&EPA
United States
Environmental Protection
Agency
Office of Ground Water and
Drinking Water
Technical Support Division
Cincinnati, Ohio 45268
EPA-814B-92-002
September 1992
Manual for the
Certification of
Laboratories Analyzing
Drinking Water
Criteria and Procedures
Quality Assurance
Third Edition
Change 2 - September 1992
Supersedes EPA/570/9-82/002, October 1982, entitled Manual for the Certification of
Laboratories Analyzing Drinking Water
Printed on Recycled Paper
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List of Effective Pages
REMOVE SUPERSEDED PAGES AND INSERT REVISED PAGES
Dates of issue for original and changed pages are as follows:
Original 0 April 1990
Change 1 October 1991
Change 2 September 1992
Page/Chapter Change No.*
No.
i (Title Page) - 2
ii (Effective Pages) (Added) 2
iii (Notice) 1
iv (Foreword) (Added) 1
v-vi (Preface) "I
vii-ix (Acknowledgments) 1
x (blank) •' 1
xi (Contents) 2
xii (Contents) 1
1-14 (Chapters l-lll) 0
15-25 (Chapter IV) 2
26-36 (Chapter IV) • • • 0
37-58.8 (Chapter V) 1
59-74 (Chapter VI) 0
75-86 (Appendices A-D) 0
87-91 (Appendices E-G) 1
93-95 (Appendix H) (Added) 1
*Zero in this column indicates an original page.
Change 2
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Contents
Page
CHAPTER I: INTRODUCTION • 1
CHAPTER II: RESPONSIBILITIES 3
Office of Drinking Water 3
Office of Research and Development 3
Regional Offices 3
Drinking Water Laboratory Certification Work Group 4
CHAPTER III: IMPLEMENTATION 5
Regional Laboratories and Programs 5
Principal State Laboratories 5
Local Laboratories 6
Other Considerations for Certification 7
Quality Assurance Plan 7
Performance on Routine Water Samples 8
Chain-of-Custody Procedures 8
Requirements for Maintaining Certification Status 8
Criteria and Procedures for Downgrading/Revoking
Certification Status 8
Reciprocity 10
Training '0
Technical Services 11
Reference Samples 11
Early Warning System for Problems with
Test Supplies and Equipment 11
Alternate Analytical Techniques 14
CHAPTER IV: CHEMISTRY 15
1. Personnel 15
2. Laboratory Facilities 15
3. Laboratory Equipment and Instrumentation 16
4. General Laboratory Practices 16
5. Analytical Methodology 16
6. Sample Collection, Handling, and Preservation 17
7. Quality Assurance 17
8. Records and Data Reporting 18
9. Action Response to Laboratory 18
XI
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Contents (continued)
Page
CHAPTER V: MICROBIOLOGY ,.-......'. 37
1. Personnel '. ...'....... 37
2. Laboratory Facilities . . . '-.• . . '. .' .'........ 37
3. Laboratory Equipment and Supplies .................. 37
4. General Laboratory Practices . .>..., ,. . . . .,. 40
5. Analytical Methodology .. . . . .>•. ',,',. . ,',..,. .... 44
6. Sample Collection, Handling, and Preservation .... I ..... 47
7. Quality Assurance /.,..... 43
8. Records and Data Reporting ....>.,....'.! ....,!.,; .... 48
9. Action Response to Laboratory 48
CHAPTER VI: RADIOCHEMISTRY^, . . . .,;-..,. , . ...;;.-.-.., . . . . 59
I .. ;!...'.- lt .
1. Personnel .",. ..;.'. /;,. . .'.'.: 59
2. Laboratory Facilities . ...',,,. . . ; \ ...... i . . .«..:. . 59
3. Laboratory Equipment and Supplies . . . . . . . . . . . . . . . . 60
4. General Laboratory Practices ,...,.,.. 61
5. Analytical Methodology . .'. .:, . . , ..,. . ... .,. , 61
6. Sample Collection, Handling, and Preservation . . . ..,.., 61
7. Quality Assurance .......... I ...... ... . ..-•. . .,. ., 61
8. Records and Data Reporting ....... . . ..:....;... 62
9. Action Response to Laboratory ,...', . 62
APPENDICES '
Appendix A: Chain-of-Custody . i 75
Appendix B: Recommended Protocol for Regions Conducting
On-site Laboratory Evaluations . . . . . , . . . . . 81
Appendix C: Abbreviations ;.........,......'.... 83
Appendix D: EPA Policy on Third Party Certification . . .; . . ... 85
Appendix E; Required Analytical Capability for
Principal State Laboratory Systems .. . . . . ... 87
Appendix F: Additional Contaminants Scheduled for
Rules in 1992-1993 .... ..... ." . . ! I '.''.. 89
Appendix G: §1445 Unregulated Chemicals to be
Monitored . . . ... ... . . . . . .91
Appendix H: Analytical Methods for Microbiology . ..93
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XII
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Chapter IV
Critical Elements for Chemistry
1. Personnel
1.1 Director
A laboratory's volume and scope of services may not require
this position. However, there should be a person either in
this position or an individual available for consultation
meeting the same requirements as the Director, If the
Director is also a supervisor, the requirements of 1.2 are also
to be met.
1.1.1 Academic training: Minimum bachelor's
degree in science is required. If bachelor's degree is
in a field other than chemistry, the individual should
have the number of credit hours in chemistry
' equivalent to a minor in chemistry.
1.1.2 Experience: Minimum of 2 years
experience in a water laboratory is required.
of
1.2 Supervisor .
Minimum requirements for the supervisor position are listed
below. If the supervisor is also an instrument operator, the
requirements of 1.3 are also to be met., • >
1.2.1 Academic training. Bachelor's degree in
science that includes the number of, credit hours in,
chemistry courses required for a rriajor In chemistry.
1.2.2 Experience. Minimum of 1 year experience in
chemical analysis of water is required.
1.3 Instrument Operators
Operators for the following instruments are needed: Atomic
Absorption (AA) - including direct aspiration, furnace and
platform analyses, Ion Chromatograph (1C), Gas
Chromatograph (GC), Gas Chromatograph/Mass
Spectrometer (GC/MS), Inductively Coupled Plasma
(ICP-AES), Inductively Coupled Plasma/Mass
Spectrometer (ICP/MS), Transmission Electron Microscope
(TEM). The following are required minimum standards for
these analyses.
