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40-CFR-23-136.3 (Test Procedures For Specified Analytes)
40-CFR-23-136.3 (Test Procedures For Specified Analytes)
CodeofFederalRegulations
Title40ProtectionofEnvironment
Volume:23
Date:20140701
OriginalDate:20140701
Title:Section136.3Identificationoftestprocedures.
Context:Title40ProtectionofEnvironment.CHAPTERIENVIRONMENTALPROTECTION
AGENCY(CONTINUED).SUBCHAPTERDWATERPROGRAMS(CONTINUED).PART136
GUIDELINESESTABLISHINGTESTPROCEDURESFORTHEANALYSISOFPOLLUTANTS.
136.3 Identificationoftestprocedures.
(a)Parametersorpollutants,forwhichmethodsareapproved,arelistedtogetherwithtestprocedure
descriptionsandreferencesinTablesIA,IB,IC,ID,IE,IF,IG,andIH.ThemethodslistedinTablesIA,
IB,IC,ID,IE,IF,IG,andIHareincorporatedbyreference,seeparagraph(b)ofthissection,withthe
exceptionofEPAMethods200.7,601613,624,625,1613,1624,and1625.ThefulltextsofMethods
601613,624,625,1613,1624,and1625areprintedinappendixAofthispart136,andthefulltextof
Method200.7isprintedinappendixCofthispart136.Thefulltextfordeterminingthemethoddetection
limitwhenusingthetestproceduresisgiveninappendixBofthispart136.ThefulltextofMethod200.7
isprintedinappendixCofthispart136.Intheeventofaconflictbetweenthereportingrequirementsof
40CFRparts122and125andanyreportingrequirementsassociatedwiththemethodslistedinthese
tables,theprovisionsof40CFRparts122and125arecontrollingandwilldetermineapermittee's
reportingrequirements.Thefulltextofthereferencedtestproceduresareincorporatedbyreferenceinto
TablesIA,IB,IC,ID,IE,IF,IG,andIH.Thedischargeparametervaluesforwhichreportsarerequired
mustbedeterminedbyoneofthestandardanalyticaltestproceduresincorporatedbyreferenceand
describedinTablesIA,IB,IC,ID,IE,IF,IG,andIHorbyanyalternatetestprocedurewhichhasbeen
approvedbytheAdministratorundertheprovisionsofparagraph(d)ofthissectionand136.4and
136.5.Undercertaincircumstancesparagraph(c)ofthissection,136.5(a)through(d)or40CFR
401.13,otheradditionaloralternatetestproceduresmaybeused.
TableIAListofApprovedBiologicalMethodsforWastewaterandSewageSludge
Standard AOAC,
Parameterandunits Method1 EPA Other
methods ASTM,USGS
Bacteria:
p.1323
MostProbableNumber
1.Coliform(fecal),numberper100 168011 9221CE
(MPN),5tube,3dilution,
mLornumberpergramdryweight 15.1681 2006.
or
1120
Membranefilter(MF)2, 9222D
p.1243 B0050854.
singlestep 1997
2.Coliform(fecal)inpresenceof 9221CE
MPN,5tube,3dilution,or p.1323
chlorine,numberper100mL 2006.
9222D
MF2,singlestep5 p.1243
1997.
3.Coliform(total),numberper100 9221B
MPN,5tube,3dilution,or p.1143
mL 2006.
MF2,singlesteportwo
p.1083 9222B1997 B0025854
step
4.Coliform(total),inpresenceof
MPN,5tube,3dilution,or p.1143 9221B2006
chlorine,numberper100mL
9222(B+
MF2withenrichment5 p.1113
B.5c)1997
9221B.1
MPN6816multipletube,
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5. E.coli, numberper100mL21 or 2006/9221F
20061214
Colilert13
multipletube/multiplewell, 9223B200
991.1510 18Colilert
or 413
18131718
mColiBlue24
MF2678singlestep 160322
19
6.Fecalstreptococci,numberper 9230B
MPN,5tube3dilution,or p.1393
100mL 2007.
9230C
MF2,or p.1363 B0055854
2007
Platecount p.1433
9230C
MF2678singlestepor 160025
2007
Platecount p.1433
8. Salmonella, numberpergram
MPNmultipletube 168223
dryweight11
AquaticToxicity:
9.Toxicity,acute,freshwater Ceriodaphniadubia
organisms,LC50,percenteffluent 2002.0.26
acute
Daphniapuplex and
2021.0.26
Daphniamagna acute
FatheadMinnow,
Pimephalespromelas,
2000.0.26
andBannerfinshiner,
Cyprinellaleedsi, acute
RainbowTrout,
Oncorhynchusmykiss,
andbrooktrout, 2019.0.26
Salvelinusfontinalis,
acute
10.Toxicity,acute,estuarineand
marineorganismsoftheAtlantic Mysid, Mysidopsisbahia,
OceanandGulfofMexico,LC50, 2007.0.26
acute
percenteffluent
SheepsheadMinnow,
Cyprinodonvariegatus, 2004.026
acute
Silverside, Menidia
beryllina,Menidia
2006.026
menidia, and Menidia
peninsulae, acute
11.Toxicity,chronic,freshwater Fatheadminnow,
organisms,NOECorIC25,percent Pimephalespromelas, 1000.0.27
effluent larvalsurvivalandgrowth
Fatheadminnow,
Pimephalespromelas,
1001.0.27
embryolarvalsurvivaland
teratogenicity
Daphnia, Ceriodaphnia
dubia, survivaland 1002.0.27
reproduction
Greenalga, Selenastrum
capricornutum, growth 1003.0.27
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12.Toxicity,chronic,estuarineand
marineorganismsoftheAtlantic Sheepsheadminnow,
OceanandGulfofMexico,NOEC Cyprinodonvariegatus, 1004.0.28
orIC25,percenteffluent larvalsurvivalandgrowth
Sheepsheadminnow,
Cyprinodonvariegatus,
1005.0.28
embryolarvalsurvivaland
teratogenicity
Inlandsilverside, Menidia
beryllina, larvalsurvival 1006.0.28
andgrowth
Mysid, Mysidopsisbahia,
survival,growth,and 1007.0.28
fecundity
Seaurchin, Arbacia
1008.0.28
punctulata, fertilization
TableIAnotes:
1Themethodmustbespecifiedwhenresultsarereported.
2A0.45mmembranefilter(MF)orotherporesizecertifiedbythemanufacturertofullyretainorganismstobecultivated
andtobefreeofextractableswhichcouldinterferewiththeirgrowth.
3MicrobiologicalMethodsforMonitoringtheEnvironment,Water,andWastes,EPA/600/878/017.1978.USEPA.
4U.S.GeologicalSurveyTechniquesofWaterResourceInvestigations,Book5,LaboratoryAnalysis,ChapterA4,Methods
forCollectionandAnalysisofAquaticBiologicalandMicrobiologicalSamples.1989.USGS.
5BecausetheMFtechniqueusuallyyieldslowandvariablerecoveryfromchlorinatedwastewaters,theMostProbable
Numbermethodwillberequiredtoresolveanycontroversies.
6Testsmustbeconductedtoprovideorganismenumeration(density).Selecttheappropriateconfigurationof
tubes/filtrationsanddilutions/volumestoaccountforthequality,character,consistency,andanticipatedorganismdensityof
thewatersample.
7WhentheMFmethodhasbeenusedpreviouslytotestwaterswithhighturbidity,largenumbersofnoncoliformbacteria,
orsamplesthatmaycontainorganismsstressedbychlorine,aparalleltestshouldbeconductedwithamultipletube
techniquetodemonstrateapplicabilityandcomparabilityofresults.
8Toassessthecomparabilityofresultsobtainedwithindividualmethods,itissuggestedthatsidebysidetestsbeconducted
acrossseasonsoftheyearwiththewatersamplesroutinelytestedinaccordancewiththemostcurrentStandardMethods
fortheExaminationofWaterandWastewaterorEPAalternatetestprocedure(ATP)guidelines.
9AnnualBookofASTMStandardsWaterandEnvironmentalTechnology,Section11.02.2000,1999,1996.ASTM
International.
10OfficialMethodsofAnalysisofAOACInternational.16thEdition,4thRevision,1998.AOACInternational.
11Recommendedforenumerationoftargetorganisminsewagesludge.
12Themultipletubefermentationtestisusedin9221B.12006.Lactosebrothmaybeusedinlieuoflauryltryptosebroth
(LTB),ifatleast25paralleltestsareconductedbetweenthisbrothandLTBusingthewatersamplesnormallytested,and
thiscomparisondemonstratesthatthefalsepositiverateandfalsenegativeratefortotalcoliformusinglactosebrothisless
than10percent.Norequirementexiststorunthecompletedphaseon10percentofalltotalcoliformpositivetubesona
seasonalbasis.
13Thesetestsarecollectivelyknownasdefinedenzymesubstratetests,where,forexample,asubstrateisusedtodetect
theenzymeglucuronidaseproducedby E.coli.
14Afterpriorenrichmentinapresumptivemediumfortotalcoliformusing9221B.12006,allpresumptivetubesorbottles
showinganyamountofgas,growthoraciditywithin48h3hofincubationshallbesubmittedto9221F2006.Commercially
availableECMUGmediaorECmediasupplementedinthelaboratorywith50g/mLofMUGmaybeused.
15Method1680:FecalColiformsinSewageSludge(Biosolids)byMultipleTubeFermentationUsingLaurylTryptoseBroth
(LTB)andECMedium,EPA821R10003.April2010.U.S.EPA.
16Samplesshallbeenumeratedbythemultipletubeormultiplewellprocedure.Usingmultipletubeprocedures,employan
appropriatetubeanddilutionconfigurationofthesampleasneededandreporttheMostProbableNumber(MPN).Samples
testedwithColilertmaybeenumeratedwiththemultiplewellprocedures,QuantiTray,QuantiTray/2000,andthe
MPNcalculatedfromthetableprovidedbythemanufacturer.
17Colilert18isanoptimizedformulationoftheColilertforthedeterminationoftotalcoliformsand E.coli thatprovides
resultswithin18hofincubationat35Cratherthanthe24hrequiredfortheColilerttestandisrecommendedformarine
watersamples.
18DescriptionsoftheColilert,Colilert18,QuantiTray,andQuantiTray/2000maybeobtainedfromIDEXX
Laboratories,Inc.
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19AdescriptionofthemColiBlue24test,isavailablefromHachCompany.
20Method1681:FecalColiformsinSewageSludge(Biosolids)byMultipleTubeFermentationusingA1Medium,EPA
821R06013.July2006.U.S.EPA.
21Recommendedforenumerationoftargetorganisminwastewatereffluent.
22Method1603: Escherichiacoli ( E.coli )inWaterbyMembraneFiltrationUsingModifiedmembraneThermotolerant
Escherichiacoli Agar(modifiedmTEC),EPA821R09007.December2009.U.S.EPA.
23Method1682: Salmonella inSewageSludge(Biosolids)byModifiedSemisolidRappaportVassiliadis(MSRV)Medium,
EPA821R06014.July2006.U.S.EPA.
24AdescriptionoftheEnterolerttestmaybeobtainedfromIDEXXLaboratoriesInc.
25Method1600:EnterococciinWaterbyMembraneFiltrationUsingmembraneEnterococcusIndoxylDGlucosideAgar
(mEI),EPA821R09016.December2009.U.S.EPA.
26MethodsforMeasuringtheAcuteToxicityofEffluentsandReceivingWaterstoFreshwaterandMarineOrganisms.EPA
821R02012.FifthEdition,October2002.U.S.EPA.
27ShorttermMethodsforEstimatingtheChronicToxicityofEffluentsandReceivingWaterstoFreshwaterOrganisms.
EPA821R02013.FourthEdition,October2002.U.S.EPA.
28ShorttermMethodsforEstimatingtheChronicToxicityofEffluentsandReceivingWaterstoMarineandEstuarine
Organisms.EPA821R02014.ThirdEdition,October2002.U.S.EPA.
TableIBListofApprovedInorganicTestProcedures
Standard
Parameter Methodology58 EPA52 ASTM USGS/AOAC/Other
methods
1.Acidity,as Electrometricendpointor D1067
CaCO3,mg/L 2310B1997 I102085.2
phenolphthaleinendpoint 06
310.2(Rev.
Automatic I203085.2
1974)1
3.Aluminum Digestion,4followedbyanyofthe
Total,4mg/L following:
3111D1999
AAdirectaspiration36 or3111E I305185.2
1999
AAfurnace 3113B2004
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
D4190
DirectCurrentPlasma(DCP)36 Seefootnote.34
08
Colorimetric(Eriochromecyanine 3500AlB
R) 2001
Manualdistillation6orgas 4500NH3B
4.Ammonia(as 350.1,Rev.2.0
diffusion(pH>11),followedby 973.493.
N),mg/L (1993) 1997
anyofthefollowing:
D1426
Nesslerization 973.493,I352085.2
08(A)
4500NH3C
Titration
1997
4500NH3D D1426
Electrode 1997orE 08(B)
1997
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Manualphenate,salicylate,or 4500NH3F
othersubstitutedphenolsin Seefootnote.60
Berthelotreactionbasedmethods 1997
Automatedphenate,salicylate,or 4500NH3G
350.130,Rev.
othersubstitutedphenolsin 19974500 I452385.2
2.0(1993)
Berthelotreactionbasedmethods NH3H1997.
