
determinative technique is not changed,
and provided that the requirements of
paragraph (b)(2) of this section are met.
(i) Potentially acceptable
modifications regardless of current
method performance include changes
between automated and manual discrete
instrumentation; changes in the
calibration range (provided that the
modified range covers any relevant
regulatory limit); changes in equipment
such as using similar equipment from a
vendor other than that mentioned in the
method (e.g., a purge-and-trap device
from OIA rather than Tekmar), changes
in equipment operating parameters such
as changing the monitoring wavelength
of a colorimeter or modifying the
temperature program for a specific GC
column; changes to chromatographic
columns (treated in greater detail in
paragraph (d) of this section); and
increases in purge-and-trap sample
volumes (provided specifications in
paragraph (e) of this section are met).
The changes are only allowed provided
that all the requirements of paragraph
(b)(2) of this section are met.
(ii) If the characteristics of a
wastewater matrix prevent efficient
recovery of organic pollutants and
prevent the method from meeting QC
requirements, the analyst may attempt
to resolve the issue by using salts as
specified in Guidance on Evaluation,
Resolution, and Documentation of
Analytical Problems Associated with
Compliance Monitoring (EPA 821-B-
93-001, June 1993), provided that such
salts do not react with or introduce the
target pollutant into the sample (as
evidenced by the analysis of method
blanks, laboratory control samples, and
spiked samples that also contain such
salts) and that all requirements of
paragraph (b)(2) of this section are met.
Chlorinated samples must be
dechlorinated prior to the addition of
such salts.
(iii) If the characteristics of a
wastewater matrix result in poor sample
dispersion or reagent deposition on
equipment and prevents the analyst
from meeting QC requirements, the
analysts may attempt to resolve the
issue by adding an inert surfactant (i.e.
a surfactant that will not affect the
chemistry of the method), which may
include Brij-35 or sodium dodecyl
sulfate (SDS), provided that such
surfactant does not react with or
introduce the target pollutant into the
sample (as evidenced by the analysis of
method blanks, laboratory control
samples, and spiked samples that also
contain such surfactant) and that all
requirements of paragraph fb)(2) of this
section are met. Chlorinated samples
must be dechlorinated prior to the
addition of such surfactant.
(2) Requirements. A modified method
must produce equivalent performance to
the approved methods for the analyte(s)
of interest, and the equivalent
performance must be documented.
(i) Requirements for Establishing
Equivalent Performance
(A) If the approved method contains
QC tests and QC acceptance criteria, the
modified method must use these QC
tests and the modified method must
meet the QC acceptance criteria. The
Analyst may only rely on QC tests and
QC acceptance criteria in a method if it
includes wastewater matrix QC tests
and QC acceptance criteria (e.g., as
matrix spikes) and both initial (start-up)
and ongoing QC tests and QC
acceptance criteria.
(B) If the approved method does not
contain QC tests and QC acceptance
criteria, or if the QC tests and QC
acceptance criteria in the method do not
meet the requirements of paragraph
(b)(2)(i)(A) of this section, the analyst
must employ QC tests specified in
Protocol for EPA Approval of Alternate
Test Procedures for Organic and
Inorganic Analytes in Wastewater and
Drinking Water (EPA-821-B-98-002,
March 1999) and meet the QC
provisions specified therein. In
addition, the Analyst must perform on-
going QC tests, including assessment of
performance of the modified method on
the sample matrix (e.g., analysis of a
matrix spike/matrix spike duplicate pair
for every twenty samples of a discharge
analyzed), and analysis of an ongoing
precision and recovery sample and a
blank with each batch of 20 or fewer
samples.
(C) Calibration must be performed
using the modified method and the
modified method must be tested with
every wastewater matrix to which it will
be applied (up to nine distinct matrices;
as described in the ATP Protocol, after
validation in nine distinct matrices, the
method may be applied to all
wastewater matrices), in addition to any
and all reagent water tests. If the
performance in the wastewater matrix or
reagent water does not meet the QC
acceptance criteria the method
modification may not be used.
(D) Analysts must test representative
effluents with the modified method, and
demonstrate that the results are
equivalent or superior to results with
the unmodified method.
(ii) Requirements for Documentation.
The modified method must be
documented in a method write-up or an
addendum that describes the
modification(s) to the approved method.
The write-up or addendum must
include a reference number (e.g.,
method number), revision number, and
revision date so that it may be
referenced accurately. In addition, the
organization that uses the modified
method must document the results of
QC tests and keep these records, along
with a copy of the method write-up or
addendum, for review by an auditor.
(3) Restrictions. An analyst may not
modify an approved analytical method
for a method-defined analyte. In
addition, an analyst may not modify an
approved method if the modification
would result in measurement of a
different form or species of an analyte
(e.g., a change to a metals digestion or
total cyanide distillation). An analyst
may also may not modify any sample
preservation and/or holding time
requirements of an approved method.
(c) Analytical Requirements for Multi-
analyte Methods (Target Analytes). For
the purpose of NPDES reporting, the
discharger or permittee must meet QC
requirements only for the analyte(s)
being measured and reported under the
NPDES permit.
(d) The following modifications to
approved methods are authorized in the
circumstances described below:
(1) Capillary Column. Use of a
capillary (open tubular) GC column
rather than a packed column is allowed
with EPA Methods 601-613, 624, 625,
and 1624B in Appendix A to this part,
provided that all QC tests for the
approved method are performed and all
QC acceptance criteria are met. When
changing from a packed column to a
capillary column, retention times will
change. Analysts are not required to
meet retention time specified in the
approved method when this change is
made. Instead, analysts must generate
new retention time tables with capillary
columns to be kept on file along with
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11241
other startup test and ongoing QC data,
for review by auditors.