1.3.1 Academic training: Bachelor's degree in
chemistry or related field. The analyst need not have
a bachelor's degree if the immediate supervisor has a
bachelor's degree in chemistry or related field or if the
analyst has the number of credit hours in chemistry
courses required for a major in chemistry.
1.3.2 Specialized training: Satisfactory
completion of a short course in GC/MS, ICP or TEM
offered by equipment manufacture/, professional
organization, university, or other qualified training
facility is e'ssential for these operators. Specialized
training for other instruments is recommended.
1.3.3 Experience: Minimum of six months
experience in the operation of either AA, 1C, GC, ICP
or TEM. Minirnuni of 12 months experience in the
operation of'the GC/MS. (see paragraph 1.5.)
1.3.4 Initial qualification: After appropriate
training, it is ess'ential that the analyst demonstrate
acceptable results in the analysis of an applicable QC
or PE sample.
1.4 Other Analysts
The following are required minimum standards for the
.analyst position.
1.4.1 Academic training: Minimum of high school
diploma or equivalent.
1.4.2 Initial qualification: After being trained in a
methods training course or by any qualified analyst,
- the person being trained shall demonstrate acceptable
. '.'- results in the analysis of an applicable QC or PE
sample. _ • •/ .
1.5 Analysts and Operators in Training
Data produced by analysts and instrument operators while
:'in the process,of obtaining the required training or
experience are acceptable when reviewed and validated by
a fully qualified analyst or the laboratory supervisor.
1.6 Waiver of Academic Training Requirement
The certification officer may waive the need for specified
'academic training, on a case-by-case basis, for highly
experienced analysts.
2. Laboratory Facilities
The laboratory facilities should be clean, have temperature
.and humidity adequately controlled in the instrument areas
and have adequate lighting at the bench top. It is important
for the laboratory to have provisions for the proper storage
and disposal of chemical wastes. Exhaust hoods are
required for preparation, extraction and analysis where
applicable.
It. is recommended that a minimum of 150 to 200 square
feet/laboratory person be available. The laboratory should
contain at least 15 linear feet of usable bench space per
analyst. Workbench space should be convenient to sink,
15
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water, gas, vacuum and electrical sources free of surges. It
is recommended that the organic and inorganic facilities be
separate rooms. The analytical and sample storage area is
to be Isolated from all potential sources of contamination.
3. Laboratory Equipment and
Instrumentation
The laboratory is only required to have those instruments
that are needed to perform the approved methods for which
certification has been requested. Those instruments must
meet the specifications in the checklist entitled "Required
Equipment and Instruments for Inorganic and Organic
Contaminants".
4. General Laboratory Practices
4.1 General
4.1.1 Chemicals/reagents: "Analytical reagent
grade" (AR) chemicals or better must be used for
analyses. Consult Standard Methods for the
Examination of Water and Wastewater" 17th edition,
part 1070C, pages 1 -42 through 1 -45for more detailed
Information on reagent grades. Individual analytical
methods in the approved reference may specify
additional requirements for the reagents to be used.
4.1.2 Laboratory safety: While specific safety
criteria are not an aspect of laboratory certification,
laboratory personnel should apply general and
customary safety practices as a part of good
laboratory procedure. Each laboratory is strongly
encouraged to have a safety plan as part of their
standard operating procedure (see OSHA
requirements). Where safety practices are included in
an approved method, they must be strictly followed.
4.2 Inorganic Contaminants
4.2.1 Reagent water: The laboratory is to have a
source of reagent water having a sensitivity value of
at least 0.5 megohms (less than 2.0 micromhos/cm)
at 25°C. High quality water meeting such
specifications may be purchased from commercial
suppliers. Quality of reagent water is best maintained
by sealing from the atmosphere. Quality checks to
meet specifications above should be made and
documented at planned intervals based on use. This
planned interval should not exceed one month.
4.2.2 Glassware preparation: Glassware should
be washed in a warm detergent solution and
thoroughly rinsed first with tap water and then with
reagent water. This cleaning procedure is sufficient for
general analytical needs, but the individual
procedures must be referred to for precautions to be
taken against contamination of glassware. It is
advantageous to maintain separate sets of suitably
prepared glassware for the nitrate, mercury, and lead
procedures due to the potential for contamination from
the laboratory environment.
4.3 Organic Contaminants
4.3.1 Reagent water: Reagent water for organic
analysis is to be free of interferences for the analytes
being measured. It may be necessary to treat water
with activated carbon to eliminate all interferences.
4.3.2 Glassware preparation: Glassware and
sample bottles should be washed in a detergent
solution and thoroughly rinsed first in tap water and
then in reagent water. Glassware should have a final
organic solvent rinse or must be baked at 400°C for
30 minutes and then dried or cooled in an area free of
organic contamination. Glassware should be covered
with organic-free aluminum foil during storage. Bottles
and cap liners, used for collection of samples for
determination of volatile organic chemicals (VOCs),
should be dried at 105°C for 1 hr, sealed, and stored
in an area free of volatile organics.
5. Analytical Methodology
5.1 General
A list of approved methodology for inorganic and organic
contaminants can be found in Tables IV-1 and IV-2,
respectively. In general, all procedural steps in these
methods are considered requirements. Other methods
cannot be used unless approval has been approved by the
Agency. Contact the appropriate certifying authority for an
alternate test procedure application. Application for the use
of an alternate method may require acceptable comparability
data. Prepackaged test kits other than the U.S.
EPA-approved DPD and the FACTS Colorimetric Test Kits
are not approved for use. Recommended methods for
inorganic contaminants that do not require the use of an
approved method are listed in Table IV-3.
5.1.1 If a'drinking water sample contains less than 1
nephelometric turbidity unit (NTU) and is properly
preserved, the sample may be analyzed directly
(without digestion) when using one of the following
total element techniques: graphite furnace -AA,
ICP/AES, ICP/MS, or direct flame aspiration AA,
Turbidity should be measured on the preserved
sample just prior to when the metal analyses are
initiated. For gaseous hydride determination of
arsenic, antimony, or selenium, or for the
determination of mercury by the cold vaportechnique,
the proper digestion technique must be followed to
ensure that the element is in the proper chemical state
for analysis.