Ion D6919
Automatedelectrode Seefootnote.7
Chromatography 09
5.Antimony Digestion,4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration36 3111B1999
AAfurnace 3113B2004
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
3114B2009
D2972
AAgaseoushydride or3114C I306285.2
08(B)
2009
D2972
AAfurnace 3113B2004 I406398.49
08(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I402005.70
(1994) 05
3500AsB D2972
Colorimetric(SDDC) I306085.2
1997 08(A)
7.BariumTotal,4 Digestion4,followedbyanyofthe
mg/L following:
D4382
AAfurnace 3113B2004
02(07)
200.5,Rev4.2
(2003)68
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
DCP36 Seefootnote.34
8.Beryllium Digestion,4followedbyanyofthe
Total,4mg/L following:
3111D1999
D3645
AAdirectaspiration or3111E I309585.2
08(A)
1999
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200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
D4190
DCP Seefootnote.34
08
Seefootnote
Colorimetric(aluminon)
61
9.Biochemical 973.443,p.17.9,I
oxygendemand DissolvedOxygenDepletion 5210B2001 157878,8See
(BOD5),mg/L footnote.1063
10.Boron 4500BB
Colorimetric(curcumin) I311285.2
Total,37mg/L 2000
200.5,Rev4.2
(2003)68 D1976
ICP/AES 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
D4190
DCP Seefootnote.34
08
D1246
11.Bromide,mg/L Electrode I112585.2
05
300.0,Rev2.1 4110B
(1993)and 2000,C D4327
IonChromatography 993.30.3
300.11,Rev1.0 2000,D 03
(1997) 2000
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
12.Cadmium Digestion,4followedbyanyofthe
Total,4mg/L following:
D3557
3111B 974.27,3p.37.9,I
02(07)
AAdirectaspiration36 1999or3111 3135852orI3136
(Aor
C1999 85.2
B)
D3557
AAfurnace 3113B2004 02(07) I413889.51
(D)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976 I1472852orI4471
ICP/AES36 3120B1999
200.7,Rev.4.4 07 97.50
(1994)
200.8,Rev.5.4 D5673
ICP/MS (1994) 3125B2009 05 993.14,3I447197.50
D4190
DCP36 Seefootnote.34
08
D3557
Voltametry11 02(07)
(C)
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Colorimetric(Dithizone) 3500CdD
1990
13.Calcium Digestion,4followedbyanyofthe
Total,4mg/L following:
D511
AAdirectaspiration 3111B1999 I315285.2
08(B)
200.5,Rev4.2
(2003)68
ICP/AES 3120B1999 I447197.50
200.7,Rev.4.4
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
DCP Seefootnote.34
3500CaB D511
Titrimetric(EDTA)
1997 08(A)
D6919
IonChromatography
09
14.Carbonaceous
biochemical DissolvedOxygenDepletionwith
oxygendemand 5210B2001 Seefootnote.3563
nitrificationinhibitor
(CBOD5),mg/L12
15.Chemical 5220B
410.3(Rev. D1252 973.46,3p.17,9I
oxygendemand Titrimetric 1997orC
1978)1 06(A) 356085.2
(COD),mg/L 1997
4500Cl B D512
16.Chloride,mg/L Titrimetric:(silvernitrate) I118385.2
1997 04(B)
4500Cl C D512
(Mercuricnitrate) 973.51,3I118485.2
1997 04(A)
Colorimetric:manual I118785.2
4500Cl E
Automated(Ferricyanide) I218785.2
1997
4500Cl D
PotentiometricTitration
1997
D512
IonSelectiveElectrode
04(C)
300.0,Rev2.1
4110B2000
(1993)and D4327 993.303,I2057
IonChromatography or4110C
300.11,Rev1.0 03 90.51
2000
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
4500ClE
Amperometricdirect(lowlevel)
2000
4500ClB
Iodometricdirect 2000
4500ClC
Backtitrationetherendpoint15
2000
4500ClF
DPDFAS
2000
4500ClG
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Spectrophotometric,DPD 2000
Electrode Seefootnote.16
17A.Chlorine
4500ClD D1253
FreeAvailable, Amperometricdirect
2000 08
mg/L
4500ClE
Amperometricdirect(lowlevel)
2000
4500ClF
DPDFAS
2000
4500ClG
Spectrophotometric,DPD
2000
18.ChromiumVI 0.45micronFiltrationfollowedby
dissolved,mg/L anyofthefollowing:
D1687
3500CrB
Colorimetric(Diphenylcarbazide) 02(07) I123085.2
2009
(A)
19.Chromium Digestion,4followedbyanyofthe
Total,4mg/L following:
D1687
AAdirectaspiration36 3111B1999 02(07) 974.27,3I323685.2
(B)
AAchelationextraction 3111C1999
D1687
AAfurnace 3113B2004 02(07) I323393.46
(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
D1976
ICP/AES36 (2003),68200.7, 3120B1999 I447197.50
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I402005.70
(1994) 05
D4190
DCP36 Seefootnote.34
08
3500CrB
Colorimetric(Diphenylcarbazide)
2009
20.Cobalt Digestion,4followedbyanyofthe
Total,4mg/L following:
3111B1999 D3558
AAdirectaspiration or3111C 08(A p.37,9I323985.2
1999 orB)
D3558
AAfurnace 3113B2004 08(C) I424389.51
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I402005.70
(1994) 05
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D4190
DCP Seefootnote.34
08
21.Color,platinum
cobaltunitsor
dominant Colorimetric(ADMI) Seefootnote.18
wavelength,hue,
luminancepurity
Spectrophotometric
22.Copper Digestion,4followedbyanyofthe
Total,4mg/L following:
D1688
AAfurnace 3113B2004 I427489.51
07(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I402005.70
(1994) 05
D4190
DCP36 Seefootnote.34
08
3500CuB
Colorimetric(Neocuproine)
1999
3500CuC
(Bathocuproine) Seefootnote.19
1999
AutomatedUV
23.Cyanide
digestion/distillationand Kelada01.55
Total,mg/L
Colorimetry
SegmentedFlowInjection,InLine
D7511
UltravioletDigestion,followedby
09
gasdiffusionamperometry
D2036
ManualdistillationwithMgCl2, 4500CN B
335.4,Rev.1.0 09(A),
1999orC 10204001X.56
followedbyanyofthefollowing: (1993)57 D7284
1999
08
D2036
FlowInjection,gasdiffusion 09(A)
amperometry D7284
08
4500CN D2036
Titrimetric p.22.9
D1999 09(A)
4500CN E D2036
Spectrophotometric,manual 1999 09(A) I330085.2
335.4,Rev.1.0 10204001X,56I
SemiAutomated20
(1993)57 430285.2
D2036
IonChromatography
09(A)
4500CN F D2036
IonSelectiveElectrode
1999 09(A)
CyanideAmenabletoChlorination
24.Cyanide (CATC)Manualdistillationwith 4500CN D2036
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Available,mg/L MgCl2,followedbyTitrimetricor G1999 09(B)
Spectrophotometric
Flowinjectionandligand
D6888
exchange,followedbygas OIA167709.44
09
diffusionamperometry59
AutomatedDistillationand
Kelada01.55
Colorimetry(noUVdigestion)
Manualmicrodiffusionand D4282
colorimetry 02
4500F C D1179
Electrode,manual
1997 04(B)
Electrode,automated I432785.2
4500F D D1179
Colorimetric,(SPADNS)
1997 04(A)
4500F E
Automatedcomplexone
1997
300.0,Rev2.1
(1993)and 4110B2000 D4327
IonChromatography 993.30.3
300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
26.GoldTotal,4 Digestion,4followedbyanyofthe
mg/L following:
AAdirectaspiration 3111B1999
231.2(Issued
AAfurnace 3113B2004
1978)1
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
DCP Seefootnote.34
27.Hardness
Total,asCaCO3, 130.1(Issued
Automatedcolorimetric
1971)1
mg/L
D1126
Titrimetric(EDTA) 2340C1997 973.52B,3I133885.2
02(07)
CaplusMgastheircarbonates,
byinductivelycoupledplasmaor
2340B1997
AAdirectaspiration.(See
Parameters13and33).
D1293
28.Hydrogenion 4500H+B
Electrometricmeasurement 99(A 973.41,3I158685.2
(pH),pHunits 2000
orB)
150.2(Dec. Seefootnote,21I
Automatedelectrode
1982)1 258785.2
29.Iridium Digestion,4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111B1999
235.2(Issued
AAfurnace
1978)1
ICP/MS 3125B2009
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30.IronTotal,4 Digestion,4followedbyanyofthe
mg/L following:
3111B1999 D1068
AAdirectaspiration36 or3111C 05(A 974.27,3I338185.2
1999 orB)
D1068
AAfurnace 3113B2004
05(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
D4190
DCP36 Seefootnote.34
08
3500Fe D1068
Colorimetric(Phenanthroline) Seefootnote.22
1997 05(D)
4500NorgB
31.Kjeldahl Manualdigestion20and 1997orC D3590
Nitrogen5Total, distillationorgasdiffusion, 1997and 02(06) I451591.45
(asN),mg/L followedbyanyofthefollowing: 4500NH3B (A)
1997
4500NH3C
Titration 973.48.3
1997
D1426
Nesslerization
08(A)
4500NH3D
D1426
Electrode 1997orE 08(B)
1997
4500NH3G
350.1Rev2.0
Semiautomatedphenate 1997.4500
1993
NH3H1997
Manualphenate,salicylate,or 4500NH3F
othersubstitutedphenolsin Seefootnote.60
Berthelotreactionbasedmethods 1997
AutomatedMethodsforTKNthat
donotrequiremanualdistillation
Automatedphenate,salicylate,or
othersubstitutedphenolsin
Berthelotreactionbasedmethods 351.1(Rev.
I455178.8
colorimetric(autodigestionand 1978)1
distillation)
Blockdigester,followedbyAuto
Seefootnote.39
distillationandTitration
Blockdigester,followedbyAuto
Seefootnote.40
distillationandNesslerization
BlockDigester,followedbyFlow
injectiongasdiffusion(distillation Seefootnote.41
notrequired)
32.LeadTotal,4 Digestion,4followedbyanyofthe
mg/L following:
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3111B1999 D3559
AAdirectaspiration36 or3111C 08(A 974.27,3I339985.2
1999. orB)
D3559
AAfurnace 3113B2004 I440389.51
08(D)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
D1976
ICP/AES36 (2003)68200.7, 3120B1999 I447197.50
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
D4190
DCP36 Seefootnote.34
08
D3559
Voltametry11
08(C)
3500PbB
Colorimetric(Dithizone)
1997
33.Magnesium Digestion,4followedbyanyofthe
Total,4mg/L following:
D511
AAdirectaspiration 3111B1999 974.27,3I344785.2
08(B)
200.5,Rev4.2
(2003)68 D1976
ICP/AES 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
DCP Seefootnote.34
Gravimetric
D6919
IonChromatography
09
34.Manganese Digestion4followedbyanyofthe
Total,4mg/L following:
D858
AAdirectaspiration36 3111B1999 07(A 974.27,3I345485.2
orB)
D858
AAfurnace 3113B2004 07(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
D4190
DCP36 Seefootnote.34
08
3500MnB
Colorimetric(Persulfate) 920.203.3
1999
(Periodate) Seefootnote.23
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Total,4mg/L (1994) 02(07)
245.2(Issued
Coldvapor,Automated
1974)1
Coldvaporatomicfluorescence 245.7Rev.2.0
I446401.71
spectrometry(CVAFS) (2005)17
PurgeandTrapCVAFS 1631E43
36.Molybdenum Digestion,4followedbyanyofthe
Total,4mg/L following:
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I447197.50
(1994) 05
DCP Seefootnote.34
37.NickelTotal,4 Digestion4followedbyanyofthe
mg/L following:
3111B1999 D1886
AAdirectaspiration36 or3111C 08(A I349985.2
1999 orB)
D1886
AAfurnace 3113B2004 I450389.51
08(C)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
(2003)68 D1976
ICP/AES36 3120B1999 I447197.50
200.7,Rev.4.4 07
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14,3I402005.70
(1994) 05
D4190
DCP36 Seefootnote.34
08
300.0,Rev2.1
38.Nitrate(asN), (1993)and 4110B2000 D4327
IonChromatography 993.30.3
mg/L 300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
4500NO3
IonSelectiveElectrode
D2000
352.1(Issued 973.50,3419D17,p.
Colorimetric(Brucinesulfate)
1971)1 28.9
NitratenitriteNminusNitriteN
Seefootnote.62
(Seeparameters39and40)
4500NO3
Automatedhydrazine
H2000
Reduction/Colorimetric Seefootnote.62
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300.0,Rev2.1
(1993)and 4110B2000 D4327
IonChromatography 993.30.3
300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
40.Nitrite(asN), 4500NO2
Spectrophotometric:Manual Seefootnote.25
mg/L B2000
I4540852,See
Automated(Diazotization)
footnote.62
300.0,Rev2.1
(1993)and 4110B2000 D4327
IonChromatography 993.30.3
300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
41.Oilandgrease Hexaneextractablematerial
1664Rev.A 5520B
Total (HEM):nHexaneextractionand
1664Rev.B42 200138
recoverable,mg/L gravimetry
5520B
SilicageltreatedHEM(SGT
1664Rev.A 200138and
HEM):Silicageltreatmentand
1664Rev.B42 5520F
gravimetry
200138
42.Organiccarbon
D7573
Total(TOC), Combustion 5310B2000 973.473,p.14.24
09
mg/L
5310C
HeatedpersulfateorUV D4839
20005310D 973.473,p.14.24
persulfateoxidation 03
2000.
43.Organic
TotalKjeldahlN(Parameter31)
nitrogen(asN),
minusammoniaN(Parameter4)
mg/L
44.Ortho
Ascorbicacid
phosphate(asP),
method:
mg/L
4500PF
365.1,Rev.2.0 1999orG
Automated (1993) 973.563,I460185.2
1999
4500PE D515
Manualsinglereagent 973.55.3
1999 88(A)
365.3(Issued
Manualtworeagent
1978)1
300.0,Rev2.1
(1993)and 4110B2000 D4327
IonChromatography 993.30.3
300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
45.Osmium Digestion4,followedbyanyofthe
Total4,mg/L following:
AAdirectaspiration, 3111D1999
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AAfurnace 252.2(Issued
1978)1
4500OB
2001,C
46.Oxygen, 2001,D D888
Winkler(Azidemodification) 973.45B3,I157578.8
dissolved,mg/L 2001,E 09(A)
2001,F
2001
4500OG D888
Electrode I157678.8
2001 09(B)
D888 Seefootnote63See
LuminescenceBasedSensor
09(C) footnote.64
47.Palladium Digestion4,followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111B1999
253.21(Issued
AAfurnace
1978)
ICP/MS 3125B2009
DCP Seefootnote.34
D1783
420.11(Rev. 5530D
Colorimetric(4AAP)manual 01(A
1978) 200527
orB)
420.4Rev.1.0
Automatedcolorimetric(4AAP)
(1993)
49.Phosphorus
Gasliquidchromatography Seefootnote.28
(elemental),mg/L
4500PF
Automatedascorbicacid 365.1Rev.2.0 1999,G
973.563,I460085.2
reduction (1993) 1999,H
1999
200.7,Rev.4.4
ICP/AES436 (1994) 3120B1999 I447197.50
51.Platinum Digestion4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111B1999
255.2(Issued
AAfurnace
1978)1
ICP/MS 3125B2009
DCP Seefootnote.34
52.Potassium Digestion4,followedbyanyofthe
Total,4mg/L following:
200.7,Rev.4.4
ICP/AES 3120B1999
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
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(1994) 05
3500KB
Flamephotometric
1997
3500KC
Electrode
1997
D6919
IonChromatography
09
53.Residue
Gravimetric,103105 2540B1997 I375085.2
Total,mg/L
54.Residue D5907
Gravimetric,180 2540C1997 I175085.2
filterable,mg/L 03
55.Residuenon
Gravimetric,103105post D5907
filterable(TSS), 2540D1997 I376585.2
washingofresidue 03
mg/L
56.Residue Volumetric,(Imhoffcone),or
2540F1997
settleable,mg/L gravimetric
57.Residue 160.4(Issued
Gravimetric,550 2540E1997 I375385.2
Volatile,mg/L 1971)1
58.Rhodium Digestion4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration,or 3111B1999
265.2(Issued
AAfurnace
1978)1
ICP/MS 3125B2009
59.Ruthenium Digestion4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration,or 3111B1999
AAfurnace 267.21
ICP/MS 3125B2009
60.Selenium Digestion4,followedbyanyofthe
Total,4mg/L following:
D3859
AAfurnace 3113B2004 I466898.49
08(B)
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
D1976
ICP/AES36 (2003)68200.7, 3120B1999
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.143,I402005.70
(1994) 05
3114B
2009,or D3859
AAgaseoushydride I366785.2
3111C 08(A)
2009.