(2) Increased sample volume in purge
and trap methodology. Use of increased
sample volumes, up to a maximum of 25
mL, is allowed for an approved method,
provided that the height of the water
column in the purge vessel is at least 5
cm. The analyst should also use one or
more surrogate analytes that are
chemically similar to the analytes of
interest in order to demonstrate that the
increased sample volume does not
adversely affect the analytical results.
PART 141—NATIONAL PRIMARY
DRINKING WATER REGULATIONS
• 11. The authority citation for part 141
continues to read as follows:
Authority: 42 U.S.C. 300f, 300g-l, 300g-2,
300g-3, 300g-4, 300g-5, 300g-6, 300J-4,
300J-9, and300j-ll.
• 12. Section 141.21 is amended by
adding four sentences to the end of
footnote 1 to the Table in paragraph
(f)(3) to read as follows:
§141.21 Coliform sampling.
*****
ffl* * «
(3)* * *
i* * * in addition, the following
online versions may also be used: 9221
A, B, D-99, 9222 A, B, C-97, and 9223
B-97. Standard Methods Online are
available at http://
www.standardmethods.org. The year in
which each method was approved by
the Standard Methods Committee is
designated by the last two digits in the
method number. The methods listed are
the only Online versions that may be
used.
*****
• 13. Section 141.23 is amended as
follows:
• a. In paragraph (a)(4)(i) by revising the
table entries for "Cyanide," "Nitrate,"
and "Nitrite".
• b. In paragraph (k)(l) by revising the
table.
§ 141.23 Inorganic chemical sampling and
analytical requirements.
(a)
DETECTION LIMITS FOR INORGANIC CONTAMINANTS
Contaminant
MCL (mg/L)
Methodology
Detection Limit (mg/L)
Cyanide 0.2
Distillation, Spectrophotometric3
Distillation, Automated, Spectrophotometric3
Distillation, Amenable, Spectrophotometric4
Distillation, Selective Electrode3.4
UV, Distillation, Spectrophotometric9
Micro Distillation, Flow Injection, Spectrophotometric3
Ligand Exchange with Amperometry*
0.02
0.005
0.02
0.05
0.0005
0.0006
0.0005
Nitrate 10 (as N)
Nitrite 1 (as N)
Manual Cadmium Reduction
Automated Hydrazine Reduction
Automated Cadmium Reduction .
Ion Selective Electrode
Ion Chromatography
Capillary Ion Electrophoresis
Spectrophotometric
Automated Cadmium Reduction .
Manual Cadmium Reduction
Ion Chromatography
Capillary Ion Electrophoresis
0.01
0.01
0.05
1
0.01
0.076
0.01
0.05
0.01
0.004
0.103
3 Screening method for total cyanides.
« Measures "free" cyanides when distillation, digestion, or ligand exchange is omitted.
9 Measures total cyanides when UV-digestor is used, and "free" cyanides when UV-digestor is bypassed.
00'
Contaminant
1 Alkalinity
2. Antimony
3. Arsenic'4
Methodology 13
Electrometric titration
Inductively Coupled Plas-
ma (ICP)— Mass Spec-
trometry.
Hydride-Atomic Absorp-
tion.
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Inductively Coupled Plas-
ma15.
ICP-Mass Spectrometry
EPA
200.82
200.9 2
200.72
200.8 2
ASTM3
01067-92 02 B
D3697-92 02
SM4(18th, 19th
ed.)
2320 B
3113B
3120 B
SM4(20thed.)
2320 B
3120 B
SM Online22
2320 B-97
1-1030-85 5.
3113 B-99
3120 B-99
Other
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11242
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
Contaminant
4 Asbestos
6. Beryllium
12 Cyanide
1 4 Lead
Methodology '3
Atomic Absorption; Plat-
form.
Atomic Absorption* Fur-
nace.
lion.
Transmission Electron
Microscopy.
Transmission Electron
Microscopy.
ma.
CP-Mass Spectrometry
nace.
nductively Coupled Plas-
ma.
CP-Mass Spectrometry
Atomic Absorption; Plat-
form.
nace.
Inductively Coupled Plas-
ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption' Fur-
nace.
EDTA titrimetric
Aspiration.
ma.
ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
nace.
nace.
Aspiration.
ma.
ICP-Mass Spectrometry ..
Atomic Absorption; Plat-
form.
Manual Distillation fol-
lowed by
Spectrophotometric
Amenable.
Manual.
Spectra-photometric
Semi-automated.
UV Distillation
Spectrophotometric.
Micro Distillation Flow
Injection,
Spectrophotometric.
Amperometry21.
SPADNS.
phoresis.
nace.
ICP-Mass Spectrometry
EPA
200.9 2
100. 19
100.2 10
200 7 2
200.8 2
200.72
200.8 2
200.9 2
200.72
200.82
200.9 2
200 7 2
200 7 2
200.8 2
200.92
200 7 2
200.82
200.9 2
335.4 6
300 O6
300.1 19
200.8 2
ASTM3
D2972-97 03 C
D2972-97 03 B
D3645-97 03 B
D511-93 03 A
D51 1-93 03 B
D69 19-03
D1688-95 02 C
D 1688-95 02 A
D1 125-95 (Reapproved
1999) A.