5.2 Non-certified analysis
Measurements for pH, temperature, turbidity, residual
disinfectant, calcium, orthophosphate, silica, alkalinity, and
conductivity need not be made in certified laboratories, but
may be made by any person acceptable to the state.
However, approved methodology must be used (Table IV-1).
The state should institute a quality assurance program to
assure validity of data from these measurements.
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5.2.1 Sealed liquid turbidity standards purchased
from the instrument manufacturer must be calibrated
against properly prepared and diluted formazin or
styrene divinylbenzene polymer standards at least
every 4 months in order to monitor for any eventual
deterioration. This calibration is to be documented.
The standards are to be replaced when they do not
fall within 15% of the assigned value of the standard.
Solid turbidity standards composed of plastic, glass,
or other materials are not reliable and should not be
used. ,
5.2.2 If visual comparison devices such as color
wheels or sealed ampules are used for determining
free chlorine residual, the standards incorporated into
such devices should be calibrated at least every six
months. These calibrations are to be documented.
Directions for preparing temporary and permanent
type visual standards can be found in Method
4500-Cl-G, Standard Methods, 17th ed., 1989. By
comparing standards and plotting such a comparison
on graph paper, a corrective factor can be derived and
, appliedtofutureresultsobtainedonthenowcalibrated
apparatus. ,
6. Sample Collection, Handling, and
Preservation
The manner in which samples are collected and handled is
critical for obtaining valid data. It is essential that a written
sampling protocol with specific sampling instructions be
available to sample collectors and for inspection by the
certification officer (see Appendix A, Chain-of-Custody).
6.1. Rejection of Samples
The laboratory is to reject any sample taken for compliance
purposes not meeting the criteria in 6.2 through 6.6 below
and notify the system/individual requesting the analyses.
6.2. Sample Containers and Preservation
The type of sample container and the required preservative
for each inorganic and organic chemical contaminant are
listed in Table IV-4 and Table IV-5, respectively.
6.3. Maximum Holding Times
Samples must be analyzed within the maximum holding
times listed in Tables IV-4 and IV-5.
6.4. Sample Collection and Transport
When the laboratory has responsibility forsample collection,
handling, and preservation, there needs to be strict
adherence to correct sampling procedures, complete
identification of the sample, and prompt transfer of the
sample to the laboratory.
6.5 Sample Collector
The collector should be trained in sampling procedures and
approved by the State regulatory authority or its delegated
representative.
6.6 Sample Report Form
The sample report form should contain the location, date and
time of collection, collector's name, preservative added,
sample type, and any special remarks concerning the
sample. Indelible ink should be used.
7. Quality Assurance
7.1 General Requirements:
7.1.1 All quality control information is to be available
for inspection by the certification officer.
7.1.2 A manual of analytical methods and the
laboratory's QA plan are also to be available to the
analysts (see Chapter Ill's discussion of the QA Plan).
7.1.3 Class S Weights or better should be available
to make periodic checks on balances. A record of
these checks is to be available for inspection. The
specific checks and their frequency are to be as
prescribed in the laboratory's QA plan and the
laboratory's operations manual, if appropriate. This
frequency should not exceed 6 months.
7.1.4 Color standards, or their equivalent such as
built-in internal standards, are to be available to verify
wavelength settings on spectrophotometers. A record
of these checks should be available for inspection.
The specific checks and their frequency are to be as
prescribed in the laboratory's QA plan and the
laboratory's operations manual, if appropriate. The
frequency of these checks should not exceed 6
months.
7.2 Analytical Quality Control
The following are required for each analyte for which a
laboratory is certified:
7.2.1 The laboratory must analyze PE samples
(when available) at least annually.
7.2.2 At least once each quarter, the laboratory
should analyze a QC sample (EPA certified QC
sample orequivalent). If errors exceed limits specified,
corrective action is to be taken and documented, and
a follow-up quality control standard analyzed as soon
as possible to demonstrate the problem has been
corrected.
7.2.3 At the beginning of each day that samples are
to be analyzed, a standard curve composed of at least
a reagent blank and three standards covering the
sample concentration range are to be prepared.
These standards should be from a source different
than the quality control standard used for 7.2.2.
7.2.4 Calibration for some methods is so
time-consuming that 7.2.3 is impractical. For these
methods, the standard curve is to be initially
developed as specified In 7.2.3. Thereafter, at the
beginning of each day on which analyses are
performed, this curve is to be verified by analysis of at
least a reagent blank and one standard in the expected
concentration range of the samples analyzed that day.
All checks should be within the control limits specified
17
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In 7.2.7 or the system recalibrated as specified in
7.2.3.
7.2.5 If the reagent blank specified in 7.2.3 (or
paragraph 7.2.4) is not carried through the full
analytical procedure, then some other blank (at least
one per day) is to be carried through the entire
analytical procedure. Results from reagent blanks
should not exceed the laboratory's method detection
limit (MDL); see paragraph 7.2.8.
7.2.6 The laboratory should add a known spike to a
minimum of 10% of the routine samples (except when
the method specifies a different percentage, i.e.,
furnace methods) to determine if the entire analytical
system Is In control. The spike concentration should
not be substantially less than the background
concentration of the sample selected for spiking.
These checks should be evenly spaced and one check
should be at the end of the day's analyses. Overtime,
samples from all routine sample sources should be
spiked. If any of these checks are not within the control
limits specified in paragraph 7.2.7, a standard should
be analyzed to determine if the "out of control"
condition was due to sample matrix or system
operation. This standard is to be analyzed through the
complete analytical system. Corrective action is to be
taken In accordance with the laboratory's QA plan.
7.2.7 Until sufficient data are available from the
laboratory, usually a minimum of 15 to 25 test results
on a specific analysis, the laboratory is to use the
control limits, if available, developed from the mean
(X) and the standard deviation (S) relationships in
Table IV-6. This Table was derived from EPA's PE
sample data. After inserting the analytical
concentration (c), including background concentration
(B) wherever appropriate, into the proper pair of
relationships, compute control limits for standards X
± 3(S) and for spike recoveries (X-B) ± 3(S). As
sufficient data becomes available, the laboratory
should develop traditional QC chart criteria for the
various QC checks specified above (see Chapter 6 of
the Handbook for Analytical QA in Water and
Wastewater Laboratories, EPA-600/4-79-019, or
similar QC reference texts for further information).