61.Silica 0.45micronfiltrationfollowedby
Dissolved,37mg/L anyofthefollowing:
4500SiO2 D859
Colorimetric,Manual I170085.2
C1997 05
4500SiO2E
Automated(Molybdosilicate) 1997orF I270085.2
1997
200.5,Rev4.2
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ICP/AES (2003)68200.7, 3120B1999 I447197.50
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
62.SilverTotal,4 Digestion4,29,followedbyanyof
31mg/L thefollowing:
3111B1999
974.273,p.379,I
AAdirectaspiration or3111C
372085.2
1999
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
D1976
ICP/AES (2003)68200.7, 3120B1999 I447197.50
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.143,I447197.50
(1994) 05
DCP Seefootnote.34
63.Sodium Digestion4,followedbyanyofthe
Total,4mg/L following:
200.5,Rev4.2
ICP/AES (2003)68200.7, 3120B1999 I447197.50
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
DCP Seefootnote.34
3500NaB
Flamephotometric
1997
D6919
IonChromatography 09
64.Specific
D1125
conductance, 120.11(Rev.
Wheatstonebridge 2510B1997 95(99) 973.403,I278185.2
micromhos/cmat 1982)
(A)
25C
4500SO42
65.Sulfate(as 375.2,Rev.2.0
SO4),mg/L Automatedcolorimetric F1997orG
(1993)
1997
4500SO42
Gravimetric C1997or 925.54.3
D1997
4500SO42 D516
Turbidimetric
E1997 07
300.0,Rev2.1
(1993)and 4110B2000 D4327
IonChromatography 993.303,I402005.70
300.11,Rev1.0 orC2000 03
(1997)
D6508
CIE/UV 4140B1997 D6508,Rev.2.54
00(05)
66.Sulfide(asS), 4500S2 B,
SamplePretreatment
mg/L C2000
4500S2 F
Titrimetric(iodine) I384085.2
2000
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Colorimetric(methyleneblue) 4500S2 D
2000
4500S2 G D4658
IonSelectiveElectrode
2000 08
67.Sulfite(as 4500SO3
SO3),mg/L Titrimetric(iodineiodate) 2 B2000
68.Surfactants, D2330
Colorimetric(methyleneblue) 5540C2000
mg/L 02
69.Temperature,
Thermometric 2550B2000 Seefootnote.32
C
70.Thallium Digestion4,followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111B1999
279.21(Issued
AAfurnace 3113B2004
1978)
200.9,Rev.2.2
STGFAA
(1994)
200.7,Rev.4.4
(1994)200.5 D1976
ICP/AES 3120B1999
Rev.4.2 07
(2003)68
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.143,I447197.50
(1994) 05
71.TinTotal,4 Digestion4,followedbyanyofthe
mg/L following:
AAfurnace 3113B2004
200.9,Rev.2.2
STGFAA
(1994)
200.5,Rev4.2
ICP/AES (2003)68200.7,
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
72.Titanium Digestion4followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111D1999
283.21(Issued
AAfurnace
1978)
200.7,Rev.4.4
ICP/AES
(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.14.3
(1994) 05
DCP Seefootnote.34
I386085.2See
73.Turbidity, 180.1,Rev.2.0 D1889 footnote.65See
Nephelometric 2130B2001
NTU53 (1993) 00 footnote.66See
footnote.67
74.Vanadium Digestion4,followedbyanyofthe
Total,4mg/L following:
AAdirectaspiration 3111D1999
D3373
AAfurnace 3113B2004
03(07)
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200.5,Rev4.2
D1976
ICP/AES (2003)68200.7, 3120B1999 I447197.50
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.143,I402005.70
(1994) 05
D4190
DCP Seefootnote.34
08
3500VB
Colorimetric(GallicAcid)
1997
75.ZincTotal4, Digestion4,followedbyanyofthe
mg/L following:
D1691
3111B1999
02(07) 974.273,p.379,I
AAdirectaspiration36 or3111C
(Aor 390085.2
1999
B)
289.21(Issued
AAfurnace
1978)
200.5,Rev4.2
D1976
ICP/AES36 (2003)68200.7, 3120B1999 I447197.50
07
Rev.4.4(1994)
200.8,Rev.5.4 D5673
ICP/MS 3125B2009 993.143,I402005.70
(1994) 05
D4190
DCP36 Seefootnote.34
08
3500ZnB
Colorimetric(Zincon) Seefootnote.33
1997
76.AcidMine
162769
Drainage
TableIBNotes:
1MethodsforChemicalAnalysisofWaterandWastes,EPA600/479020.RevisedMarch1983and1979,where
applicable.U.S.EPA.
2MethodsforAnalysisofInorganicSubstancesinWaterandFluvialSediments,TechniquesofWaterResource
InvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA1.,unlessotherwisestated.1989.USGS.
3OfficialMethodsofAnalysisoftheAssociationofOfficialAnalyticalChemists,MethodsManual,SixteenthEdition,4th
Revision,1998.AOACInternational.
4Forthedeterminationoftotalmetals(whichareequivalenttototalrecoverablemetals)thesampleisnotfilteredbefore
processing.Adigestionprocedureisrequiredtosolubilizeanalytesinsuspendedmaterialandtobreakdownorganicmetal
complexes(toconverttheanalytetoadetectableformforcolorimetricanalysis).Fornonplatformgraphitefurnaceatomic
absorptiondeterminationsadigestionusingnitricacid(asspecifiedinSection4.1.3ofMethodsfortheChemicalAnalysisof
WaterandWastes)isrequiredpriortoanalysis.Theprocedureusedshouldsubjectthesampletogentle,acidrefluxingand
atnotimeshouldthesamplebetakentodryness.Fordirectaspirationflameatomicabsorptiondeterminations(FLAA)a
combinationacid(nitricandhydrochloricacids)digestionispreferredpriortoanalysis.Theapprovedtotalrecoverable
digestionisdescribedasMethod200.2inSupplementIofMethodsfortheDeterminationofMetalsinEnvironmental
SamplesEPA/600R94/111,May,1994,andisreproducedinEPAMethods200.7,200.8,and200.9fromthesame
Supplement.However,whenusingthegaseoushydridetechniqueorforthedeterminationofcertainelementssuchas
antimony,arsenic,selenium,silver,andtinbynonEPAgraphitefurnaceatomicabsorptionmethods,mercurybycoldvapor
atomicabsorption,thenoblemetalsandtitaniumbyFLAA,aspecificormodifiedsampledigestionproceduremaybe
requiredandinallcasesthereferencedmethodwriteupshouldbeconsultedforspecificinstructionand/orcautions.For
analysesusinginductivelycoupledplasmaatomicemissionspectrometry(ICPAES),thedirectcurrentplasma(DCP)
techniqueortheEPAspectrochemicaltechniques(platformfurnaceAA,ICPAES,andICPMS)useEPAMethod200.2or
anapprovedalternateprocedure(e.g.,CEMmicrowavedigestion,whichmaybeusedwithcertainanalytesasindicatedin
TableIB)thetotalrecoverabledigestionproceduresinEPAMethods200.7,200.8,and200.9maybeusedforthose
respectivemethods.Regardlessofthedigestionprocedure,theresultsoftheanalysisafterdigestionprocedureare
reportedastotalmetals.
5Coppersulfateorothercatalyststhathavebeenfoundsuitablemaybeusedinplaceofmercuricsulfate.
6Manualdistillationisnotrequiredifcomparabilitydataonrepresentativeeffluentsamplesareonfiletoshowthatthis
preliminarydistillationstepisnotnecessary:however,manualdistillationwillberequiredtoresolveanycontroversies.In
general,theanalyticalmethodshouldbeconsultedregardingtheneedfordistillation.Ifthemethodisnotclear,the
laboratorymaycompareaminimumof9differentsamplematricestoevaluatetheneedfordistillation.Foreachmatrix,a
matrixspikeandmatrixspikeduplicateareanalyzedbothwithandwithoutthedistillationstep.(Atotalof36samples,
assuming9matrices).Ifresultsarecomparable,thelaboratorymaydispensewiththedistillationstepforfutureanalysis.
Comparableisdefinedas<20%RPDforalltestedmatrices).Alternativelythetwopopulationsofspikerecoverypercentages
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maybecomparedusingarecognizedstatisticaltest.
7IndustrialMethodNumber37975WEAmmonia,AutomatedElectrodeMethod,TechniconAutoAnalyzerII.February19,
1976.Bran&LuebbeAnalyzingTechnologiesInc.
8TheapprovedmethodisthatcitedinMethodsforDeterminationofInorganicSubstancesinWaterandFluvialSediments,
TechniquesofWaterResourcesInvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA1.1979.USGS.
9AmericanNationalStandardonPhotographicProcessingEffluents.April2,1975.AmericanNationalStandardsInstitute.
10InSituMethod100382009,BiochemicalOxygenDemand(BOD)MeasurementbyOpticalProbe.2009.InSitu
Incorporated.
11Theuseofnormalanddifferentialpulsevoltagerampstoincreasesensitivityandresolutionisacceptable.
12Carbonaceousbiochemicaloxygendemand(CBOD5)mustnotbeconfusedwiththetraditionalBOD5testmethodwhich
measurestotalBOD.Theadditionofthenitrificationinhibitorisnotaproceduraloption,butmustbeincludedtoreportthe
CBOD5parameter.AdischargerwhosepermitrequiresreportingthetraditionalBOD5maynotuseanitrificationinhibitorin
theprocedureforreportingtheresults.Onlywhenadischarger'spermitspecificallystatesCBOD5isrequiredcanthe
permitteereportdatausinganitrificationinhibitor.
13OICChemicalOxygenDemandMethod.1978.OceanographyInternationalCorporation.
14Method8000,ChemicalOxygenDemand,HachHandbookofWaterAnalysis,1979.HachCompany.
15Thebacktitrationmethodwillbeusedtoresolvecontroversy.
16OrionResearchInstructionManual,ResidualChlorineElectrodeModel9770.1977.OrionResearchIncorporated.The
calibrationgraphfortheOrionresidualchlorinemethodmustbederivedusingareagentblankandthreestandardsolutions,
containing0.2,1.0,and5.0mL0.00281Npotassiumiodate/100mLsolution,respectively.
17Method245.7,MercuryinWaterbyColdVaporAtomicFluorescenceSpectrometry,EPA821R05001.Revision2.0,
February2005.USEPA.
18NationalCouncilofthePaperIndustryforAirandStreamImprovement(NCASI)TechnicalBulletin253,December1971.
19Method8506,BiocinchoninateMethodforCopper,HachHandbookofWaterAnalysis.1979.HachCompany.
20Whenusingamethodwithblockdigestion,thistreatmentisnotrequired.
21IndustrialMethodNumber37875WA,Hydrogenion(pH)AutomatedElectrodeMethod,Bran&Luebbe(Technicon)
AutoanalyzerII.October1976.Bran&LuebbeAnalyzingTechnologies.
22Method8008,1,10PhenanthrolineMethodusingFerroVerIronReagentforWater.1980.HachCompany.
23Method8034,PeriodateOxidationMethodforManganese,HachHandbookofWastewaterAnalysis.1979.Hach
Company.
24MethodsforAnalysisofOrganicSubstancesinWaterandFluvialSediments,TechniquesofWaterResources
InvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA3,(1972Revised1987)p.14.1987.USGS.
25Method8507,Nitrogen,NitriteLowRange,DiazotizationMethodforWaterandWastewater.1979.HachCompany.
26Justpriortodistillation,adjustthesulfuricacidpreservedsampletopH4with1+9NaOH.
27ThecolorimetricreactionmustbeconductedatapHof10.00.2.
28Addison,R.F.,andR.G.Ackman.1970.DirectDeterminationofElementalPhosphorusbyGasLiquidChromatography,
JournalofChromatograph y,47(3):421426.
29Approvedmethodsfortheanalysisofsilverinindustrialwastewatersatconcentrationsof1mg/Landaboveare
inadequatewheresilverexistsasaninorganichalide.Silverhalidessuchasthebromideandchloridearerelativelyinsoluble
inreagentssuchasnitricacidbutarereadilysolubleinanaqueousbufferofsodiumthiosulfateandsodiumhydroxidetopH
of12.Therefore,forlevelsofsilverabove1mg/L,20mLofsampleshouldbedilutedto100mLbyadding40mLeachof2
MNa2S2O3andNaOH.Standardsshouldbepreparedinthesamemanner.Forlevelsofsilverbelow1mg/Ltheapproved
methodissatisfactory.
30TheuseofEDTAdecreasesmethodsensitivity.AnalystsmayomitEDTAorreplacewithanothersuitablecomplexing
reagentprovidedthatallmethodspecifiedqualitycontrolacceptancecriteriaaremet.
31Forsamplesknownorsuspectedtocontainhighlevelsofsilver(e.g.,inexcessof4mg/L),cyanogeniodideshouldbe
usedtokeepthesilverinsolutionforanalysis.Prepareacyanogeniodidesolutionbyadding4.0mLofconcentrated
NH4OH,6.5gofKCN,and5.0mLofa1.0NsolutionofI2to50mLofreagentwaterinavolumetricflaskanddiluteto
100.0mL.Afterdigestionofthesample,adjustthepHofthedigestateto>7topreventtheformationofHCNunderacidic
conditions.Add1mLofthecyanogeniodidesolutiontothesampledigestateandadjustthevolumeto100mLwithreagent
water(NOTacid).Ifcyanogeniodideisaddedtosampledigestates,thensilverstandardsmustbepreparedthatcontain
cyanogeniodideaswell.Prepareworkingstandardsbydilutingasmallvolumeofasilverstocksolutionwithwaterand
adjustingthepH>7withNH4OH.Add1mLofthecyanogeniodidesolutionandletstand1hour.Transfertoa100mL
volumetricflaskanddilutetovolumewithwater.