D2036-98A
D2036-98 B
D2036-98A
D6888-04
D4327-97 03
D1179-93 99 B
D3559-96 03 D
SM»(18th, 19th
ed.)
3113 B ..
3114 B
3120 B
3111D
3113 B
3120 B
3113 B
3113 B
3500-Ca D ..
3111 B
3120 B .. .
3120 B
3113 B
3113 B
3111 B
3120 B
2510 B
4500-CN- C ..
4500-CN- G ..
4500-CN- E ..
4500-CN- F
4110 B
4500-F- B D
4500-F- C
4500-F- E ... .
3113 B
SM« (20th ed.)
3120 B
3120 B
3500-Ca B
3120 B
3120 B
3120 B
2510 B
4500-CN- C.
4500-CN- G ..
4500-CN- E ...
4500-CN- F ...
4110 B
4500-F " B D
4500-F- C
4500-F- E
SM Online22
3113 B-99
3114 B 97
3120 B 99
3111 D 99
3113 B-99
31208-99.
3113 B-99
3113 B-99
3500-Ca B-97.
3111 B-99
3120 B-99
3120 B-99
3113 B-99
3113 B-99
3111 B-99
3120 B-99
2510 B-97.
4500-CN- G-
99.
4500-CN- E-
99.
4500-CN- F-
99.
4110 B-00
4500-F- B D-
97.
4500-F- C-97.
4500-F- E-97
31 13 B-99.
Other
I-3300-85 5
Kelada-01 17
QuikChem 10-
204-00-1-
X18
OIA-1677
DW20
380-75WE11
129-71W"
D6508, Rev.
223
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Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11243
Contaminant
15. MagnGsium . .
16. Mercury
17. Nickel
18. Nitrate
19. Nitrite
20. Ortho-phos-
phate12.
21. pH
22 Selenium
23. Silica
24. Sodium
25. Temperature
26. Thallium
Methodology "
Atomic Absorption; Plat-
form.
Differential Pulse Anodic
Stripping Voltametry.
Atomic Absorption
ICP
Complexation Titrimetric
Methods.
Manual, Cold Vapor
Automated, Cold Vapor ..
ICP-Mass Spectrometry
Inductively Coupled Plas-
ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Ion Chromatography
Automated Cadmium Re-
duction.
Manual Cadmium Reduc-
tion.
Capillary Ion Electro-
phoresis.
Ion Chromatography
Automated Cadmium Re-
duction.
Manual Cadmium Reduc-
tion.
Spectrophotometric
Capillary Ion Electro-
phoresis.
Colorimetric Automated
Ascorbic Acid.
Colorimetric ascorbic
acid, single reagent.
Colorimetric
Phosphomolybdate;
Automated-seg-
mented flow;
Ion Chromatography
Capillary Ion Electro-
phoresis.
Electrometric
tion.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Colorimetric Molybdate
Blue.
mented Flow.
Colorimetric
Molybdosilicate
Heteropoly blue
Automated for Molyb-
date-reactive Silica.
Inductively Coupled Plas-
ma.
Inductively Coupled Plas-
ma.
Atomic Absorption' Direct
Aspiration.
Thermometric
ICP-Mass Soectrometrv
EPA
200.9 2
200 7 2
245.1 2
245.2 1
200.82
200.72 ..
200.82
200.92
300.0 6
300.1 '»
353.2 6 ..
300 Oe
300.1 «
3S3.26
365 1 6 .
300.0 e ..
300.1 ">
150.1,
150.2'
200.82
200.9 2
200.7 2 ..
200.72
200.8 2
ASTM3
0511-93 03 B
0511-93, 03 A
069 1 9-03
D3223-97 02
04327-97 03
03867-90 A
D3867-90 B
04327-97 03
03867-90 A
03867-90 B
0515-88 A
04327-97 03
01293-95 99
03859-98 03 A
D3859-98 03 B
0859-94 00
D69 19-03
SM"(18th, 19th
ad.)
3111 B
3120 B
3500-Mg E
3112B
3120 B
3111 B
3113 B
4110 B
4500-NO3- F
4500-NO3~ 0
4500-NO3- E
4110 B
4500-NO3- F
4500-NO3- E
4500-NO2~ B
4500-P F
4500-P E
4110 B
4500-H+ B
3114 B
3113 B
4500-Si D
4500-Si E .. .
4500-Si F
3120 B
3111 B
2550
SM4(20thed.)
3120 B
3500-Mg B
3120 B
4110 B
4500-NO3- F
4500-NO3~ D
4500-NO3- E
4110 B
4500-NO3^ F
4500-NO3- E
4500-NO2~ B
4500-P F
4500-P E
4110B
4500-H + B
4500-SiC>2 C
4500-SiO2 D
4500-Si02 E
3120 B
2550
SM Online22
3111 B-99.
3120 B-99.
3500-Mg B-97.
3112 B-99.
3120 B-99.
3111 B-99
3113 B-99.
4110 B-00
4500-NO3~ F-
00.
4500-NO3- D-
00.
4500-NO3- E-
00.
4110 B-00
4500-NO3- F-
00.
4500-NO3- E-
00.
4500-NO2- B-
00.
4110 B-00.
4500-H* B-00.
3114 B-97
3113 B-99
4500-SiO2 C-
97.
4500-SiO2 D-
97.
4500-SiO2 E-
97.