Since percent recovery may not be a constant, the
percent recovery data may have to be separated into
concentration Intervals before control limits are
calculated for each interval. If any of these control
limits are tighter than the matching control limits in
Table IV-6, the laboratory shall use the tighter criteria.
Otherwise, control limits in Table IV-6 are required.
The laboratory should continue to calculate traditional
control limits for each analyte as additional results
become available.
7.2.8 It is further recommended that the laboratory
calculate the MDL at least annually in accordance with
the procedure given in 40 CFR Part 136, Appendix B.
This procedure is available from EPA, Environmental
Monitoring Systems Laboratory, 26 W. Martin Luther
King Drive, Cincinnati, Ohio, 45268.
8. Records and Data Reporting
8.1 Laboratory Records.
Records of chemical analyses are to be kept by the
laboratory for a minimum of 3 years. This includes all raw
data, calculations, and quality control data. These data files
may be either manual or computer based. Hard copy should
be developed as soon as possible and stored for
recordkeeping purposes. The following information should
be available as a sample data report or summary record:
8.1.1 Date, place, time of sampling, preservative
added, and name of person who collected the sample.
8.1.2 Identification of sample as to whether it is a
routine distribution system sample, check sample, raw
or finished water sample, or other special purpose
sample.
8.1.3 Date of receipt of sample and date of analysis.
8.1.4 Laboratory and persons responsible for
performing analysis.
8.1.5 Analytical technique/method used, and quality
control data.
8.1.6 Results of analysis.
9. Action Response to Laboratory Results
When action response is a designated laboratory
responsibility, the laboratory must notify the proper authority
of noncompliance sample results and request resampling
from the same sampling point immediately.
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18
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Table IV-1. Approved Methodology for Inorganic Contaminants
Reference (Method Number)
Contaminant
Alkalinity
Antimony
Arsenic
Asbestos
Barium
Beryllium
Cadmium
Calcium
Chromium
Conductivity
Copper
•
Cyanide
Fluoride
Lead
Mercury
Nickel
Nitrate-N
Nitrite-N
MCL
mg/l
_
0.006
0.05
7mf/111
2
0.004
0.005
0.1
1.3*
0.2
4
0.015*
0.002
0.1
10
1
Methodology1
Titrimetric
Atomic Absorption : platform
: gaseous hydride
: furnace /•
Inductively coupled plasma mass spectrometry
Atomic Absorption : furnace
: gaseous hydride
: spectrophotometric
: inductively coupled plasma
Transmission electron microscopy
Atomic Absorption : furnace
: direct aspiration
Inductively coupled plasma emission spectrometry
Atomic absorption : furnace
: platform
Inductively coupled plasma emission spectrometry
mass spectrometry
Atomic Absorption : furnace
Inductively coupled plasma emission spectrometry
EDTA titrimetric
Atomic absorption : direct aspiration
Inductively coupled plasma emission spectrometry
Atomic Absorption : furnace
Inductively coupled plasma emission spectrometry
Conductance
Atomic absorption : furnace
: platform
: direct aspiration
Inductively coupled plasma emission spectrometry
mass spectrometry
Manual Distillation : followed by
: Spectrophotometric
: Autospectrophotometric
: Selective Electrode Method
: Amenable Spectrophotometric
Colorimetric SPADNS, with distillation
Potentiometric ion selective electrode
Automated Alizarin fluoride blue, with distillation
Automated ion selective electrode
Atomic Absorption : furnace technique
: platform
Inductively coupled plasma mass spectrometry
Manual cold vapor technique
Automated cold vapor technique
Atomic absorption furnace
platform
direct
Inductively coupled plasma emission spectrometry
mass spectrometry
Manual cadmium reduction
Automated hydrazine reduction
Automated cadmium reduction
Ion selective electrode
Ion Chromatography
Spectrophotometric
Cadmium reduction : automated
; rnanual
Ion Chromatography
EPA2
310.1
200.96
204.2
200.86
206.2
206.3
206.4
_ ^pp
200.7A22
HO
EPA12
208.2
208.1
c
200.76
210.2
200.9
200 .76
e
200.86
213.2
—fi
200.78
215.2
215.1
200.7s
218.2
200 .76
120.1
220.2
200.96
220.1
e
200.7s
C
200. a6
335.2
335.3
335.1
340.1
340.2
340.3
239.216
200.9s
*.fi
200.8s
245.1s
245.2
249.2
200.96
249.1
200.76
200.8s
353.3
353.1
353.2
300.0A18
354.1
353.2
353.3
300.0A18
ASTM3
D1067-88B
D3697-87
D2972-88B
D2972-88A
D3645-84B
D511-88A
D51 1-88B
D1125-82B
D1688-90C
D1688-90A
D2036-89A
D2036-89A
D2036-89B
D1179-72A
D1179-72B
D3559-85D
D3223-86
D3867-90
D3867-90
D3867-90
D3867-90
SM4 Other
2320 I-1030-855
3113B
31 13B8
307A I-1062-855
307B
«•* *v^0
3120
3113B
3111D
_ . _. _ in
3120
3113B
31 2010
3113B
3500-Ca-D
31 1 1 -B
3120
3113B
n-< OrtIO
3120
2510
3113B
3111-B
_ , __1Q
3120
4500CN-C
4500CN-E I-3300-85S
4500CN-F
4500CN-G .
413AandC7
41 3B7
41 3E7 1 29-71 W14
380-75WE15
3113B
3112B
3111B
A
31 1B
in
31 2010
4500NO3-E
4500NO3-F
WeWWG/5880
_ . . .. 19
B1011
4500NO3-F
4500NO3-E
B101119
19.0
Change 2
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Table IV-1. Approved Methodology for Inorganic Contaminants
MCL
Contaminant mg/L
Reference (Method Number)
Methodology1
EPA2 ASTM3
SM4
Other
O-Phosphate
Unffltered, no digestion or hydrolysis
—
pH —
Residual Disinfectant
Chlorine —
Ozone —
Chlorine —
Dioxide
Selenium 0.05
Silica, —
fllffkrAyl
iiiioroo
Sodium 20 mg/l+
Temperature —
Thallium 0.002
Turbidity —
* Action level.