32WaterTemperatureInfluentialFactors,FieldMeasurementandDataPresentation,TechniquesofWaterResources
InvestigationsoftheU.S.GeologicalSurvey,Book1,ChapterD1.1975.USGS.
33Method8009,ZinconMethodforZinc,HachHandbookofWaterAnalysis,1979.HachCompany.
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34MethodAES0029,DirectCurrentPlasma(DCP)OpticalEmissionSpectrometricMethodforTraceElementalAnalysisof
WaterandWastes.1986Revised1991.ThermoJarrellAshCorporation.
35InSituMethod100482009,CarbonaceousBiochemicalOxygenDemand(CBOD)MeasurementbyOpticalProbe.
2009.InSituIncorporated.
36Microwaveassisteddigestionmaybeemployedforthismetal,whenanalyzedbythismethodology.ClosedVessel
MicrowaveDigestionofWastewaterSamplesforDeterminationofMetals.April16,1992.CEMCorporation
37Whendeterminingboronandsilica,onlyplastic,PTFE,orquartzlaboratorywaremaybeusedfromstartuntilcompletion
ofanalysis.
38Onlyusenhexane(nHexane85%minimumpurity,99.0%min.saturatedC6isomers,residuelessthan1mg/L)
extractionsolventwhendeterminingOilandGreaseparametersHexaneExtractableMaterial(HEM),orSilicaGelTreated
HEM(analogoustoEPAMethods1664Rev.Aand1664Rev.B).Useofotherextractionsolventsisprohibited.
39MethodPAIDK01,Nitrogen,TotalKjeldahl,BlockDigestion,SteamDistillation,TitrimetricDetection.RevisedDecember
22,1994.OIAnalytical.
40MethodPAIDK02,Nitrogen,TotalKjeldahl,BlockDigestion,SteamDistillation,ColorimetricDetection.Revised
December22,1994.OIAnalytical.
41MethodPAIDK03,Nitrogen,TotalKjeldahl,BlockDigestion,AutomatedFIAGasDiffusion.RevisedDecember22,1994.
OIAnalytical.
42Method1664Rev.BistherevisedversionofEPAMethod1664Rev.A.U.S.EPA.February1999,RevisionA.Method
1664,nHexaneExtractableMaterial(HEMOilandGrease)andSilicaGelTreatednHexaneExtractableMaterial(SGT
HEMNonpolarMaterial)byExtractionandGravimetry.EPA821R98002.U.S.EPA.February2010,RevisionB.Method
1664,nHexaneExtractableMaterial(HEMOilandGrease)andSilicaGelTreatednHexaneExtractableMaterial(SGT
HEMNonpolarMaterial)byExtractionandGravimetry.EPA821R10001.
43Method1631,MercuryinWaterbyOxidation,PurgeandTrap,andColdVaporAtomicFluorescenceSpectrometry,
EPA821R02019.RevisionE.August2002,U.S.EPA.TheapplicationofcleantechniquesdescribedinEPA'sMethod
1669: SamplingAmbientWaterforTraceMetalsatEPAWaterQualityCriteriaLevels, EPA821R96011,are
recommendedtoprecludecontaminationatlowlevel,tracemetaldeterminations.
44MethodOIA167709,AvailableCyanidebyLigandExchangeandFlowInjectionAnalysis(FIA).2010.OIAnalytical.
45OpenFileReport00170,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofAmmoniumPlusOrganicNitrogenbyaKjeldahlDigestionMethodandanAutomatedPhotometricFinish
thatIncludesDigestCleanupbyGasDiffusion.2000.USGS.
46OpenFileReport93449,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofChromiuminWaterbyGraphiteFurnaceAtomicAbsorptionSpectrophotometry.1993.USGS.
47OpenFileReport97198,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofMolybdenumbyGraphiteFurnaceAtomicAbsorptionSpectrophotometry.1997..USGS.
48OpenFileReport92146,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofTotalPhosphorusbyKjeldahlDigestionMethodandanAutomatedColorimetricFinishThatIncludes
Dialysis.1992.USGS.
49OpenFileReport98639,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofArsenicandSeleniuminWaterandSedimentbyGraphiteFurnaceAtomicAbsorptionSpectrometry.1999.
USGS.
50OpenFileReport98165,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofElementsinWholewaterDigestsUsingInductivelyCoupledPlasmaOpticalEmissionSpectrometryand
InductivelyCoupledPlasmaMassSpectrometry.1998.USGS.
51OpenFileReport93125,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofInorganicandOrganicConstituentsinWaterandFluvialSediments.1993..USGS.
52Unlessotherwiseindicated,allEPAmethods,excludingEPAMethod300.11,arepublishedinU.S.EPA.May1994.
MethodsfortheDeterminationofMetalsinEnvironmentalSamples,SupplementI,EPA/600/R94/111orU.S.EPA.August
1993.MethodsfortheDeterminationofInorganicSubstancesinEnvironmentalSamples,EPA/600/R93/100.EPAMethod
300.1isUSEPA.Revision1.0,1997,includingerratacoversheetApril27,1999.DeterminationofInorganicIonsinDrinking
WaterbyIonChromatography.
53Styrenedivinylbenzenebeads(e.g.,AMCOAEPA1orequivalent)andstabilizedformazin(e.g.,HachStablCalTMor
equivalent)areacceptablesubstitutesforformazin.
54MethodD6508,TestMethodforDeterminationofDissolvedInorganicAnionsinAqueousMatricesUsingCapillaryIon
ElectrophoresisandChromateElectrolyte.December2000.WatersCorp.
55Kelada01,KeladaAutomatedTestMethodsforTotalCyanide,AcidDissociableCyanide,andThiocyanate,EPA821B
01009,Revision1.2,August2001.USEPA.Note:A450WUVlampmaybeusedinthismethodinsteadofthe550W
lampspecifiedifitprovidesperformancewithinthequalitycontrol(QC)acceptancecriteriaofthemethodinagiven
instrument.Similarly,modifiedflowcellconfigurationsandflowconditionsmaybeusedinthemethod,providedthattheQC
acceptancecriteriaaremet.
56QuikChemMethod10204001X,DigestionandDistillationofTotalCyanideinDrinkingandWastewatersusingMICRO
DISTandDeterminationofCyanidebyFlowInjectionAnalysis.Revision2.2,March2005.LachatInstruments.
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57WhenusingsulfideremovaltestproceduresdescribedinEPAMethod335.41,reconstituteparticulatethatisfilteredwith
thesamplepriortodistillation.
58Unlessotherwisestated,ifthelanguageofthistablespecifiesasampledigestionand/ordistillationfollowedbyanalysis
withamethod,approveddigestionand/ordistillationarerequiredpriortoanalysis.
59SamplesanalyzedforavailablecyanideusingOIAnalyticalmethodOIA167709orASTMmethodD688809thatcontain
particulatemattermaybefilteredonlyaftertheligandexchangereagentshavebeenaddedtothesamples,becausethe
ligandexchangeprocessconvertscomplexescontainingavailablecyanidetofreecyanide,whichisnotremovedbyfiltration.
Analystsarefurthercautionedtolimitthetimebetweentheadditionoftheligandexchangereagentsandsamplefiltrationto
nomorethan30minutestoprecludesettlingofmaterialsinsamples.
60AnalystsshouldbeawarethatpHoptimaandchromophoreabsorptionmaximamightdifferwhenphenolisreplacedbya
substitutedphenolasthecolorreagentinBerthelotReaction(phenolhypochloritereaction)colorimetricammonium
determinationmethods.Forexamplewhenphenolisusedasthecolorreagent,pHoptimumandwavelengthofmaximum
absorbanceareabout11.5and635nm,respectivelysee,Patton,C.J.andS.R.Crouch.March1977.Anal.Chem.
49:464469.ThesereactionparametersincreasetopH>12.6and665nmwhensalicylateisusedasthecolorreagent
see,Krom,M.D.April1980.TheAnalyst105:305316.
61IfatomicabsorptionorICPinstrumentationisnotavailable,thealuminoncolorimetricmethoddetailedinthe19thEdition
of StandardMethods maybeused.Thismethodhaspoorerprecisionandbiasthanthemethodsofchoice.
62Easy(1Reagent)NitrateMethod,RevisionNovember12,2011.CraigChinchilla.
63HachMethod10360,LuminescenceMeasurementofDissolvedOxygeninWaterandWastewaterandforUseinthe
DeterminationofBOD5andcBOD5.Revision1.2,October2011.HachCompany.Thismethodmaybeusedtomeasure
dissolvedoxygenwhenperformingthemethodsapprovedinTableIBformeasurementofbiochemicaloxygendemand
(BOD)andcarbonaceousbiochemicaloxygendemand(CBOD).
64InSituMethod100282009,DissolvedOxygen(DO)MeasurementbyOpticalProbe.2009.InSituIncorporated.
65MitchellMethodM5331,DeterminationofTurbiditybyNephelometry.Revision1.0,July31,2008.LeckMitchell.
66MitchellMethodM5271,DeterminationofTurbiditybyNephelometry.Revision1.0,July31,2008.LeckMitchell.
67OrionMethodAQ4500,DeterminationofTurbiditybyNephelometry.Revision5,March12,2009.ThermoScientific.
68EPAMethod200.5,DeterminationofTraceElementsinDrinkingWaterbyAxiallyViewedInductivelyCoupledPlasma
AtomicEmissionSpectrometry,EPA/600/R06/115.Revision4.2,October2003.USEPA.
69Method1627,KineticTestMethodforthePredictionofMineDrainageQuality,EPA821R09002.December2011.US
EPA.
70TechniquesandMethodsBook5B1,DeterminationofElementsinNaturalWater,Biota,SedimentandSoilSamples
UsingCollision/ReactionCellInductivelyCoupledPlasmaMassSpectrometry,Chapter1,SectionB,MethodsoftheNational
WaterQualityLaboratory,Book5,LaboratoryAnalysis,2006.USGS.
71WaterResourcesInvestigationsReport014132,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWater
QualityLaboratoryDeterminationofOrganicPlusInorganicMercuryinFilteredandUnfilteredNaturalWaterWithCold
VaporAtomicFluorescenceSpectrometry,2001.USGS.
TableICListofApprovedTestProceduresforNonPesticideOrganicCompounds
Parameter1 Method EPA27 Standardmethods ASTM Other
1.Acenaphthene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000
92(98)
2.Acenaphthylene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
3.Acrolein GC 603.
6244,
GC/MS
1624B.
4.Acrylonitrile GC 603.
6244,
GC/MS
1624B.
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5.Anthracene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
624,
GC/MS 6200B1997.
1624B
Spectro Seefootnote3,
7.Benzidine
photometric p.1.
6255,
GC/MS 6410B2000.
1625B
HPLC 605.
8.Benzo(a)anthracene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
9.Benzo(a)pyrene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
10.Benzo(b)fluoranthene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
11.Benzo(g,h,i)perylene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
12.Benzo(k)fluoranthene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
Seefootnote3,
13.Benzylchloride GC
p.130.
Seefootnote6,
GC/MS
p.S102.
14.Butylbenzylphthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
15.bis(2Chloroethoxy)methane GC 611.
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16.bis(2Chloroethyl)ether GC 611.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
17.bis(2Ethylhexyl)phthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
21.4Bromophenylphenylether GC 611.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
Seefootnote3,
22.Carbontetrachloride GC 601 6200C1997
p.130.
624,
GC/MS 6200B1997.
1624B
625, Seefootnote9,
GC/MS 6410B2000.
1625B p.27.
Seefootnote3,
24.Chlorobenzene GC 601,602 6200C1997
p.130.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
26.2Chloroethylvinylether GC 601.
624,
GC/MS
1624B.
Seefootnote3,
27.Chloroform GC 601 6200C1997
p.130.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
29.2Chloronaphthalene GC 612.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
625, Seefootnote9,
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GC/MS 1625B 6410B2000 p.27.
31.4Chlorophenylphenylether GC 611.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
32.Chrysene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
33.Dibenzo(a,h)anthracene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
624,
GC/MS 6200B1997.
1624B
624, Seefootnote9,
GC/MS 6200B1997
1625B p.27.
624, Seefootnote9,
GC/MS 6200B1997
1625B p.27.
624, Seefootnote9,
GC/MS 6200B1997
1625B p.27.
625,
38.3,3'Dichlorobenzidine GC/MS 6410B2000.
1625B
HPLC 605.
39.Dichlorodifluoromethane GC 601.
GC/MS 6200C1997.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
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45.1,2Dichloropropane GC 601 6200C1997.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
48.Diethylphthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
50.Dimethylphthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
51.Dinbutylphthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
52.Dinoctylphthalate GC 606.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
Seefootnote9,
53.2,4Dinitrophenol GC 604 6420B2000
p.27.
625,
GC/MS 6410B2000.
1625B
54.2,4Dinitrotoluene GC 609.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
55.2,6Dinitrotoluene GC 609.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
Seefootnote3,
56.Epichlorohydrin GC
p.130.
Seefootnote6,
GC/MS
p.S102.
624,
GC/MS 6200B1997.
1624B
58.Fluoranthene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
59.Fluorene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
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1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
60.1,2,3,4,6,7,8Heptachloro
GC/MS 1613B.
dibenzofuran
61.1,2,3,4,7,8,9Heptachloro
GC/MS 1613B.
dibenzofuran
62.1,2,3,4,6,7,8Heptachloro
GC/MS 1613B.
dibenzopdioxin
63.Hexachlorobenzene GC 612.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
64.Hexachlorobutadiene GC 612.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
65.Hexachlorocyclopentadiene GC 612.
6255, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
66.1,2,3,4,7,8Hexachloro
GC/MS 1613B.
dibenzofuran
67.1,2,3,6,7,8Hexachloro
GC/MS 1613B.
dibenzofuran
68.1,2,3,7,8,9Hexachloro
GC/MS 1613B.
dibenzofuran
69.2,3,4,6,7,8Hexachloro
GC/MS 1613B.
dibenzofuran
70.1,2,3,4,7,8Hexachlorodibenzop
GC/MS 1613B.
dioxin
71.1,2,3,6,7,8Hexachlorodibenzop
GC/MS 1613B.
dioxin
72.1,2,3,7,8,9Hexachlorodibenzop
GC/MS 1613B.
dioxin
73.Hexachloroethane GC 612.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
74.Indeno(1,2,3c,d)pyrene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
75.Isophorone GC 609.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
Seefootnote3,
76.Methylenechloride GC 601 6200C1997.
p.130.