3120 B-99
3111 B 99
2550-00
Other
Method 1001 ie
B-1011 8
601 7
D6508, Rev.
223
B-10118
D6508, Rev.
2 23
I-1601-856
1-2601 -90 5
I-2598-85 5
D6508, Rev.
223
1-1 700-85 6
I-2700-85 5
•
-------
11244
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
Contaminant
Methodology <3
Atomic Absorption; Plat-
form.
EPA
200.9 2.
ASTM3
SM4(18th, 19th
ed.)
SM'(20thed.)
SM Online22
Other
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents listed in footnotes 1-11, 16-20, and 22-23 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. Informa-
tion 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 3334, Washington, DC 20460 (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:ffwww.archives.gov/federal_'Bgister/code ot_federal_regulations/ibr_locations.html.
' "Methods for Chemical Analysis of Water and Wastes." ipA/600<4-79/020. March 1983. Available at NTIS,~PB84-128677.
2 "Methods for the Determination of Metals in Environmental Samples—Supplement I." EPA/600/R-94/111, May 1994. Available at NTIS, PB95-125472.
sAnnual Book of ASTM Standards, 1994, 1996, 1999, or 2003, 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 Conshohocken, PA 19428.
'Standard Methods for the Examination ot 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, 3113 B and 3114 B in the 20th
edition may not be used. •
5Method 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 1-1030-85, 1-1601-85; 1-1700-85; I-2598-85; I-2700-85; and I-3300-85 See Techniques of Water Resources Investigation of the
U.S. Geological Survey, Book 5, Chapter A-1. 3rd edition.. 1989; Available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.
""Methods for the Determination of Inorganic Substances in Environmental Samples," EPA/600/R-93/100, August 1993. Available at NTIS, PB94-120821.
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, Boston, MA 02129.
"Method B-1011. "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography," August 1987. Copies may be obtained from Waters Cor-
poration Technical Services Division, 34 Maple Street, Milford, MA 01757. Telephone: 508/482-2f31, Fax: 508/482-3625.
"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.
'"Method 100.2, "Determination of Asbestos Structure Over 10-um 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 Wastevvater," December 1972, and Method No. 380-75WE, "Fluoride in Water and Wastewater," February 1976, Technicon In-
dustrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089.
12 Unfittered, no digestion or hydrolysis.
w 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 pneu-
matic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and
lead by Method 3113 B; and lead by Method D3559-90D, unless multple in-furnace depositions are made.
14lf 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 yl of 30%
hydrogen peroxide per 100 ml of solution. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain 1 mg/L of sodium hypochlorite.
15Starting 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 0.05 mg/L may not be used for compliance determinations Tor 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.
'«The 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.
17The description for the Kelada-01 Method, "Kelada Automated "est Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate," Revision 1.2, August 2001, EPA # 821-B-
..i a given instrument. Similarly _. ......... , ., . . ..
1»The 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 Hd., Milwaukee, Wl 53218. Telephone: 414-358-4200.
""Methods for the Determination of Organic and Inorganic Compounds in Drinking Water," Vol. 1, EPA 815-R-00-014, August 2000. Available at NTIS, PB2000-106981.
20Method OIA-1677, DW "Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry," January 2004. EPA-821-R-04-001, Available from ALPKEM, A Division of Ol Ana-
lytical, P.O. Box 9010, College Station, TX 77842-9010.
21 Sulfide levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide method to determine if a sulfide in-
terference is present, and treat samples accordingly.
^Standard Methods Online are available at http^/www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last
two digits in the method number. The methods listed are the only online versions that may be used.
23Method D6508 Rev 2, 'Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte," available from
Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
• 14. Section 141.24 is amended as
follows:
• a. By revising the introductory text of
paragraph (e)(l).
• b. By revising entries 23, 24, 26, 30,
49, and 50 in the table to paragraph
c. By adding a new footnote 5 to the
table to paragraph (e)(l).
§141.24 Organic chemicals, sampling and
analytical requirements.
*****
(e)* * *
(1) The following documents are
incorporated by reference. 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, 1301 Constitution Avenue, NW.,
EPA West, Room 3334, Washington, DC
20460 (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/
federal_register/
code_of_federal_regulations/
ibr_locations.html. Method 508A and
515.1 are in Methods for the
Determination of Organic Compounds
in Drinking Water, EPA/600/4-88-039,
December 1988, Revised, July 1991.
Methods 547, 550 and 550.1 are in
Methods for the Determination 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-92-129, 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 Isotope-Dilution HRGC/HRMS,"
EPA/821-B-94-005, October 1994.
These documents are available from the
National Technical Information Service,
NTIS PB91-231480, PB91-146027,
PB92-207703, PB95-261616 and PB95-
104774, U.S. Department of Commerce,
5285 Port Royal Road, Springfield,
Virginia 22161. The toll free number is:
800-553-6847. Method 6651 shall be
followed in accordance 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 accordance 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 Examination
of Water and Wastewater; any of these
publications may be used. The APHA
documents are available from APHA,
1015 Fifteenth Street NW., Washington,
DC 20005. Other required analytical test
procedures germane to the conduct of
these analyses are contained in
Technical Notes on Drinking Water
Methods, EPA/600/R-94-173, October
1994, NTIS PB95-104766. EPA Methods
515.3 and 549.2 are available from U.S.