+ Reporting level.
Colorimetric : Ascorbic acid
: Manual; 2 reagent
1 reagent
Auto; Segmented
Discrete
Ion Chromatography
Electrom etric- individual measurement
online measurement
Amperometric Titration
Amperometric Titration-low level
DPD Colorimetric Method
DPD Titrimetric
Syringaldazine (FACTS)
Indigo Method
Amperometric Method
DPD Colorimetric Method
Atomic Absorption : furnace
: gaseous hydride
Colorimetric-molybdate blue -manual
-automated
molybdosilicate -manual
heteropoly blue -manual
molybdate reactive silica -automated
Inductively coupled plasma emission spectrometry
Atomic Absorption : direct aspiration
Inductively coupled plasma emission spectrometry
Flame Photometric
Thermometric
Atomic absorption : platform
: furnace
Inductively coupled plasma mass spectrometry
Nephelometric
365.3
365.2 D515-88A
300.0A18
150.1 D1293-84B
150.2
270.2 D3859-88*
D3859-84A
370.1 D859-88
200.76
273.1
200.76
D1428-82A
200.9s
279.2
200.8s
4500-P-E
4110
4500-H
4500C1-D
4500C1-E
4500C1-G
4500C1-F
4500C1-H
4500C102-C
4500C102-D
3113B
3114B
4500SI-D
4500SJ-E
4500SJ-F
31 2010
31 2010
3500Na-D
OCCn
£OOU
31 13B
21 4A7
1-2601 -855
I-OKOQ-W?5
1 *L\J SJO OO
20
I-3667-855
I-1700-855
I-2700-855
««,.«,. ,u«,,,,4u« H usea. oee seaion M .1. '' 'he Samp'e may be analyzed without di9estion if a total
'c£Ki°f™%*£* ^'fK,0'»Wal^rn£d Wa.sles-" EPA-600/4-79-020, March 1983, Environmental Monitoring Systems Laboratory
Cincinnati, OH 45268. Available from ORD publications, CERI, EPA, Cincinnati, OH 45268. i-« 15lh Edition' Association of Official Analytical Chemists, 1 990.
, March 1987, U.S. EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268.
Change 2
19.1
-------
Table IV-2. Approved Methodology for Organic Contaminants
Reference
Contaminant
MCL mg/l Methodology
EPA
Non-Volatile SOCs
Adipates [Di(ethylhexyl)adipate]
Alachlor
Aldicarb*
Aldicarb sulfoxide*
Aldicarb sulfone*
Atrazine
Carbofuran
Chlordane
Dalapon
Dibromochloropropane(DBCP)
2,4-D
Dinoseb
Diquat
Endothall
Endrin
Ethylene dibromide (EDB)
Glyph osate
Heptachlor
Heptachlor epoxide
Hexachlorobenzene
Hexachlorocyclopentadiene
Lindane
0.4 Gas Chromatography-Liquid/Liquid or Liquid/Solid Extraction-
Photoionization Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.002 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Nitrogen/Phosphorus Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
High Performance Liquid Chromatography-Post Column Reactor
High Performance Liquid Chromatography-Post Column Reactor
- High Performance Liquid Chromatography-Post Column Reactor
0.003 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Nitrogen/Phosphorus Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.04 High Performance Liquid Chromatography-Post Column Reactor
0.002 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.2 Gas Chromatography-Electron Capture Detector
0.0002 Gas Chromatography-Microextraction-EIectron Capture Detector
0.07 Gas Chromatography-Electron Capture Detector
0.007 Gas Chromatography-Electron Capture Detector
0.02 High Performance Liquid Chromatography-Liquid/Solid Extraction-
Ultraviolet Detector
0.1 Gas Chromatography-Liquid/Solid Extraction-Electron Capture Detector
0.002 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.00005 Gas Chromatography-Microextraction-Electron Capture Detector
0.7 High Performance Liquid Chromatography-Post Column Reactor-
Fluorescent Detector
0.0004 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.0002 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
0.001 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction-
/Mass Spectroscopy
0.05 Gas Chromatography-Microextraction-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction-
/Mass Spectroscopy
0.0002 Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
525.1
505
507
525.1
531.1
531.1
531.1
505
507
525.1
531.1
505
508
525.1
515.1
504
515.1"
515.1
5492
5482
505
508
525.1
504
5472
505
508
525.1
505
508
525.1
505
508
525.1
505
525.1
505
508
525.1
20.0
Change 2
-------
Table IV-2. Approved Methodology for Organic Contaminants
Contaminant
MCL mg/1 Methodology
Reference
EPA
Methoxychlor
Oxamyl (Vydate)
PAHs [Benzo(a)pyrene]
0.2
0.0002
Pentachlorophenol
Phttialates [DI(ethylhexyl)phthalate] 0.006
Pldoram 0.5
Polychlorfnated bfphenyls(screen)
as decachloroblphenyl 0.0005
Slmazlne 0.004
Toxaphene 0.003
2,3.7,8 TCDD (Dloxln) 3x10'8
2,4.5-TP (Silvex) 0.05
Total Trlhalomethanes (TTHM) 0.10
Maximum Trihalomethane
Potential (MTP)
Volatile Organic Contamlnants(VOC)
Benzene 0.005
Carbon tetrachloride 0.005
Chtorobenzene 0.1
Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
High Performance Liquid Chromatography-Post Column Reactor-
Fluorescent Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
High Performance Liquid Chromatography-Liquid/Liquid Extraction-
Ultraviolet and Fluorescent Detectors
High Performance Liquid Chromatography-Liquid/Solid Extraction
Ultraviolet and Fluorescent Detectors
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
Gas Chromatography-Liquid/Liquid or Liquid/Solid Extraction-
Photoionization Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
Gas Chromatography-Electron Capture Detector
Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Packed Column-Gas Chromatography
Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Nitrogen/Phosphorus Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
Gas Chromatography-Microextraction-Electron Capture Detector
Gas Chromatography-Electron Capture Detector
Capillary Column-Gas Chromatography-Liquid/Solid Extraction
/Mass Spectroscopy
Capillary Column-Gas Chromatography-Liquid/Liquid Extraction
High Resolution Mass Spectroscopy
Gas Chromatography-Electron Capture Detector
Purge and Trap; Gas Chromatography
Gas Chromatography-Liquid/Liquid Extraction
TTHM after incubation
505
508
525.1
531.1
525.1
5502
550.12
515.1
525.1
5062
525.1
515.1
505
508
508A
505
507
525.1
505
508
525.1
1613
515.1*
501.14
501.2s
510.1
6
Purge and Trap; Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Gas Chromatography-Photoionization Detector 503.1
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy 524.1
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy 524.2
Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap; Capillary Column-Gas Chromatography- 502.2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy 524.1
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy 524.2
Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap; Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Gas Chromatography-Photoionization Detector 503.1
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy 524.1
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy 524.2
Change 2
20.1
-------
Table 1V-2. Approved Methodology for Organic Contaminants
Reference
Contaminant
MCLmg/l Methodology
p-Dichlorobenzene
o-Dichlorobenzene
*
1,2-Dichloroethane
1,1-Dichloroethylene
c-1,2-Dichloroethylene
t-1,2-Dichloroethylene
Dichloromethane(Methylene chloride)* 0.005
1,2-Dichloropropane
Ethylbenzene
Styrene
0.075 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Gas Chromatography-Photoionization Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
0.6 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Gas Chromatography-Photoionization Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
0.005 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
0.007 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy .
0.07 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Capillary-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
0.1 Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector '
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy-
Purge and Trap; Gas Chromatography-Electrolytic Conductivity Detector
Purge and Trap; Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap; Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap; Capillary Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Gas Chromatography-Photoionization Detector
Purge and Trap;Packed Column-Gas Chromatography/Mass Spectroscopy
Purge and Trap;CapilIary Column-Gas Chromatography/Mass
Spectroscopy
0.1 Purge and Trap;Capillary Column-Gas Chromatography-
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Gas Chromatography-Photoionization Detector
Purge and Trap;Packed Column-Gas Chromatography/Mass
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass Spectroscopy
502.1
502.2
0.005
0.7
503.1
524.1
524.2
502.1
502.2
503.1
524.1
524.2
502.1
502.2
524.1
o24.2
502.1
502.2
524.1
524.2
502.1
502.2
524.1
524.2
502.1
502.2
524.1
524.2
502.1
502.2
524.1
524.2
502.1
502.2
524.1
524.2
502.2
503.1
524.1
524.2
502.2
503.1
524.1
524.2
20.2
Ghange2
-------
Tabla IV-2. Approved Methodology for Organic Contaminants
Contaminant
MCLmg/1 Methodology
Reference
EPA
Tetrachtoroethylene
0.005
Toluene
1,2,4-Trichtarobenzene'
1,1,1 -Trichtoroe thane
0.07
0.2
1,1,2-Trichtoroethane*
0.005
Trichtoroethylene
0.005
Vinyl chloride
0.002
Xyiene (total)
10
Purge and Trap;Gas Chromatography-Electrolytic Conductivity Detector • 502.1
Purge and Trap;Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector • •-.,- .
Purge and Trap;Gas Chromatography-Photoionization Detector 503,1'
Purge and Trap;Packed Column-Gas Chromatography/Mass 5241
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography- 5022
Photoionization Detector-Electrolytic Conductivity Detector ' :
Purge and Trap;Gas Chromatography-Photoionization Detector 503.1
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Gas Chromatography-Photoionization Detector 593.1
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap;Capillary Column-Gas Chromatography- 502.2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap;Capillary Column-Gas Chromatography- 502.2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap;Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Gas Chromatography-Photoionization Detector 503.1
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Gas Chromatography-Electrolytic Conductivity Detector 502.1
Purge and Trap;Capillary Column-Gas Chromatography- 502.2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass 524 2
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography- 502 2
Photoionization Detector-Electrolytic Conductivity Detector
Purge and Trap;Gas Chromatography-Photoionization Detector 503.1
Purge and Trap;Packed Column-Gas Chromatography/Mass 524 1
Spectroscopy
Purge and Trap;Capillary Column-Gas Chromatography/Mass Spectroscopy 524 2
Change 2
20.3
-------
Table IV-2. Approved Methodology for Organic Contaminants
* MCL was stayed 5/29/92.
** Boron trifluoride may be used for esteriflcation. ,
1 "Methods for the Determination of Organic Compounds in Drinking Water," EPA 600/4-88.-039, December 1988 (Revised July 1991),
EPA Environmental Monitoring Systems Laboratory, Cincinnati, Ohio 45268.
2 "Methods for the Determination of Organic Compounds in Drinking Water," Supplement 1, EPA 600/4-90-020, July 1990, EMSL, EPA,
Cincinnati, Ohio 45268.
3 Federal Register, Vol. 56, No. 26, Thursday, February 7,1991, p. 5098-5122.
4 "The Analysis of Trihalomethanes in finished Waters by the Purge and Trap Method," Method 501.1, EMSL, EPA, Cincinnati, Ohio
45268.
5 The Analysis of Trihalomethanes in Drinking Water by Liquid/Liquid Extraction," Method 501.2, EMSL, EPA, Cincinnati, Ohio 45268.
6 The Determination of the Maximum Total Trihalomethane Potential," Method 510.1, EMSL, EPA, Cincinnati, Ohio 45268.
20.4
Change 2
-------
Table 1V-3. Recommended Methods for Secondary Contaminants
Reference (Method Number)
Contaminant
Alumfaum
Chloride
Corrosivity
Iron
Manganese
Residue,
total filterable
Silver
Suilata
Zinc
Methodology1
Atomic Absorption
Inductively couplet
Potentiometric
Langelier Index
Aggressive Index
Atomic Absorption
Inductively coupled
Atomic Absorption
Inductively coupled
Gravimetric
Atomic Absorption
Inductively coupled
Turbid (metric
Atomic Absorption
Inductively coupled
direct aspiration
furnace
platform
plasma emission spectrometry
mass spectrometry
: direct aspiration
: furnace
plasma emission spectrometry
: direct aspiration
: furnace
plasma emission spectrometry
direct absorption
furnace
platform
plasma emission spectrometry
mass spectrometry
: direct aspiration
plasma emission spectrometry
EPA2
202.1
202.2
200.97
200. 77
200.87
236.1
236.2
200 .77
243.1
243.2
200 .77
• ,*•,
160.1
272.1
272.2
200.97
200.77 .