624,
GC/MS 6200B1997.
1624B
625, Seefootnote9,
GC/MS 6410B2000.
1625B p.27.
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78.Naphthalene GC 610.
625, Seefootnote9,
GC/MS 6410B2000.
1625B p.27
79.Nitrobenzene GC 609.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 92
(98).
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
82.NNitrosodimethylamine GC 607.
6255, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
83.NNitrosodinpropylamine GC 607.
6255, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
84.NNitrosodiphenylamine GC 607.
6255, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
87.2,2'Oxybis(2chloropropane)[also
GC 611.
knownasbis(2Chloroisopropyl)ether]
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
Seefootnote3,
88.PCB1016 GC 608 p.43See
footnote.8
Seefootnote3,
89.PCB1221 GC 608 p.43See
footnote.8
Seefootnote3,
90.PCB1232 GC 608 p.43See
footnote.8
Seefootnote3,
91.PCB1242 GC 608 p.43See
footnote.8
92.PCB1248 GC 608.
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Seefootnote3,
93.PCB1254 GC 608 p.43See
footnote.8
Seefootnote3,
94.PCB1260 GC 608 p.43See
footnote.8
95.1,2,3,7,8Pentachloro
GC/MS 1613B.
dibenzofuran
96.2,3,4,7,8Pentachloro
GC/MS 1613B.
dibenzofuran
97.1,2,3,7,8,Pentachlorodibenzop
GC/MS 1613B.
dioxin
Seefootnote3,
98.Pentachlorophenol GC 604 6420B2000
p.140.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
99.Phenanthrene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
101.Pyrene GC 610.
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
D4657
HPLC 610 6440B2000 92
(98).
613,625
103.2,3,7,8Tetrachlorodibenzop
GC/MS 5a,
dioxin
1613B
Seefootnote3,
104.1,1,2,2Tetrachloroethane GC 601 6200C1997
p.130.
624,
GC/MS 6200B1997.
1624B
Seefootnote3,
105.Tetrachloroethene GC 601 6200C1997
p.130.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
Seefootnote3,
107.1,2,4Trichlorobenzene GC 612
p.130.
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624,
GC/MS 6200B1997.
1624B
Seefootnote3,
109.1,1,2Trichloroethane GC 601 6200C1997.
p.130.
624,
GC/MS 6200B1997.
1624B
624,
GC/MS 6200B1997.
1624B
625, Seefootnote9,
GC/MS 6410B2000
1625B p.27.
624,
GC/MS 6200B1997.
1624B
D7065
114.Nonylphenol GC/MS
06.
D7065
115.BisphenolA(BPA) GC/MS
06.
D7065
116.ptertOctylphenol(OP) GC/MS
06.
117.NonylphenolMonoethoxylate D7065
GC/MS
(NP1EO) 06.
118.NonylphenolDiethoxylate D7065
GC/MS
(NP2EO) 06.
Adsorptionand
119.AdsorbableOrganicHalides
Coulometric 1650.11
(AOX)
Titration
InSituAcetylation
120.ChlorinatedPhenolics 1653.11
andGC/MS
TableICnotes:
1Allparametersareexpressedinmicrogramsperliter(g/L)exceptforMethod1613B,inwhichtheparametersare
expressedinpicogramsperliter(pg/L).
2ThefulltextofMethods601613,624,625,1613B,1624B,and1625BareprovidedatAppendixA,TestProceduresfor
AnalysisofOrganicPollutants,ofthisPart136.Thestandardizedtestproceduretobeusedtodeterminethemethod
detectionlimit(MDL)forthesetestproceduresisgivenatAppendixB,DefinitionandProcedurefortheDeterminationofthe
MethodDetectionLimit,ofthisPart136.
3MethodsforBenzidine:ChlorinatedOrganicCompounds,PentachlorophenolandPesticidesinWaterandWastewater.
September1978.U.S.EPA.
4Method624maybeusedforquantitativedeterminationofacroleinandacrylonitrile,providedthatthelaboratoryhas
documentationtosubstantiatetheabilitytodetectandquantifytheseanalytesatlevelsnecessarytocomplywithany
associatedregulations.Inaddition,theuseofsampleintroductiontechniquesotherthansimplepurgeandtrapmaybe
required.QCacceptancecriteriafromMethod603shouldbeusedwhenanalyzingsamplesforacroleinandacrylonitrilein
theabsenceofsuchcriteriainMethod624.
5Method625maybeextendedtoincludebenzidine,hexachlorocyclopentadiene,Nnitrosodimethylamine,Nnitrosodin
propylamine,andNnitrosodiphenylamine.However,whentheyareknowntobepresent,Methods605,607,and612,or
Method1625B,arepreferredmethodsforthesecompounds.
5aMethod625,screeningonly.
6SelectedAnalyticalMethodsApprovedandCitedbytheUnitedStatesEnvironmentalProtectionAgency,Supplementto
the15thEditionof StandardMethodsfortheExaminationofWaterandWastewater. 1981.AmericanPublicHealth
Association(APHA).
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7Eachanalystmustmakeaninitial,onetimedemonstrationoftheirabilitytogenerateacceptableprecisionandaccuracy
withMethods601603,624,625,1624B,and1625BinaccordancewithprocedureseachinSection8.2ofeachofthese
Methods.Additionally,eachlaboratory,onanongoingbasismustspikeandanalyze10%(5%forMethods624and625and
100%formethods1624Band1625B)ofallsamplestomonitorandevaluatelaboratorydataqualityinaccordancewith
Sections8.3and8.4ofthesemethods.Whentherecoveryofanyparameterfallsoutsidethewarninglimits,theanalytical
resultsforthatparameterintheunspikedsamplearesuspect.Theresultsshouldbereported,butcannotbeusedto
demonstrateregulatorycompliance.ThesequalitycontrolrequirementsalsoapplytotheStandardMethods,ASTM
Methods,andothermethodscited.
8OrganochlorinePesticidesandPCBsinWastewaterUsingEmporeTMDisk.RevisedOctober28,1994.3MCorporation.
9MethodO311687isinOpenFileReport93125,MethodsofAnalysisbyU.S.GeologicalSurveyNationalWaterQuality
LaboratoryDeterminationofInorganicandOrganicConstituentsinWaterandFluvialSediments.1993.USGS.
10AnalystsmayuseFluidManagementSystems,Inc.PowerPrepsysteminplaceofmanualcleanupprovidedtheanalyst
meetstherequirementsofMethod1613B(asspecifiedinSection9ofthemethod)andpermittingauthorities.Method1613,
RevisionB,TetrathroughOctaChlorinatedDioxinsandFuransbyIsotopeDilutionHRGC/HRMS.RevisionB,1994.U.S.
EPA.ThefulltextofthismethodisprovidedinAppendixAto40CFRPart136andat
http://water.epa.gov/scitech/methods/cwa/index.cfm
11Method1650,AdsorbableOrganicHalidesbyAdsorptionandCoulometricTitration.RevisionC,1997.U.S.EPA.Method
1653,ChlorinatedPhenolicsinWastewaterbyInSituAcetylationandGCMS.RevisionA,1997.U.S.EPA.Thefulltextfor
bothofthesemethodsisprovidedatappendixAinpart430,ThePulp,Paper,andPaperboardPointSourceCategory.
TableIDListofApprovedTestProceduresforPesticides1
Parameter Method EPA2710 Standardmethods ASTM Other
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
1.Aldrin GC 608,617 D581296
2000 310483Seefootnote8,3M0222.
(02)
Seefootnote3,p.83Seefootnote9,O
2.Ametryn GC 507,619
310693Seefootnote6,p.S68.
Seefootnote3,p.94Seefootnote6,p.
3.Aminocarb TLC
S60.
HPLC 632.
Seefootnote3,p.83Seefootnote6,p.
4.Atraton GC 619
S68.
Seefootnote3,p.83Seefootnote6,p.
5.Atrazine GC 507,619
S68Seefootnote9,O310693.
HPLC/MS Seefootnote12,O206001.
GCMS Seefootnote11,O112695.
Seefootnote3,p.104Seefootnote6,
7.Barban TLC
p.S64.
HPLC 632.
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote8,
8.BHC GC 608,617 D5812
2000 3M0222.
96(02)
D308690,
6630B2000&C
9.BHC GC 608,617 D5812 Seefootnote8,3M0222.
2000
96(02)
D308690,
6630B2000&C
10.BHC GC 608,617 D5812 Seefootnote8,3M0222.
2000
96(02)
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GC/MS 625 6410B2000.
D308690,
11.BHC 6630B2000&C Seefootnote3,p.7Seefootnote4,O
GC 608,617 D5812
(Lindane) 2000 310483Seefootnote8,3M0222.
96(02)
D308690,
12.Captan GC 617 6630B2000 D5812 Seefootnote3,p.7.
96(02)
Seefootnote3,p.94,Seefootnote6,p.
13.Carbaryl TLC
S60.
HPLC 531.1,632.
GC/MS Seefootnote11,O112695.
14.Carbo Seefootnote4,page27Seefootnote6,
GC 617 6630B2000
phenothion p.S73.
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
15.Chlordane GC 608,617 D5812
2000 310483Seefootnote8,3M0222.
96(02)
16. Seefootnote3,p.104Seefootnote6,
TLC
Chloropropham p.S64.
HPLC 632.
Seefootnote3,p.115Seefootnote4,
17.2,4D GC 615 6640B2001
O310583.
HPLC/MS Seefootnote12,O206001.
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
18.4,4'DDD GC 608,617 D5812
2000 310583Seefootnote8,3M0222.
96(02)
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
19.4,4'DDE GC 608,617 D5812
2000 310483Seefootnote8,3M0222.
96(02)
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
20.4,4'DDT GC 608,617 D5812
2000 310483Seefootnote8,3M0222.
96(02)
Seefootnote3,p.25Seefootnote6,p.
21.DemetonO GC 614,622
S51.
Seefootnote3,p.25Seefootnote6,p.
22.DemetonS GC 614,622
S51.
507,614, Seefootnote3,p.25Seefootnote4,O
23.Diazinon GC
622,1657 310483Seefootnote6,p.S51.
HPLC/MS Seefootnote12,O206001.
25. Seefootnote4,page27Seefootnote6,
GC 622.1
Dichlofenthion p.S73.
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D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
28.Dieldrin GC 608,617 D5812
2000 310483Seefootnote8,3M0222.
96(02)
Seefootnote4,page27Seefootnote6,
29.Dioxathion GC 614.1,1657
p.S73.
507,614, Seefootnote3,p.25Seefootnote6p.
30.Disulfoton GC
622,1657 S51.
Seefootnote3,p.104Seefootnote6,
31.Diuron TLC
p.S64.
HPLC 632.
D308690,
32.Endosulfan 6630B2000&C Seefootnote3,p.7Seefootnote4,O
GC 608,617 D5812
I 2000 310483Seefootnote8,3M022).
96(02)
D308690,
33.Endosulfan 6630B2000&C Seefootnote3,p.7Seefootnote8,
GC 608,617 D5812
II 2000 3M0222.
96(02)
34.Endosulfan
GC 608,617 6630C2000 Seefootnote8,3M0222.
Sulfate
505,508, D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
35.Endrin GC 608,617, D5812
2000 310483Seefootnote8,3M0222.
1656 96(02)
525.1,525.2,
GC/MS 6410B2000.
6255
36.Endrin
GC 608,617 6630C2000 Seefootnote8,3M0222.
aldehyde
GC/MS 625.
614, Seefootnote4,page27Seefootnote6,
37.Ethion GC
614.1,1657 p.S73.
GC/MS Seefootnote13,O200201.
Seefootnote3,p.104Seefootnote6,
38.Fenuron TLC
p.S64.
HPLC 632.
HPLC/MS Seefootnote12,O206001.
39.Fenuron Seefootnote3,p.104Seefootnote6,
TLC
TCA p.S64.
HPLC 632.
505,508, D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
40.Heptachlor GC 608,617, D5812
2000 310483Seefootnote8,3M0222.
1656 96(02)
525.1,525.2,
GC/MS 6410B2000.
625
D308690, Seefootnote3,p.7Seefootnote4,O
41.Heptachlor 6630B2000&C
GC 608,617 D5812 310483Seefootnote6,p.S73See
epoxide 2000
96(02) footnote8,3M0222.
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GC/MS 625 6410B2000.
6630B2000&C Seefootnote4,O310483Seefootnote
42.Isodrin GC 617
2000 6,p.S73.
Seefootnote3,p.104Seefootnote6,
43.Linuron GC
p.S64.
HPLC 632.
GC/MS Seefootnote11,O112695.
Seefootnote3,p.25Seefootnote6,p.
44.Malathion GC 614,1657 6630B2000
S51.
GC/MS Seefootnote11,O112695.
Seefootnote3,p.94Seefootnote6,p.
45.Methiocarb TLC
S60.
HPLC 632.
HPLC/MS Seefootnote12,O206001.
505,508, D308690,
46. 6630B2000&C Seefootnote3,p.7Seefootnote4,O
GC 608.2,617, D5812
Methoxychlor 2000 310483Seefootnote8,3M0222.
1656 96(02)
47. Seefootnote3,p.94Seefootnote6,
TLC
Mexacarbate p.S60.
HPLC 632.
D308690,
6630B2000&C Seefootnote3,p.7Seefootnote4,O
48.Mirex GC 617 D5812
2000 310483.
96(02)
Seefootnote3,p.104Seefootnote6,
49.Monuron TLC
p.S64.
HPLC 632.
50.Monuron Seefootnote3,p.104Seefootnote6,
TLC
TCA p.S64.
HPLC 632.
Seefootnote3,p.104Seefootnote6,
51.Neburon TLC
p.S64.
HPLC 632.
HPLC/MS Seefootnote12,O206001.
GC/MS Seefootnote11,O112695.
53.Parathion Seefootnote4,page27Seefootnote3,
GC 614 6630B2000
ethyl p.25.
GC/MS Seefootnote11,O112695.
D308690 ,
6630B2000&C
54.PCNB GC 608.1,617 D5812 Seefootnote3,p.7.
2000
96(02)
D308690,
55.Perthane GC 617 D5812 Seefootnote4,O310483.
96(02)
Seefootnote3,p.83Seefootnote6,p.
56.Prometon GC 507,619
S68Seefootnote9,O310693.
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GC/MS 525.2 Seefootnote11,O112695.
Seefootnote3,p.83Seefootnote6,p.
57.Prometryn GC 507,619
S68Seefootnote9,O310693.
507,619, Seefootnote3,p.83Seefootnote6,p.
58.Propazine GC
1656 S68Seefootnote9,O310693.
GC/MS 525.1,525.2.