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11245
Environmental Protection Agency,
National Exposure Research Laboratory
(NERL)-Cincinnati, 26 West Martin
Luther King Drive, Cincinnati, OH
45268. ASTM Method D 5317-93, 98
(Reapproved 2003) is available in the
Annual Book of ASTM Standards,
(1999), Vol. 11.02, ASTM International,
100 Barr Harbor Drive, West
Conshohocken, PA 19428, any edition
containing the cited version of the
method may be used. EPA Method
515.4, "Determination of Chlorinated
Acids in Drinking Water by Liquid-
Liquid Microextraction, Derivatization
and Fast Gas Chromatography with
Electron Capture Detection," Revision
1.0, April 2000, EPA/815/B-00/001 and
EPA Method 552.3, "Determination of
Haloacetic Acids and Dalapon in
Drinking Water by Liquid-Liquid
Microextraction, Derivatization, and Gas
Chromatography with Electron Capture
Detection," Revision 1.0, July 2003, EPA
815-B-03-002, can be accessed and
downloaded directly online at http://
www.epa.gov/safewater/methods/
sourcalt.html. Syngenta Method AG-
625, "Atrazine in Drinking Water by
Immunoassay," February 2001, is
available from Syngenta Crop
Protection, Inc., 410 Swing Road, P.O.
Box 18300, Greensboro, NC 27419.
Telephone: 336-632-6000. Method
531.2 "Measurement of N-
methylcarbamoyloximes and N-
methylcarbamates 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
directly online at http://www.epa.gov/
safewater/methods/sourcalt.html.
Contaminant
EPA Method'
Standard
Methods
ASTM
Other
23. 2,4-D4 (as acids, salts, and esters)
24. 2,4,5-TP< (Silvex)
515.2, 555,
515.1, 515.3,
515.4.
515.2, 555,
515.1, 515.3,
515.4.
D5317-93, 98
(Reapproved
2003).
D5317-93, 98
(Reapproved
2003).
26. Atrazine 2 .
507, 525.2,
508.1,505,
551.1.
Syngenta5 AG-625
30. Dalapon
552.1 515.1,
552.2, 515.3,
515.4, 552.3.
49. Pentachlorophenol ...
50. Picloram4
515.2,525.2,
555, 515.1,
515.3, 515.4.
515.2, 555,
515.1, 515.3,
515.4.
05317-93,98
(Reapproved
2003).
05317-93,98
(Reapproved
2003).
1 For previously approved EPA methods which remain available for compliance monitoring until June 1, 2001, see paragraph (e)(2) of this sec-
tion.
Substitution of the detector specified in Method 505, 507, 508, or 508.1 for the purpose of achieving lower detection limits is allowed as fol-
lows: Either an electron capture or nitrogen phosphorus detector may be used provided all regulatory requirements and quality control criteria are
met.
4Accurate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA Methods 515.1, 515.2, 515.3, 515.4,
and 555 and ASTM Method D 5317-93, 98 (Reapproved 2003).
6 This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for drinking water treatment. In sam-
ples from all other systems, any result for atrazine generated by Method AG-625 that is greater than one-half the maximum contaminant level
(MCL) (in other words, greater than 0.0015mg/L or 1.5 ug/L) must be confirmed using another approved method for this contaminant and should
use additional volume of the original sample collected for compliance monitoring. In instances where a result from Method AG-625 triggers such
confirmatory testing, the confirmatory result is to be used to determine compliance.
• 15. Section 141.25 is amended by
revising the table in paragraph (a) to
read as follows:
§141.25 Analytical methods for
radioactivity.
(a)* * *
Contaminant
Naturally Occurring:
Gross alpha" and beta
Gross alpha11
Methodology
Evaporation
Coprecipitation
Reference (Method of Page Number)
EPA1
900.0
EPA2
p. 1 ...
EPA3
00-01
00-02
EPA"
p. 1
SM5
302,71108,
7110B-00.
7110 C, 7110
C-00.
ASTM6
USGS7
R-1 120-76.
DOE»
Other
-------
11246
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
Contaminant
Radium 228
Man-Made:
Radioactive Iodine
Radioactive Strontium 89,
90.
Methodology
Radon emanation ...
Radiochemical
Radiochemical
Radiochemical
Fluorometric
ICP-MS
Alpha Spectrometry
Laser
Phosphorimetry.
Radiochemical
Gamma Ray Spec-
trometry.
Radiochemical
Gamma Ray Spec-
trometry.
Radiochemical
Liquid Scintillation ..
Gamma Ray Spec-
trometry.
Reference (Method of Page Number)
EPA'
903.1
903.0
904.0
908.0
908.1
200.8"
901.0
901.1
902.0
901.1
905.0
906.0
901.1
902.0
901.0
EPA* EPA3
p. 16
p. 13
p. 24
p. 4 ...
p 6
p. 9 ...
p. 29
p. 34
Ra-04
Ra-03
Ra-05
00-07
Sr-04
H-02 ..
EPA4
p. 19
P. 19
p. 33
p. 92
p. 92
p. 65
p. 87
p. 92
SMS
305, 7500-Ra
C, 7500-
Ra C-01.
304, 7500-Ra
B, 7500-Ra
B-01.
7500-Ra D,
7500-Ra
D-01.
7500-U B,
7500-U B-
00.
7500-U C
(17th Ed.).
3125
7500-U C
(18th, 19th-,
or 20th
Ed.), 7500-
U C-00.
7500-Cs B,
7500-Cs
B-00.
7120, 7120-
97.
7500-I B,
7500-I B-
00.
7500-I C,
7500-I C-
00.
7500-I D,
7500-I D-
00.