200.87
375.4
289.1
200. 77
ASTM3 SM4
303C5
3045
31 208
408C11
20311
D1068-90A 303A5
D1068-90C 304s
31 208
D858-90A 303A5
D858-90C 3045
31 208 ,
2540-C
303A5
304s
• 3120B8
427-C11
301A11
Others
I-3051-856
C400-00'12
-. I-1750-846
I-3720-856
I, the sample may be analyzed without digestion if a total
I -i^^^SS^C^N^^^S^ Environment Monitoring Systems Laboratory,
. _ -^ America,, society of Testing Materials, 1916 Race Street, Philadelphia PA 19103
jVWalerVolluironT^ 1?'h Editi°n' American Public Health Associa'i°n, American Water Works
\ Examination of Water and Wastewater," 16th Edition, American Public Health Association American Water Works
. —_-...-,., ..«.„, . v.,u,,on Control Federation, 1985. ' .
iiia'il?^ 'r8 D.ele.rm.ination °' Inorganic Substances in Water and Fluvial Sediments," Techniques of Water-Resources Investigations of the
United States Geoloaical Snn™ Ron.,* r.h=,ntQr A1,1989, Open-File Services Section, Western Distribution Branch, U.S. Geological Survey!, Mi
— _r, L/vJ 80225. i
i Environmental Samples," EPA 600/4-91-01 O.June 1991, EPA Environmental Monitoring Systems
A 400 ml aliquot must be prepared by 3030F part 3b prior to analysis
%ms l^^tor^AS OH04n5S268Water ^ '^ Chromat°9raPhy'" Metnod 300-OA. Au9ust 1991 . EPA Environmental Monitoring •
Sa StrSEd°MA 01TO* USin9 ^ C°lUm" Cnromat°3raPny-" Method-A-1000, Millipore Corp., .Waters Chromatography Division, 34
SS^^ 14th Edition' American Publi? Health Ass^iation' American Water wo^
" Cement p'Pe- 4 in- through 1 6 in. for Water and Other Liquids," AWWA C400-80, Revision of C400-77, AWWA,
"Ollidal Methods of Analysis of the AOAC," 15th Edition, Association of Official Analytical Chemists, 1 990.
Change 2
21
-------
Table IV-4. Sample Collection, Containers, and Preservation for Inorganic Contaminants1
Contaminant
Alkalinity
Antimony
Arsenic
Asbestos
Barium
Beryllium
Cadmium
Calcium
Chloride
Chromium
Copper
Cyanide
Fluoride
Free Chlorine
Residual
Lead
Mercury
Nickel
Nitrate N
Total Nitrate/Nitrite
Nitrite-N
o-Phosphate
pH
Selenium
Silica
Sodium
Temperature
Thallium
Total Filterable
Residue (TDS)
Turbidity
Preservative2
Cool4°C
Cone HNOa to pH <2
Cone HNOa to pH <2
Cool 4°C5
Cone HNOa to pH <2
Cone HNOa to pH <2
Cone HNOa to pH < 2
Cone HNOa to pH <2
None
Cone HNOa to pH <2
Cone HNOs to pH < 2
NaOHtopH >12,
Cool 4°C
0.6g ascorbic acid6
None
None
Cone HNOa to pH <2
Cone HNOa to pH <-2
Cone HNOa to pH < 2
Cool 4°C
Cone H2SO4, to pH < 2
Cool 4°C
Filter immediately, Cool 4°C
None
Cone HNOa to pH < 2
Cool 4°C
Cone HNOa to pH< 2
None
Cone HNOa to pH <2
Cool 4°C
Cool 4°C
Container3
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
P or G
PorG,.
PorG
PorG
'
PorG
PorG
P or G
PorG
PorG
PorG
PorG ' '
PorG
PorG
PorG
PorG ,
P
' P or G
P or G
PorG
PorG
PorG
Maximum
Holding Time4
14 days
6 months
6 months
6 months
6 months
6 months
6 months
28 days <
6 months '
I ' '
i 6 months
14 days
1 month
Analyze immediately7
6 months
28 days
6 months
28 days
28 days
48 hours
48 hours
Analyze immediately7
6 months
28 days
6 months
Analyze immediately
6 months
7 days
48 hours
1 The laboratory director must reject any samples, taken for compliance purposes, not meeting these criteria and notify the authority requesting the
2 IHHNo'a cannot be used because of shipping restrictions, immediately ship the sample to the laboratory at ambient temperature. Upon receipt, the
sample must be acidified with cone. HNO3 to pH <2 and held.for at least 16 hours before analysis.
3 P = plastic, hard or soft; G = glass, hard or soft.
In all cases, samples should be analyzed as soon after collection as possible.
5 '
,
These samples should never be frozen. ,
6 Ascorbic acid should only be used in the presence of residual chlorine.
7 "Analyze immediately" generally means within 15 minutes of sample collection.