Seefootnote3,p.104Seefootnote6,
59.Propham TLC
p.S64.
HPLC 632.
HPLC/MS Seefootnote12,O206001.
Seefootnote3,p.94Seefootnote6,p.
60.Propoxur TLC
S60.
HPLC 632.
61. Seefootnote3,p.83Seefootnote6,p.
TLC
Secbumeton S68.
GC 619.
Seefootnote3,p.104Seefootnote6,
62.Siduron TLC
p.S64.
HPLC 632.
HPLC/MS Seefootnote12,O206001.
505,507, Seefootnote3,p.83Seefootnote6,p.
63.Simazine GC
619,1656 S68Seefootnote9,O310693.
6630B2000&C
64.Strobane GC 617 Seefootnote3,p.7.
2000
Seefootnote3,p.104Seefootnote6,
65.Swep TLC
p.S64.
HPLC 632.
Seefootnote3,p.115Seefootnote4,
66.2,4,5T GC 615 6640B2001
O310583.
67.2,4,5TP Seefootnote3,p.115Seefootnote4,
GC 615 6640B2001
(Silvex) O310583.
68. Seefootnote3,p.83Seefootnote6,p.
GC 619,1656
Terbuthylazine S68.
GC/MS Seefootnote13,O200201.
505,508, D308690,
6630B2000&C Seefootnote3,p.7Seefootnote8See
69.Toxaphene GC 608,617, D5812
2000 footnote4,O310583.
1656 96(02)
525.1,525.2,
GC/MS 6410B2000.
625
508,617, Seefootnote3,p.7Seefootnote9,O
70.Trifluralin GC 6630B2000
627,1656 310693.
TableIDnotes:
1Pesticidesarelistedinthistablebycommonnamefortheconvenienceofthereader.Additionalpesticidesmaybefound
underTableIC,whereentriesarelistedbychemicalname.
2Thestandardizedtestproceduretobeusedtodeterminethemethoddetectionlimit(MDL)forthesetestproceduresis
givenatAppendixB,DefinitionandProcedurefortheDeterminationoftheMethodDetectionLimit,ofthisPart136.
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3MethodsforBenzidine,ChlorinatedOrganicCompounds,PentachlorophenolandPesticidesinWaterandWastewater.
September1978.U.S.EPA.ThisEPApublicationincludesthinlayerchromatography(TLC)methods.
4MethodsfortheDeterminationofOrganicSubstancesinWaterandFluvialSediments,TechniquesofWaterResources
InvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA3.1987.USGS.
5ThemethodmaybeextendedtoincludeBHC,BHC,endosulfanI,endosulfanII,andendrin.However,whentheyare
knowntoexist,Method608isthepreferredmethod.
6SelectedAnalyticalMethodsApprovedandCitedbytheUnitedStatesEnvironmentalProtectionAgency,Supplementto
the15thEditionof StandardMethodsfortheExaminationofWaterandWastewater. 1981.AmericanPublicHealth
Association(APHA).
7Eachanalystmustmakeaninitial,onetime,demonstrationoftheirabilitytogenerateacceptableprecisionandaccuracy
withMethods608and625inaccordancewithproceduresgiveninSection8.2ofeachofthesemethods.Additionally,each
laboratory,onanongoingbasis,mustspikeandanalyze10%ofallsamplesanalyzedwithMethod608or5%ofallsamples
analyzedwithMethod625tomonitorandevaluatelaboratorydataqualityinaccordancewithSections8.3and8.4ofthese
methods.Whentherecoveryofanyparameterfallsoutsidethewarninglimits,theanalyticalresultsforthatparameterinthe
unspikedsamplearesuspect.Theresultsshouldbereported,butcannotbeusedtodemonstrateregulatorycompliance.
ThesequalitycontrolrequirementsalsoapplytotheStandardMethods,ASTMMethods,andothermethodscited.
8OrganochlorinePesticidesandPCBsinWastewaterUsingEmporeTMDisk.RevisedOctober28,1994.3MCorporation.
9MethodO310693isinOpenFileReport9437,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWater
QualityLaboratoryDeterminationofTriazineandOtherNitrogenContainingCompoundsbyGasChromatographyWith
NitrogenPhosphorusDetectors.1994.USGS.
10EPAMethods608.1,608.2,614,614.1,615,617,619,622,622.1,627,and632arefoundinMethodsforthe
DeterminationofNonconventionalPesticidesinMunicipalandIndustrialWastewater,EPA821R92002,April1992,U.S.
EPA.ThefulltextofMethods608and625areprovidedatAppendixA,TestProceduresforAnalysisofOrganicPollutants,
ofthisPart136.EPAMethods505,507,508,525.1,531.1and553areinMethodsfortheDeterminationof
NonconventionalPesticidesinMunicipalandIndustrialWastewater,VolumeII,EPA821R93010B,1993,U.S.EPA.EPA
Method525.2isinDeterminationofOrganicCompoundsinDrinkingWaterbyLiquidSolidExtractionandCapillaryColumn
GasChromatography/MassSpectrometry,Revision2.0,1995,U.S.EPA.EPAmethods1656and1657areinMethodsFor
TheDeterminationofNonconventionalPesticidesInMunicipalandIndustrialWastewater,VolumeI,EPA821R93010A,
1993,U.S.EPA.
11MethodO112695isinOpenFileReport95181,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWater
QualityLaboratoryDeterminationofpesticidesinwaterbyC18solidphaseextractionandcapillarycolumngas
chromatography/massspectrometrywithselectedionmonitoring.1995.USGS.
12MethodO206001isinWaterResourcesInvestigationsReport014134,MethodsofAnalysisbytheU.S.Geological
SurveyNationalWaterQualityLaboratoryDeterminationofPesticidesinWaterbyGraphitizedCarbonBasedSolidPhase
ExtractionandHighPerformanceLiquidChromatography/MassSpectrometry.2001.USGS.
13MethodO200201isinWaterResourcesInvestigationsReport014098,MethodsofAnalysisbytheU.S.Geological
SurveyNationalWaterQualityLaboratoryDeterminationofmoderateusepesticidesinwaterbyC18solidphase
extractionandcapillarycolumngaschromatography/massspectrometry.2001.USGS.
14MethodO112191isinOpenFileReport91519,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWater
QualityLaboratoryDeterminationoforganonitrogenherbicidesinwaterbysolidphaseextractionandcapillarycolumngas
chromatography/massspectrometrywithselectedionmonitoring.1992.USGS.
TableIEListofApprovedRadiologicTestTestProcedures
Standard
Methods Standard
EPA USGS
Reference(methodnumberorpage) 18th, Methods ASTM
1 2
19th, Online
Parameter 20thEd.
Method
andunits
pp.
1.Alpha Proportional
75
Total, or 7110
900.0 7110B D194390,96 and
pCiper scintillation B00
78
liter counter
3
2.Alpha Proportional
Counting or Appendix 7110 D1943
7110B p.79
error,pCi scintillation B B00 90,96
perliter counter
pp.
3.Beta
Proportional 7110 D1890 75
Total,pCi 900.0 7110B
counter B00 90,96 and
perliter
783
4.Beta
Proportional Appendix 7110 D1890
Counting 7110B p.79
counter B B00 90,96
error,pCi
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5.(a)
Radium 7500
TotalpCi Proportional D2460
903.0 7500RaB RaB
perliter(b) counter 90,97
01
Ra,pCiper
liter
7500
Scintillation D3454
903.1 7500RaC Ra p.81
counter 91,97
C01
1PrescribedProceduresforMeasurementofRadioactivityinDrinkingWater,
EPA600/480032(1980),U.S.EnvironmentalProtectionAgency,August
1980.
2Fishman,M.J.andBrown,Eugene,SelectedMethodsoftheU.S.
GeologicalSurveyofAnalysisofWastewaters,U.S.GeologicalSurvey,
OpenFileReport76177(1976).
3Themethodfoundonp.75measuresonlythedissolvedportionwhilethe
methodonp.78measuresonlythesuspendedportion.Therefore,thetwo
resultsmustbeaddedtoobtainthetotal.
TableIFListofApprovedMethodsforPharmaceuticalPollutants
Pharmaceuticalspollutants CASregistryNo. Analyticalmethodnumber
acetonitrile 75058 1666/1671/D3371/D3695.
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2propanone(acetone) 67641 D3695/D4763/524.2.
Table1Fnote:
1.1624C:mxylene108383,o,pxyleneE14095(NotaCASnumberthisisthenumberprovidedintheEnvironmental
MonitoringMethodsIndex(EMMI)database.)1666:m,pxylene136777612,oxylene95476.
TableIGTestMethodsforPesticideActiveIngredients(40CFRPart455)
EPAsurvey CAS
Pesticidename EPAanalyticalmethodNo.(s)3
code No.
43121
8 Triadimefon 507/633/525.1/525.2/1656
433
2,4D2,4DSaltsandEsters[2,4Dichloro
16 94757 1658/515.1/615/515.2/555
phenoxyaceticacid]
2,4DB2,4DBSaltsandEsters[2,4
17 94826 1658/515.1/615/515.2/555
Dichlorophenoxybutyricacid]
7786
22 Mevinphos 1657/507/622/525.1/525.2
347
21725
25 Cyanazine 629/507
462
1918
26 Propachlor 1656/508/608.1/525.1/525.2
167
MCPAMCPASaltsandEsters[2Methyl4
27 94746 1658/615/555
chlorophenoxyaceticacid]
DichlorpropDichlorpropSaltsandEsters[2(2,4 12036
30 1658/515.1/615/515.2/555
Dichlorophenoxy)propionicacid] 5
MCPPMCPPSaltsandEsters[2(2Methyl4
31 93652 1658/615/555
chlorophenoxy)propionicacid]
21564
35 TCMTB[2(Thiocyanomethylthio)benzothiazole] 637
170
23950
39 Pronamide 525.1/525.2/507/633.1
585
70998
41 Propanil 632.1/1656
8
21087
45 Metribuzin 507/633/525.1/525.2/1656
649
30560
52 Acephate 1656/1657
191
50594
53 Acifluorfen 515.1/515.2/555
666
15972
54 Alachlor 505/507/645/525.1/525.2/1656
608
11606
55 Aldicarb 531.1
3
83412
58 Ametryn 507/619/525.2
8
1912
60 Atrazine 505/507/619/525.1/525.2/1656
249
17804
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62 Benomyl 352 631
31440
68 BromacilBromacilSaltsandEsters 507/633/525.1/525.2/1656
9
1689
69 Bromoxynil 1625/1661
845
1689
69 Bromoxyniloctanoate 1656
992
23184
70 Butachlor 507/645/525.1/525.2/1656
669
2425
73 Captafol 1656
061
1563
76 Carbofuran 531.1/632
662
2675
80 Chloroneb 1656/508/608.1/525.1/525.2
776
1897
82 Chlorothalonil 508/608.2/525.1/525.2/1656
456
96111
84 Stirofos 1657/507/622/525.1/525.2
5
2921
86 Chlorpyrifos 1657/508/622
882
51630
90 Fenvalerate 1660
581
33341
103 Diazinon 1657/507/614/622/525.2
5
29800
107 Parathionmethyl 1657/614/622
0
1861 508/608.2/525.1/525.2/515.12/515.2
110 DCPA[Dimethyl2,3,5,6tetrachloroterephthalate]
321 2/1656
13893
118 Nabonate[Disodiumcyanodithioimidocarbonate] 630.1
2
33054
119 Diuron 632/553
1
14573
123 Endothall 548/548.1
3
55283
125 Ethalfluralin 1656/627Seefootnote1
686
56312
126 Ethion 1657/614/614.1
2
13194
127 Ethoprop 1657/507/622/525.1/525.2
484
60168
132 Fenarimol 507/633.1/525.1/525.2/1656
889
1071
138 Glyphosate[N(Phosphonomethyl)glycine] 547
836
33820
144 Isopropalin 1656/627
530
33055
148 Linuron 553/632
2
12175
150 Malathion 1657/614
5
10265
154 Methamidophos 1657
926
16752
156 Methomyl 531.1/632
775
14259
172 Nabam 630/630.1
6
30076
173 Naled 1657/622
5
27314
175 Norflurazon 507/645/525.1/525.2/1656
132
1861
178 Benfluralin 1656/627Seefootnote1
401
11590
182 Fensulfothion 1657/622
2
29804
183 Disulfoton 1657/507/614/622/525.2
4
73211
185 Phosmet 1657/622.1
6
12379
192 Organotinpesticides Ind01/200.7/200.9
543
35400
197 Bolstar 1657/622
432
40487
204 Pendimethalin 1656
421
52645
208 Permethrin 608.2/508/525.1/525.2/1656/1660
531
29802
212 Phorate 1657/622
2
12803
218 Busan85[Potassiumdimethyldithiocarbamate] 630/630.1
0
Busan40[PotassiumNhydroxymethylN 51026
219 630/630.1
methyldithiocarbamate] 289
13741
220 KNMethyl[PotassiumNmethyldithiocarbamate] 630/630.1
7
1610
223 Prometon 507/619/525.2
180
7287
224 Prometryn 507/619/525.1/525.2
196
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230 PyrethrinI 12121 1660
1
12129
232 PyrethrinII 1660
9
12234
239 Simazine 505/507/619/525.1/525.2/1656
9
12804
241 CarbamS[Sodiumdimethyldithiocarbamate] 630/630.1
1
13742
243 Vapam[Sodiummethyldithiocarbamate] 630/630.1
8
34014
252 Tebuthiuron 507/525.1/525.2
181
5902
254 Terbacil 507/633/525.1/525.2/1656
512
13071
255 Terbufos 1657/507/614.1/525.1/525.2
799
5915
256 Terbuthylazine 619/1656
413
88650
257 Terbutryn 507/619/525.1/525.2
0
53374
259 Dazomet 630/630.1/1659
4
8001
262 Toxaphene 1656/505/508/608/617/525.1/525.2
352
15050
263 Merphos[Tributylphosphorotrithioate] 1657/507/525.1/525.2/622
5
1582
264 Trifluralin1 1656/508/617/627/525.2
098
13730
268 Ziram[Zincdimethyldithiocarbamate] 630/630.1
4
Table1Gnotes:
1MonitorandreportastotalTrifluralin.
2ApplicabletotheanalysisofDCPAdegradates.
3EPAMethods608.1through645,1645through1661,andInd01areavailableinMethodsForTheDeterminationof
NonconventionalPesticidesInMunicipalandIndustrialWastewater,VolumeI,EPA821R93010A,RevisionI,August
1993,U.S.EPA.EPAMethods200.9and505through555areavailableinMethodsForTheDeterminationof
NonconventionalPesticidesInMunicipalandIndustrialWastewater,VolumeII,EPA821R93010B,August1993,U.S.