7120, 7120-
97.
303, 7500-Sr
B, 7500-Sr
B-01.
306, 7500-
3H B,
7500-3H
B-00.
7120, 7120-
97.
7500-Cs B,
7500-Cs
B-00.
7500-I B,
7500-I B-
00.
ASTM «
D34 54-97
D2460-97
D2907-97
D5673-03.
D3972-
97, 02.
D5174-
97, 02.
D2459-72
D3649-
91,98a.
D3649-
91, 98a.
D4785-
93, OOa.
D4107-
91, 98
(Re-
ap-
proved
2002).
D3649-
91, 98a.
D4785-
93, OOa.
USGS?
R-1 141-76
R-1 140-76
R-1 142-76
R-1 180-76,
R-1 181-
76.
R-1 182-76
R-1 11 1-76.
R-1 11 0-76
R-1 160-76
R-1 171-76.
R-1 110-76
DOE8
Ra-04
U-04.
U-02.
4.5.2.3.
4.5.2.3.
Sr-01,
Sr-02.
Ga-01-R.
Other
NY9,
GA«
NY 8;
NJ10,
GA">
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 and 13 through 14 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 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 Ave-
nue, NW., Room 3334 . Washington, DC 20460 (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this mate-
rial at NARA. call 202-741-6030. or go to: http://www.archives.gov/federal_registar/code_otjgderal_regulations/!tirjocations.html.
' "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 In-
formation Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800-553-6847), PB 80-224744.
2 "Interim Radiochemical Methodology for Drinking Water," EPA 600/4-75-008 (revised), March 1976. Available NTIS, ibid.
3 "Radiochemistry Procedures Manual," EPA 520/5-84-006, December 1987. Available NTIS, bid.
4 "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 Wastewator," 13th, 17th, 18th, 19th 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, 7500-1 C, 7500-1 D, 7500-Sr B, and 7500-:'H 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 editions. Method 7120 is only in the 19th and 20th editions. Method
3125 is only in the 20th edition. Methods 7110 B-00, 7110 C-00, 7500-Ra B-01, 7500-Ra C-01, 7500-Ra D-01, 7500-U B-00, 7500-U C-00, 7500-I B-00, 7500-I C-00, 7500-I D-00,
7120-97, 7500-Sr B-01, and TSOO-^H B-00 are available online at http://www.stantts.filmettKxis.org. The year In which each method was approved by the Standard Methods Committee is
designated by the last two digits in the method number. The methods listed are the only online versions that may be used.
"Annual Book of ASTM Standards, Vol. 11.01 and 11.02, 2002; ASTM International; any year containing the cited version of the method may be used. Copies of these two volumes and
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.
7 "Methods for Determination of Radioactive Substances in Water and Fluvial Sediments," Chapter A5 in Book 5 of Techniques of Water-Resources Investigations of the United States Geo-
logical Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal Center, Denver, CO 80225-0425.
»"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 Qa-01-R
is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S. Department ot Energy (DOE), 376 Hudson Street, New York, NY 10014-3621.
9"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-
ment ot Health, Empire State Plaza, Albany. NY 12201.
10"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 Swing Street, Trenton, NJ 08625.
11 Natural uranium and thorium-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods; americium-241 is approved with co-
precipitation methods.
12 It uranium (U) is determined by mass, a 0.67 pCi/u.g of uranium conversron factor must be used. This conversion factor is based on the 1:1 activity ratio of U-234 and U-238 that is
characteristic of naturally occurring uranium.
13 "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 Met-
als in Environmental Samples—Supplement I,1" EPA 600-R-94-111, May 1994. Available at NTIS, PB 95-125472.
-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11247
14"Tha Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors," Revision 1.2, December 2004. Available from the
Environmental Resources Center, Georgia Institute of Technology, 620 Cherry Street, Atlanta, GA 30332-0335, USA, Telephone: 404-894-3776. This method may be used to analyze for ra-
dium-226 and radium-228 in samples collected after January 1. 2005 to satisfy the radium-226 and radium-228 monitoring requirements specified at 40 CFR 141.26.
• 16. Section 141.74 is amended as
follows:
• a. By revising the entry for turbidity
in the table in paragraph (a)(l).
• b. By revising footnotes 1,8,10,11,
and 12 to the table in paragraph (a)(l).
• c. By adding footnote 13 to the table
in paragraph (a)(l).
• d. By revising paragraph (a)(2).
§ 141.74 Analytical and monitoring
requirements.
(a)* * *
(1)* * *
Organism
Methodology
Citation1
Turbidity13 Nephelometric Method 2130 B
Nephelometric Method 180.1 9
Great Lakes Instruments Method 210
Hach FilterTrak 1013312
*****
1 Except where noted, all methods refer to 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 pub-
lished in any of these three editions may be used. In addition, the following online versions may also be used: 2130 B-01, 9215 B-00, 9221 A,
B, C, E-99, 9222 A, B, C, D-97, and 9223 B-97. Standard Methods Online are available at httpMvww.standardmethods.org. The year in which
each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed
are the only Online versions that may be used.
SA-1 broth may be held up to 7 days in a tightly closed screw cap tube at 4 °C.
9"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, Wl 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., 1 IDEXX Drive, Westbrook, ME 04092, telephone (800) 321-0207.
12 A description of the Hach FilterTrak Method 10133, "Determination of Turbidity by Laser Nephelometry," January 2000, Revision 2.0, can be
obtained from; Hach Co., P.O. Box 389, Loveland, CO 80539-0389, telephone: 800-227-4224.