22
Change 2
-------
Tafate IV-5. Sample Collection, Containers, and Preservation for Organic Contaminants
Holding Time
Contaminant
Non-Volatile SOCs
TTHMs
VOCs
Method
504
505
506
507
508A
508
515.1
525.1
531.1
547
548
549
550
550.1
1613
501.1
501.2
510.1
502.1
502.2
503.1
Preservative
3 mg/40 ml sodium thiosulfate
HCI to pH 2
Cool 4° C
3 mg/40 ml sodium thiosulfate
Cool 4° C
60 mg/l sodium thiosulfate
Cool 4°C
10 mg/l mercuric chloride"
80 mg/l sodium thiosulfate
Cool 4° C
Cool 4° C
10 mg/l mercuric chloride"
80 mg/l sodium thiosulfate
Cool 4° C
10 mg/l mercuric chloride"
80 mg/I sodium thiosulfate
Cool 4° C
40-50 mg/l sodium sulfite
HCI to pH < 2
Cool 4° C
Monochloracetic acid to pH 3
80 mg/I sodium thiosulfate
Cool 4° C until storage
Store at -10°C
100 mg/I sodium thiosulfate
Cool 4°C
Cool 4°C
100 mg/I sodium thiosulfate
H2S04topH2
Cool 4°C
,100 mg/l sodium thiosulfate
6N HCL to pH < 2
Cool 4°C
100 mg/l sodium thiosulfate
6N HCL to pH < 2
Cool 4°C
80mg/l sodium thiosulfate
Cool 4°C
3 mg/40 ml sodium thiosulfate
(except for MTTHM) or Sodium
Sulfite
3 mg/40 ml sodium thiosulfate
(except for MTTHM) or Sodium
Sulfite
Cool 4° C
25 mg/40 ml ascorbic acid or
3 mg/40 ml sodium thiosulfate
1:1 HCItopH<2
Cool 4° C
25 mg/40 ml ascorbic acid or
3 mg/40 ml sodium thiosulfate
1:1 HCItopH<2
Cool 4° C
25 mg/60 ml ascorbic acid or
3 mg/40 ml sodium thiosulfate
1:1 HCItopH<2
Cool 4° C
Container
Glass
Teflon cap liners
Glass
Teflon cap liners
Glass(dark)
Teflon cap liners
Glass (dark)
Teflon cap liners
Glass
Teflon cap liners
Glass
Teflon cap liners
Glass(dark)
Teflon cap liners
Glass
Teflon cap liners
Glass
Teflon cap liners
Glass(dark)
Teflon cap liners
Glass
Teflon cap liners
Amber PVC high density
or amber silanized glass
Glass(dark)
Teflon cap liners
Glass (dark)
Teflon cap liners
Glass (dark)
Glass
Silicon/Teflon cap liners
Glass
Silicon/Teflon cap liners
Glass (dark)
Silicon/Teflon cap liners
Glass
Silicon/Teflon cap liners
Glass
Silicon/Teflon cap liners
Glass
Silicon/Teflon cap liners
To Extraction
28 days
14 days*
14 days
14 days
14 days
7 days
14 days
7 days
28daysat-10°C
14 days
7 days
7 days
7 days
7 days
—
14 days
14 days
14 days
14 days
14 days
14 days
After Extraction
Analyze
immediately
Analyze
immediately
14 days
14 days
30 days
14 days
28 days
30 days
No extract
No extract
1 day
21 days
40 days
40 days
40 days
—
—
—
—
"
Change 2
23.0
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Table IV-5. Sample Collection, Containers, and Preservation for Organic Contaminants
Holding Time
Contaminant
Method
Preservative
Container
To Extraction After Extraction
524.1 25 mg/60 ml ascorbic acid
1:1 HCI to pH < 2
Cool 4° C
524.2 25 mg/60 ml ascorbic acid
1:1 HCI to pH< 2
Cool 4° C "
Glass 14 days
Silicon/Teflon cap liners
Glass .' 14 days
Silicon/Teflon cap liners
The holding time for Heptachlor under this method is 7 days.
Samples that have been preserved with HgCte may be disposed of in at least two ways: as a hazardous waste, or by passing over an
absorbent column (i.e., Alumina, activated with carbon, etc.) for mercury absorption, with the effluent analyzed periodically for break-
through. The absorbent would then be disposed of as a hazardous waste. Other techniques may be applicable.
23.1
Change 2
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±30% at£ 0.006 mg/L
2 standard deviations based on study statistics
±15% at > 0.15 mg/L
±15% at > 0.001 mg/L
±20% at > 0.002 mg/L
±15% at > 0.01 mg/L
±10% at > 0.050 mg/L
±25% at > 0.1 mg/L
±10%at£l to 10 mg/L
±30% at > 0.005
±30% at > 0.0005 mg/L
±15% at SL 0.01 mg/L
±10% at > 0.4 mg/L
±15% at > 0.4 mg/L
±20% at > 0.01 mg/L
±30% at£ 0.002 mg/L
Tabte 1V-6. Laboratory Certification Criteria Based on Percent Deviation from True Values
inorganic
Antimony
Arsenic*
Asbestos
Barium
Beryllium
Cadmium
Chlorine
Chlorine dioxide
Chromium
Copper
Cyanide
Fluoride
Iron
Lead
Manganese
Mercury
Nickel
Nitrate
Nitrite
Ozone
Selenium
Sodium
Thallium
Turbidity
Certification criteria have not been provided due to certification being a state prerogative for the following parameters: alkalinity, calcium,
conductivity, orthophosphate, pH, silica, and temperature.
Oraanlcs
VOCs ±20% >10 ng/I
±40%s10ng/l
Non-Volatile SOCs
Adipatos
[Di(othylhexyl) adipate]
Alachlor
Aldicarb
Aldicarb sulfoxide
Aldicarb sulfone
Atrazlne
Carbofuran
Chtordane
Dalapon
DBCP
2,4-D
Dinoseb
Diquat
Endothall
Endrin
EOB
Glyphosate
Heptachlor
Heptachlor epoxlde
Hexachlorobenzene
Hexachlorocyclopentadiene
Lin da no
Methoxychlor
Oxamyl (Vydate)
PAHs [Bonzo (a) pyrene]
Pentachlorophenol
Phth slates
[Di(ethylhezyl)phthalate]
Pfctoram
PCBsas
Decachlorobiphenyl
SJmazine
Toxaphene
2,3,7,8 TCDD(Dioxin)
2.4.5-TP (silvex)
2 standard deviations based on study statistics
±45%
Stayed
Stayed
Stayed
±45%
±45%
±45%
2 standard deviations based on study statistics
±40%
±50%
2 standard deviations based on study statistics
2 standard deviations based on study statistics
2 standard deviations based on study statistics
±30%
±40%
2 standard deviations based on study statistics
±45%
±45%
2 standard deviations based on study statistics
2 standard deviations based on study statistics
±45%
±45%
2 standard deviations based on study statistics
2 standard deviations based on study statistics
±50%
2 standard deviations based on study statistics
2 standard deviations based on study statistics
0-200%
2 standard deviations based on study statistics
±45%
2 standard deviations based on study statistics
±50%
* Current crkeria will be revised in 1994.
" C - estimate of concentration.
Change 2
24
*U.S.GOVERNMENTPfUNnNGOFFlCE:1992 -€f8 -003/60065
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