&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         REMOVE SUPERSEDED PAGES AND INSERT REVISED PAGES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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                                              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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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

-------
   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

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   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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