13Styrene divinyl benzene beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g. Hach StablCal™ or equivalent) are accept-
able substitutes for formazin.
(2) Public water systems must
measure residual disinfectant
concentrations with one of the
analytical methods in the following
table. If approved by the State, residual
disinfectant concentrations for free
chlorine and combined chlorine also
may be measured by using DPD
colorimetric test kits. In addition States
may approve the use of the ITS free
chlorine test strip for the determination
of free chlorine. Use of the test strips is
described in Method D99-003, "Free
Chlorine Species (HOC1- and OC1-) by
Test Strip," Revision 3.0, November 21,
2003, available from Industrial Test
Systems, Inc., 1875 Langston St., Rock
Hill, SC 29730. Free and total chlorine
residuals may be measured
continuously by adapting a specified
chlorine residual method for use with a
continuous monitoring instrument
provided the chemistry, accuracy, and
precision remain the same. Instruments
used for continuous monitoring must be
calibrated with a grab sample
measurement at least every five days, or
with a protocol approved by the State:
Residual
Free Chlorine
Total Chlorine
Chlorine Dioxide
Ozone
Methodology
Amperometric Titration
DPD Ferrous Titrimetric
DPD Colorimetric
Syringaldazine (FACTS)
Amperometric Titration
Amperometric Titration (low level measure-
ment).
DPD Ferrous Titrimetric
DPD Colorimetric
lodometric Electrode
Amperometric Titration
DPD Method
Amperometric Titration
Spectrophotometric
Indiao Method
SM1
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 I
4500-CIO2 C
4500-CIO2 D
4500-CIO2 E
4500-O, B
SM Online2
4500-CI D-00
4500-CI F-00.
4500-CI G-00.
4500-CI H-00
4500-CI D-00
4500-CI E-00.
4500-CI F-00.
4500-CI G-00
4500-CI I-OO
4500-CIO2 C-00.
4500-CIO2 E-00
4500-O, B-97.
Other
D 1253-03 3
D1 253-03 3
327 0 Revision 1 1 4
1 All the listed methods are contained in the 18th, 19th, and 20th editions of Standard Methods for the Examination of Water and Wastewater,
1992, 1995, and 1998; the cited methods published in any of these three editions may be used.
2Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard
Methods Committee is designated by the last two digits in the method number. The methods listed are the only Online versions that may be
used.
3Annual Book of ASTM Standards, Vol. 11.01, 2004 ; ASTM International; any year containing the cited version of the method may be used.
Copies of this method may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700 West Conshohocken, PA 19428-2959.
"EPA Method 327.0, Revision 1.1, "Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using Lissamine Green B and Horse-
radish Peroxidase with Detection by Visible Spectrophotometry," USEPA, May 2005, EPA 815-R-05-008. Available online at http://
www.epa.gov/safewater/methods/sourcalt.html.
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11248
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
PART 143—NATIONAL SECONDARY
DRINKING WATER REGULATIONS
• 17. The authority citation for part 143
continues to read as follows:
Authority: 42 U.S.C. 300f et seq.
m 18. Section § 143.4 is amended by
revising the table in paragraph (b) to
read as follows:
§143.4 Monitoring.
* * * *
(b)* * *
Contaminant
2 Chloride
3 Color
7 Odor
8 Silver
9 Sulfate
10 Total Dissolved Solids
1 1 Zinc
EPA
200 7 2
200 8 2
200 9 2
300 O1
300. 1e
200 72
200 9 2
200 7 2
200 8 2
200 9 2
200 7 2
200 8 2
200 9 2
3000'
300. 16
375 2 '
200 7 2
200. 8 2
ASTM3
D4327-97 03
D512-89 (Re-
approved
1999) B.
D4327-97 03
D516-90, 02 ...
SM" 18th and 19th ed.
3120 B
31 13 B
31 11 D
4110B
4500-CI- D '.
4500-Ch B
2120 B . .
5540 C
3120 B
3111 B
3113 B
3120 B .. . .
3111 B
3113 B
2150 B
3120 B
3111 B
31 13 B
4110 B
4500-SO42- F
4500-SO42-C, D
4500-SO42~ E
2540 C .
3120 B
3111 B
SM420thed.
3120 B
4110 B
4500-CI- D
4500-CI- B
2120 B
5540 C
3120 B
3120 B
2150 B
3120 B
4110 B
4500-SOi2- F.
4500-SO42-C, D.
4500-SO42- E.
2540 C
3120 B
SM7 Online
3120 B-99
3113 B-99
31 1 1 D-99
4110 B-00
4500-CI- D-97.
4500-CI- B-97
2120 B-01.
5540 C-00
3120 B-99
311 1 B-99
3113 B-99.
3120 B-99.
3111 B-99
3113 B-99.
2150 B-97.
3120 B-99.
3111 B-99
3113 B-99
4110 B-00
2540 C-97.
3120 B-99
3111 B-99.
Other
D6508, Rev. 2s
I-3720-85 5
D6508, Rev. 2s
The procedures shall be done in accordance wrth the documents listed below. The incorporation by reference ot the following documents was approved by the Director of the Federal Reg-
ister 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 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 3334,
Washington, DC (Telephone: 202-566-2426); or at the National Arcnwes and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030,
or go to: hftp://mm.archives.gov/feaeral_register/code_otJederaLregulations/ibr_locations.html.