EPA.ThefulltextofMethods608,625and1625areprovidedatAppendixAofthisPart136.ThefulltextofMethod200.7
isprovidedatappendixCofthispart136.
TableIHListofApprovedMicrobiologicalMethodsforAmbientWater
AOAC,
Standard
Parameterandunits Method1 EPA ASTM, Other
methods
USGS
Bacteria:
1.Coliform(fecal),numberper MostProbableNumber
p.132
100mLornumberpergramdry (MPN),5tube,3 9221CE2006.
3
weight dilution,or
p.124
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MF2,singlestep5 3 9222D1997.
p.111 9222
MF2withenrichment
3 (B+B.5c)1997.
9221B.1
MPN6814,multiple
5. E.coli, numberper100mL 2006/9221F2006
tube,or
1113
Colilert1216,
Multipletube/multiple
9223B200412 991.1510 Colilert1812
well,or
1516.
9222B1997/9222
MF25678,twostep, 1103.1 D539293
G199718,9213D
or 19 9.
2007
1603
20, mColiBlue
Singlestep
1604 2417.
21
p.136 B005585
MF2,or 9230C2007
3 4.
p.143
Platecount
3
1600
Singlestep,or 9230C2007.
24
p.143
Platecount
3.
Protozoa:
1622
25,
8. Cryptosporidium Filtration/IMS/FA
1623
26
1623
9. Giardia Filtration/IMS/FA
26
Table1Hnotes:
1Themethodmustbespecifiedwhenresultsarereported.
2A0.45mmembranefilter(MF)orotherporesizecertifiedbythemanufacturertofullyretainorganismstobecultivated
andtobefreeofextractableswhichcouldinterferewiththeirgrowth.
3MicrobiologicalMethodsforMonitoringtheEnvironment,Water,andWastes.EPA/600/878/017.1978.USEPA.
4U.S.GeologicalSurveyTechniquesofWaterResourceInvestigations,Book5,LaboratoryAnalysis,ChapterA4,Methods
forCollectionandAnalysisofAquaticBiologicalandMicrobiologicalSamples.1989.USGS.
5BecausetheMFtechniqueusuallyyieldslowandvariablerecoveryfromchlorinatedwastewaters,theMostProbable
Numbermethodwillberequiredtoresolveanycontroversies.
6Testsmustbeconductedtoprovideorganismenumeration(density).Selecttheappropriateconfigurationof
tubes/filtrationsanddilutions/volumestoaccountforthequality,character,consistency,andanticipatedorganismdensityof
thewatersample.
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7WhentheMFmethodhasnotbeenusedpreviouslytotestwaterswithhighturbidity,largenumbersofnoncoliform
bacteria,orsamplesthatmaycontainorganismsstressedbychlorine,aparalleltestshouldbeconductedwithamultiple
tubetechniquetodemonstrateapplicabilityandcomparabilityofresults.
8Toassessthecomparabilityofresultsobtainedwithindividualmethods,itissuggestedthatsidebysidetestsbeconducted
acrossseasonsoftheyearwiththewatersamplesroutinelytestedinaccordancewiththemostcurrentStandardMethods
fortheExaminationofWaterandWastewaterorEPAalternatetestprocedure(ATP)guidelines.
9AnnualBookofASTMStandardsWaterandEnvironmentalTechnology.Section11.02.2000,1999,1996.ASTM
International.
10OfficialMethodsofAnalysisofAOACInternational,16thEdition,VolumeI,Chapter17.1995.AOACInternational.
11Themultipletubefermentationtestisusedin9221B.12006.Lactosebrothmaybeusedinlieuoflauryltryptosebroth
(LTB),ifatleast25paralleltestsareconductedbetweenthisbrothandLTBusingthewatersamplesnormallytested,and
thiscomparisondemonstratesthatthefalsepositiverateandfalsenegativeratefortotalcoliformusinglactosebrothisless
than10percent.Norequirementexiststorunthecompletedphaseon10percentofalltotalcoliformpositivetubesona
seasonalbasis.
12Thesetestsarecollectivelyknownasdefinedenzymesubstratetests,where,forexample,asubstrateisusedtodetect
theenzymeglucuronidaseproducedby E.coli.
13Afterpriorenrichmentinapresumptivemediumfortotalcoliformusing9221B.12006,allpresumptivetubesorbottles
showinganyamountofgas,growthoraciditywithin48h3hofincubationshallbesubmittedto9221F2006.Commercially
availableECMUGmediaorECmediasupplementedinthelaboratorywith50g/mLofMUGmaybeused.
14Samplesshallbeenumeratedbythemultipletubeormultiplewellprocedure.Usingmultipletubeprocedures,employan
appropriatetubeanddilutionconfigurationofthesampleasneededandreporttheMostProbableNumber(MPN).Samples
testedwithColilertmaybeenumeratedwiththemultiplewellprocedures,QuantiTrayorQuantiTray/2000,andthe
MPNcalculatedfromthetableprovidedbythemanufacturer.
15Colilert18isanoptimizedformulationoftheColilertforthedeterminationoftotalcoliformsand E.coli thatprovides
resultswithin18hofincubationat35C,ratherthanthe24hrequiredfortheColilerttest,andisrecommendedfor
marinewatersamples.
16DescriptionsoftheColilert,Colilert18,QuantiTray,andQuantiTray/2000maybeobtainedfromIDEXX
LaboratoriesInc.
17AdescriptionofthemColiBlue24testmaybeobtainedfromHachCompany.
18Subjecttotalcoliformpositivesamplesdeterminedby9222B1997orothermembranefilterprocedureto9222G1997
usingNAMUGmedia.
19Method1103.1: Escherichiacoli ( E.coli )inWaterbyMembraneFiltrationUsingmembraneThermotolerant
Escherichiacoli Agar(mTEC),EPA821R10002.March2010.USEPA.
20Method1603: Escherichiacoli ( E.coli )inWaterbyMembraneFiltrationUsingModifiedmembraneThermotolerant
Escherichiacoli Agar(ModifiedmTEC),EPA821R09007.December2009.USEPA.
21PreparationanduseofMIagarwithastandardmembranefilterprocedureissetforthinthearticle,Brenneretal.1993.
NewMediumfortheSimultaneousDetectionofTotalColiformand Escherichiacoli inWater.Appl.Environ.Microbiol.
59:35343544andinMethod1604:TotalColiformsand Escherichiacoli ( E.coli )inWaterbyMembraneFiltrationbyUsing
aSimultaneousDetectionTechnique(MIMedium),EPA821R02024,September2002,USEPA.
22AdescriptionoftheEnterolerttestmaybeobtainedfromIDEXXLaboratoriesInc.
23Method1106.1:EnterococciinWaterbyMembraneFiltrationUsingmembraneEnterococcusEsculinIronAgar(mE
EIA),EPA821R09015.December2009.USEPA.
24Method1600:EnterococciinWaterbyMembraneFiltrationUsingmembraneEnterococcusIndoxylDGlucosideAgar
(mEI),EPA821R09016.December2009.USEPA.
25Method1622usesafiltration,concentration,immunomagneticseparationofoocystsfromcapturedmaterial,
immunofluorescenceassaytodetermineconcentrations,andconfirmationthroughvitaldyestaininganddifferential
interferencecontrastmicroscopyforthedetectionof Cryptosporidium. Method1622: Cryptosporidium inWaterby
Filtration/IMS/FA,EPA821R05001.December2005.USEPA.
26Method1623usesafiltration,concentration,immunomagneticseparationofoocystsandcystsfromcapturedmaterial,
immunofluorescenceassaytodetermineconcentrations,andconfirmationthroughvitaldyestaininganddifferential
interferencecontrastmicroscopyforthesimultaneousdetectionof Cryptosporidium and Giardia oocystsandcysts.Method
1623. Cryptosporidium and Giardia inWaterbyFiltration/IMS/FA.EPA821R05002.December2005.USEPA.
(b)Thedocumentsrequiredinthissectionareincorporatedbyreferenceintothissectionwithapproval
oftheDirectoroftheFederalRegisterinaccordancewith5U.S.C.552(a)and1CFRpart51.Copiesof
thedocumentsmaybeobtainedfromthesourceslistedinparagraph(b)ofthissection.Documentsmay
beinspectedatEPA'sWaterDocket,EPAWest,1301ConstitutionAvenueNW.,RoomB102,
Washington,DC(Telephone:2025662426)orattheNationalArchivesandRecordsAdministration
(NARA).ForinformationontheavailabilityofthismaterialatNARA,call2027416030,orgoto:
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. Thesetest
proceduresareincorporatedastheyexistonthedayofapprovalandanoticeofanychangeinthese
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testprocedureswillbepublishedintheFederalRegister.Thefulltextsofthemethodsfromthe
followingreferenceswhicharecitedinTablesIA,IB,IC,ID,IE,IF,IGandIHareincorporatedby
referenceintothisregulationandmaybeobtainedfromthesourceidentified.Allcostscitedaresubject
tochangeandmustbeverifiedfromtheindicatedsource.
(1)EnvironmentalMonitoringandSupportLaboratory,U.S.EnvironmentalProtectionAgency,Cincinnati
OH(USEPA).Availableat http://water.epa.gov/scitech/methods/cwa/index.cfm orfrom:National
TechnicalInformationService,5285PortRoyalRoad,Springfield,Virginia22161
(i)MicrobiologicalMethodsforMonitoringtheEnvironment,Water,andWastes.1978.EPA/600/8
78/017,Pub.No.PB290329/A.S.
(A)PartIIIAnalyticalMethodology,SectionBTotalColiformMethods,page108.TableIA,Note3
TableIH,Note3.
(B)PartIIIAnalyticalMethodology,SectionBTotalColiformMethods,2.6.2TwoStepEnrichment
Procedure,page111.TableIA,Note3TableIH,Note3.
(C)PartIIIAnalyticalMethodology,SectionBTotalColiformMethods,4MostProbableNumber(MPN)
Method,page114.TableIA,Note3TableIH,Note3.
(D)PartIIIAnalyticalMethodology,SectionCFecalColiformMethods,2DirectMembraneFilter(MF)
Method,page124.TableIA,Note3TableIH,Note3.
(E)PartIII,AnalyticalMethodology,SectionCFecalColiformMethods,5MostProbableNumber(MPN)
Method,page132.TableIA,Note3TableIH,Note3.
(F)PartIIIAnalyticalMethodology,SectionDFecalStreptococci,2MembraneFilter(MF)Method,page
136.TableIA,Note3TableIH,Note3.
(G)PartIIIAnalyticalMethodology,SectionDFecalStreptococci,4MostProbableNumberMethod,
page139.TableIA,Note3TableIH,Note3.
(H)PartIIIAnalyticalMethodology,SectionDFecalStreptococci,5PourPlateMethod,page143.Table
IA,Note3TableIH,Note3.
(ii)[Reserved]
(2)EnvironmentalMonitoringandSupportLaboratory,U.S.EnvironmentalProtectionAgency,Cincinnati
OH(USEPA).Availableat http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i)Method300.1(includingErrataCoverSheet,April27,1999),DeterminationofInorganicIonsin
DrinkingWaterbyIonChromatography,Revision1.0,1997.TableIB,Note52.
(ii)Method551,DeterminationofChlorinationDisinfectionByproductsandChlorinatedSolventsin
DrinkingWaterbyLiquidLiquidExtractionandGasChromatographyWithElectronCaptureDetection.
1990.TableIF.
(3)NationalExposureRiskLaboratoryCincinnati,U.S.EnvironmentalProtectionAgency,CincinnatiOH
(USEPA).Availablefrom http://water.epa.gov/scitech/methods/cwa/index.cfm orfromtheNational
TechnicalInformationService(NTIS),5285PortRoyalRoad,Springfield,VA22161.Telephone:800
5536847.
(i)MethodsfortheDeterminationofInorganicSubstancesinEnvironmentalSamples.August1993.
EPA/600/R93/100,Pub.No.PB94120821.TableIB,Note52.
(A)Method180.1,DeterminationofTurbiditybyNephelometry.Revision2.0.TableIB,Note52.
(B)Method300.0,DeterminationofInorganicAnionsbyIonChromatography.Revision2.1.TableIB,
Note52.
(C)Method335.4,DeterminationofTotalCyanidebySemiAutomatedColorimetry.Revision1.0.Table
IB,Notes52and57.
(D)Method350.1,DeterminationofAmmoniumNitrogenbySemiAutomatedColorimetry.Revision2.0.
TableIB,Notes30and52.
(E)Method351.2,DeterminationofTotalKjeldahlNitrogenbySemiAutomatedColorimetry.Revision
2.0.TableIB,Note52.
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(F)Method353.2,DeterminationofNitrateNitriteAutomatedColorimetry.Revision2.0.TableIB,Note
52.
(G)Method365.1,DeterminationofPhosphorusbyAutomatedColorimetry.Revision2.0.TableIB,Note
52.
(H)Method375.2,DeterminationofSulfatebyAutomatedColorimetry.Revision2.0.TableIB,Note52.
(I)Method410.4,DeterminationofChemicalOxygenDemandbySemiAutomatedColorimetry.
Revision2.0.TableIB,Note52.
(ii)MethodsfortheDeterminationofMetalsinEnvironmentalSamples,SupplementI.May1994.
EPA/600/R94/111,Pub.No.PB95125472.TableIB,Note52.
(A)Method200.7,DeterminationofMetalsandTraceElementsinWaterandWastesbyInductively
CoupledPlasmaAtomicEmissionSpectrometry.Revision4.4.TableIB,Note52.
(B)Method200.8,DeterminationofTraceElementsinWaterandWastesbyInductivelyCoupled
PlasmaMassSpectrometry.Revision5.3.TableIB,Note52.
(C)Method200.9,DeterminationofTraceElementsbyStabilizedTemperatureGraphiteFurnaceAtomic
AbsorptionSpectrometry.Revision2.2.TableIB,Note52.
(D)Method218.6,DeterminationofDissolvedHexavalentChromiuminDrinkingWater,Groundwater,
andIndustrialWastewaterEffluentsbyIonChromatography.Revision3.3.TableIB,Note52.
(E)Method245.1,DeterminationofMercuryinWaterbyColdVaporAtomicAbsorptionSpectrometry.
Revision3.0.TableIB,Note52.
(4)NationalExposureRiskLaboratoryCincinnati,U.S.EnvironmentalProtectionAgency,CincinnatiOH
(USEPA).Availableat http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i)EPAMethod200.5,DeterminationofTraceElementsinDrinkingWaterbyAxiallyViewedInductively
CoupledPlasmaAtomicEmissionSpectrometry.Revision4.2,October2003.EPA/600/R06/115.Table
IB,Note68.