' "Methods for the Determination of Inorganic Substances in Environmental Samples," EPA/600/R-93-100, August 1993. Available at NTIS, PB94-120821.
2"Methods for the Determination of Metals in Environmental Samples—Supplement I," EPA/600/R-94-111, May 1994. Available at NTIS, PB 95-125472.
3 Annual Book ot ASTM Standards, 1994, 1996, 1999, or 2004. 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 the ASTM International, 100 Barr Hartor Drive, West Conshohocken, PA 19428.
'Standard Methods tor the Examination ot Water and Wastewaler, 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 n any of these three editions may be used, except that the versions of 3111 B, 3111 D, and 3113 B in the 20th edition
may not be used.
5Method I-3720-85, 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.
•"Methods for the Determination of Organic and Inorganic Compojnds in Drinking Water," Vol. 1, EPA 815-R-00-014, August 2000. Available at NTIS, PB2000-106981.
'Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last
two digits in the method number. The methods listed are the only online versions that may be used.
8Method D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrtees Using Capillary Ion Electrophoresis and Chromate Electrolyte," available from
Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
PART 430—THE PULP, PAPER, AND
PAPERBOARD POINT SOURCE
CATEGORY
• 19. The authority citation for part 430
continues to read as follows:
Authority: Sections 301, 304, 306, 307,
308, 402, and 501 of the Clean Water Act, as
amended, (33 U.S.C. 1311,1314, 1316, 1317,
1318,1342, and 1361), and Section 112 of the
Clean Air Act, as amended (42 U.S.C. 7412).
• 20. Section 430.02 is amended by
adding paragraph (g) to read as follows:
§430.02 Monitoring requirements.
*****
(g) Analyst may use NCASI Method
CP-86.07, "Chlorinated Phenolics in
Water by In situ Acetylation and GC/MS
Determination" (January 2002) for
determination of certain chlorinated
phenols, chlorinated guaiacols,
chlorinated catechols, chlorinated
benzaldehydes (i.e., vanillins and
syringaldehydes), and trichlorsyringol
(analytes specified in the method) in
bleach plant filtrate as an alternative to
EPA Method 1653. NCASI Method CP-
86.07 is available from the Publications
Coordinator, NCASI, P.O. Box 13318,
Research Triangle Park, NC 27709-3318.
Telephone: 919-588-1987.
PART 455—PESTICIDE CHEMICALS
• 21. The authority citation for Part 455
continues to read as follows:
Authority: Sees. 301, 304, 306, 307, and
501, Pub. L. 92-500, 86 Stat. 816, Pub. L. 95-
217, 91 Stat. 156, and Pub. L. 100-4 (33
U.S.C. 1311, 1314, 1316, 1317, 1361).
• 22. Section 455.50 is revised to read
as follows:
§ 455.50 Identification of test procedures.
The pesticide active ingredients to
which this section applies and for
which effluent limitations guidelines
and standards are specified in this Part
are named, together with the Chemical
Abstracts Service (CAS) number
(provided to assist in identifying the
pesticide active ingredient only) and
analytical method(s) designation(s) in
Table IG at 40 CFR 136.3(a). Except as
provided in 40 CFR 136.5, the discharge
parameter values required under the
Clean Water Act must be determined by
one of the analytical methods cited and
described in Table IG at 40 CFR
136.3(a). Pesticide manufacturers may
not use the analytical method cited in
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Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
11249
Table IB, Table 1C, or Table ID of 40 CFR
136.3(a) to make these determinations
(except where the method cited in those
tables is identical to the method
specified in Table IG at 40 CFR
13 6.3 (a)). The full texts of the analytical
methods cited in Table IG at 40 CFR
136.3(a) are contained in the Methods
For The Determination of
Nonconventional Pesticides In
Municipal and Industrial Wastewater,
Volume I, EPA 821-R-93-010A (August
1993 Revision I) and Volume II, EPA
821-R-93-010B (August 1993) (the
"Compendium"). Each pesticide
chemical manufacturer that is required
to determine discharge parameter values
under this Part using one of the
analytical methods cited in Table IG at
40 CFR 136.3(a) must request in writing
a copy of the Compendium from the
permit authority or local control
authority (as applicable) prior to
determining such discharge parameter
values, unless the manufacturer already
has a copy.
• 23. Part 455 is amended by removing
and reserving Table 7 to Part 455.
PART 465—COIL COATING POINT
SOURCE CATEGORY
• 24. The authority citation for Part 465
continues to read as follows:
Authority: Sees. 301,304 (b), (c), (e), and
(g), 306 (b) and (c), 307 (b) and (c), and 501
of the Clean Water Act (the Federal Water
Pollution Control Act of 1972, as amended by
the Clean Water Act of 1977)(the "Act"); 33
U.S.C. 1311, 1314 (b), (c), (e), and (g), 1316
(b) and (c), 1317 (b) and (c}, and 1361; 86
Stat. 816, Pub. L. 92-500; 91 Stat. 1567, Pub.
L. 95-217.
• 25. Section 465.03 is amended by
revising paragraph (c) to read as follows:
§465.03 Monitoring and reporting
requirements.
* * * * *
(c) The analytical method required for
determination of petroleum
hydrocarbons (non-polar material) is
given under the listing for "oil and
grease" at 40 CFR I36.3(a), Table IB and
must be used after December 31, 2005.
* A * * *
[FRDoc. 07-1073 Filed 3-9-07; 8:45 am]
BILLING CODE 6560-50-P
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