(ii)EPAMethod525.2,DeterminationofOrganicCompoundsinDrinkingWaterbyLiquidSolid
ExtractionandCapillaryColumnGasChromatography/MassSpectrometry.Revision2.0,1995.Table
ID,Note10.
(5)OfficeofResearchandDevelopment,CincinnatiOH.U.S.EnvironmentalProtectionAgency,
CincinnatiOH(USEPA).Availableat http://water.epa.gov/scitech/methods/cwa/index.cfm orfrom
ORDPublications,CERI,U.S.EnvironmentalProtectionAgency,CincinnatiOH45268.
(i)MethodsforBenzidine,ChlorinatedOrganicCompounds,Pentachlorophenol,andPesticidesinWater
andWastewater.1978.TableIC,Note3TableID,Note3.
(ii)MethodsforChemicalAnalysisofWaterandWastes.March1979.EPA600/479020.TableIB,
Note1.
(iii)MethodsforChemicalAnalysisofWaterandWastes.RevisedMarch1983.EPA600/479020.
TableIB,Note1.
(A)Method120.1,Conductance,SpecificConductance,mhosat25C.Revision1982.TableIB,Note
1.
(B)Method130.1,Hardness,Total(mg/LasCaCO3),Colorimetric,AutomatedEDTA.Issued1971.
TableIB,Note1.
(C)Method150.2,pH,ContinuousMonitoring(Electrometric).December1982.TableIB,Note1.
(D)Method160.4,Residue,Volatile,Gravimetric,Ignitionat550C.Issued1971.TableIB,Note1.
(E)Method206.5,Arsenic,SampleDigestionPriortoTotalArsenicAnalysisbySilver
DiethyldithiocarbamateorHydrideProcedures.Issued1978.TableIB,Note1.
(F)Method231.2,Gold,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(G)Method245.2,Mercury,AutomatedColdVaporTechnique.Issued1974.TableIB,Note1.
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(H)Method252.2,Osmium,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(I)Method253.2,Palladium,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(J)Method255.2,Platinum,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(K)Method265.2,Rhodium,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(L)Method279.2,Thallium,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(M)Method283.2,Titanium,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(N)Method289.2,Zinc,AtomicAbsorption,FurnaceTechnique.Issued1978.TableIB,Note1.
(O)Method310.2,Alkalinity,Colorimetric,Automated,MethylOrange.Revision1974.TableIB,Note1.
(P)Method351.1,Nitrogen,Kjeldahl,Total,Colorimetric,AutomatedPhenate.Revision1978.TableIB,
Note1.
(Q)Method352.1,Nitrogen,Nitrate,Colorimetric,Brucine.Issued1971.TableIB,Note1.
(R)Method365.3,Phosphorus,AllForms,Colorimetric,AscorbicAcid,TwoReagent.Issued1978.
TableIB,Note1.
(S)Method365.4,Phosphorus,Total,Colorimetric,Automated,BlockDigestorAAII.Issued1974.
TableIB,Note1.
(T)Method410.3,ChemicalOxygenDemand,Titrimetric,HighLevelforSalineWaters.Revision1978.
TableIB,Note1.
(U)Method420.1,Phenolics,TotalRecoverable,Spectrophotometric,Manual4AAPWithDistillation.
Revision1978.TableIB,Note1.
(iv)PrescribedProceduresforMeasurementofRadioactivityinDrinkingWater.1980.EPA600/480
032.TableIE.
(A)Method900.0,GrossAlphaandGrossBetaRadioactivity.TableIE.
(B)Method903.0,AlphaEmittingiRadioIsotopes.TableIE.
(C)Method903.1,Radium226,RadonEmanationTechnique.TableIE.
(D)AppendixB,ErrorandStatisticalCalculations.TableIE.
(6)OfficeofScienceandTechnology,U.S.EnvironmentalProtectionAgency,WashingtonDC(US
EPA).Availableat http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i)Method1625C,SemivolatileOrganicCompoundsbyIsotopeDilutionGCMS.1989.TableIF.
(ii)[Reserved]
(7)OfficeofWater,U.S.EnvironmentalProtectionAgency,WashingtonDC(USEPA).Availableat
http://water.epa.gov/scitech/methods/cwa/index.cfm orfromNationalTechnicalInformationService,
5285PortRoyalRoad,Springfield,Virginia22161.
(i)Method1631,MercuryinWaterbyOxidation,PurgeandTrap,andColdVaporAtomicFluorescence
Spectrometry.RevisionE,August2002.EPA821R02019,Pub.No.PB2002108220.TableIB,Note
43.
(ii)Kelada01,KeladaAutomatedTestMethodsforTotalCyanide,AcidDissociableCyanide,and
Thiocyanate.Revision1.2,August2001.EPA821B01009,Pub.No.PB2001108275.TableIB,Note
55.
(iii)Inthecompendium AnalyticalMethodsfortheDeterminationofPollutantsinPharmaceutical
ManufacturingIndustryWastewaters. July1998.EPA821B98016,Pub.No.PB95201679.TableIF,
Note1.
(A)EPAMethod1666,VolatileOrganicCompoundsSpecifictothePharmaceuticalIndustrybyIsotope
DilutionGC/MS.TableIF,Note1.
(B)EPAMethod1667,Formaldehyde,Isobutyraldehyde,andFurfuralbyDerivatizationFollowedbyHigh
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PerformanceLiquidChromatography.TableIF.
(C)Method1671,VolatileOrganicCompoundsSpecifictothePharmaceuticalManufacturingIndustryby
GC/FID.TableIF.
(iv)MethodsForTheDeterminationofNonconventionalPesticidesInMunicipalandIndustrial
Wastewater,VolumeI.RevisionI,August1993.EPA821R93010A,Pub.No.PB94121654.Tables
ID,IG.
(A)Method608.1,OrganochlorinePesticides.TableID,Note10TableIG,Note3.
(B)Method608.2,CertainOrganochlorinePesticides.TableID,Note10TableIG,Note3.
(C)Method614,OrganophosphorusPesticides.TableID,Note10TableIG,Note3.
(D)Method614.1,OrganophosphorusPesticides.TableID,Note10TableIG,Note3.
(E)Method615,ChlorinatedHerbicides.TableID,Note10TableIG,Note3.
(F)Method617,OrganohalidePesticidesandPCBs.TableID,Note10TableIG,Note3.
(G)Method619,TriazinePesticides.TableID,Note10TableIG,Note3.
(H)Method622,OrganophosphorusPesticides.TableID,Note10TableIG,Note3.
(I)Method622.1,ThiophosphatePesticides.TableID,Note10TableIG,Note3.
(J)Method627,DinitroanilinePesticides.TableID,Note10TableIG,Notes1and3.
(K)Method629,Cyanazine.TableIG,Note3.
(L)Method630,DithiocarbamatePesticides.TableIG,Note3.
(M)Method630.1,DithiocarbamatePesticides.TableIG,Note3.
(N)Method631,BenomylandCarbendazim.TableIG,Note3.
(O)Method632,CarbamateandUreaPesticides.TableID,Note10TableIG,Note3.
(P)Method632.1,CarbamateandAmidePesticides.TableIG,Note3.
(Q)Method633,OrganonitrogenPesticides.TableIG,Note3.
(R)Method633.1,NeutralNitrogenContainingPesticides.TableIG,Note3.
(S)Method637,MBTSandTCMTB.TableIG,Note3.
(T)Method644,Picloram.TableIG,Note3.
(U)Method645,CertainAminePesticidesandLethane.TableIG,Note3.
(V)Method1656,OrganohalidePesticides.TableID,Note10TableIG,Notes1and3.
(W)Method1657,OrganophosphorusPesticides.TableID,Note10TableIG,Note3.
(X)Method1658,PhenoxyAcidHerbicides.TableIG,Note3.
(Y)Method1659,Dazomet.TableIG,Note3.
(Z)Method1660,PyrethrinsandPyrethroids.TableIG,Note3.
(AA)Method1661,Bromoxynil.TableIG,Note3.
(BB)Ind01.MethodsEV024andEV025,AnalyticalProceduresforDeterminingTotalTinand
TriorganotininWastewater.TableIG,Note3.
(v)MethodsForTheDeterminationofNonconventionalPesticidesInMunicipalandIndustrial
Wastewater,VolumeII.August1993.EPA821R93010B,Pub.No.PB94166311.TableIG.
(A)Method200.9,DeterminationofTraceElementsbyStabilizedTemperatureGraphiteFurnaceAtomic
AbsorptionSpectrometry.TableIG,Note3.
(B)Method505,AnalysisofOrganohalidePesticidesandCommercialPolychlorinatedBiphenyl(PCB)
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ProductsinWaterbyMicroextractionandGasChromatography.TableID,Note10TableIG,Note3.
(C)Method507,TheDeterminationofNitrogenandPhosphorusContainingPesticidesinWaterbyGas
ChromatographywithaNitrogenPhosphorusDetector.TableID,Note10TableIG,Note3.
(D)Method508,DeterminationofChlorinatedPesticidesinWaterbyGasChromatographywithan
ElectronCaptureDetector.TableID,Note10TableIG,Note3.
(E)Method515.1,DeterminationofChlorinatedAcidsinWaterbyGasChromatographywithanElectron
CaptureDetector.TableIG,Notes2and3.
(F)Method515.2,DeterminationofChlorinatedAcidsinWaterUsingLiquidSolidExtractionandGas
ChromatographywithanElectronCaptureDetector.TableIG,Notes2and3.
(G)Method525.1,DeterminationofOrganicCompoundsinDrinkingWaterbyLiquidsSolidExtraction
andCapillaryColumnGasChromatography/MassSpectrometry.TableID,Note10TableIG,Note3.
(H)Method531.1,MeasurementofNMethylcarbamoyloximesandNMethylcarbamatesinWaterby
DirectAqueousInjectionHPLCwithPostColumnDerivatization.TableID,Note10TableIG,Note3.
(I)Method547,DeterminationofGlyphosateinDrinkingWaterbyDirectAqueousInjectionHPLC,Post
ColumnDerivatization,andFluorescenceDetection.TableIG,Note3.
(J)Method548,DeterminationofEndothallinDrinkingWaterbyAqueousDerivatization,LiquidSolid
Extraction,andGasChromatographywithElectronCaptureDetector.TableIG,Note3.
(K)Method548.1,DeterminationofEndothallinDrinkingWaterbyIonExchangeExtraction,Acidic
MethanolMethylationandGasChromatography/MassSpectrometry.TableIG,Note3.
(L)Method553,DeterminationofBenzidinesandNitrogenContainingPesticidesinWaterbyLiquid
LiquidExtractionorLiquidSolidExtractionandReversePhaseHighPerformanceLiquid
Chromatography/ParticleBeam/MassSpectrometryTableID,Note10TableIG,Note3.
(M)Method555,DeterminationofChlorinatedAcidsinWaterbyHighPerformanceLiquid
ChromatographyWithaPhotodiodeArrayUltravioletDetector.TableIG,Note3.
(vi)Inthecompendium MethodsfortheDeterminationofOrganicCompoundsinDrinkingWater.
RevisedJuly1991,December1998.EPA600/488039,Pub.No.PB92207703.TableIF.
(A)EPAMethod502.2,VolatileOrganicCompoundsinWaterbyPurgeandTrapCapillaryColumnGas
ChromatographywithPhotoionizationandElectrolyticConductivityDetectorsinSeries.TableIF.
(B)[Reserved]
(vii)Inthecompendium MethodsfortheDeterminationofOrganicCompoundsinDrinkingWater
SupplementII. August1992.EPA600/R92129,Pub.No.PB92207703.TableIF.
(A)EPAMethod524.2,MeasurementofPurgeableOrganicCompoundsinWaterbyCapillaryColumn
GasChromatography/MassSpectrometry.TableIF.
(B)[Reserved]
(viii)MethodsforMeasuringtheAcuteToxicityofEffluentsandReceivingWaterstoFreshwaterand
MarineOrganisms,FifthEdition.October2002.EPA821R02012,Pub.No.PB2002108488.TableIA,
Note26.
(ix)ShortTermMethodsforMeasuringtheChronicToxicityofEffluentsandReceivingWatersto
FreshwaterOrganisms,FourthEdition.October2002.EPA821R02013,Pub.No.PB2002108489.
TableIA,Note27.
(x)ShortTermMethodsforMeasuringtheChronicToxicityofEffluentsandReceivingWaterstoMarine
andEstuarineOrganisms,ThirdEdition.October2002.EPA821R02014,Pub.No.PB2002108490.
TableIA,Note28.
(8)OfficeofWater,U.S.EnvironmentalProtectionAgency,WashingtonDC(USEPA).Availableat
http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i)Method245.7,MercuryinWaterbyColdVaporAtomicFluorescenceSpectrometry.Revision2.0,
February2005.EPA821R05001.TableIB,Note17.
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(v)StandardMethodsfortheExaminationofWaterandWastewater.19thEdition,1995.TablesIA,IB,
IC,ID,IE,andIH.
(vi)StandardMethodsfortheExaminationofWaterandWastewater.20thEdition,1998.TablesIA,IB,
IC,ID,IE,andIH.
(vii)StandardMethodsfortheExaminationofWaterandWastewater.21stEdition,2005.TableIB,
Notes17and27.
(viii)2120,Color.2001.TableIB.
(ix)2130,Turbidity.2001.TableIB.
(x)2310,Acidity.1997.TableIB.
(xi)2320,Alkalinity.1997.TableIB.
(xii)2340,Hardness.1997.TableIB.
(xiii)2510,Conductivity.1997.TableIB.
(xiv)2540,Solids.1997.TableIB.
(xv)2550,Temperature.2000.TableIB.
(xvi)3111,MetalsbyFlameAtomicAbsorptionSpectrometry.1999.TableIB.
(xvii)3112,MetalsbyColdVaporAtomicAbsorptionSpectrometry.2009.TableIB.
(xviii)3113,MetalsbyElectrothermalAtomicAbsorptionSpectrometry.2004.TableIB.
(xix)3114,ArsenicandSeleniumbyHydrideGeneration/AtomicAbsorptionSpectrometry.2009.Table
IB.
(xx)3120,MetalsbyPlasmaEmission.1999.TableIB.
(xxi)3125,MetalsbyInductivelyCoupledPlasmaMassSpectrometry.2009.TableIB.
(xxii)3500Al,Aluminum.2001.TableIB.
(xxiii)3500As,Arsenic.1997.TableIB.
(xxiv)3500Ca,Calcium.1997.TableIB.
(xxv)3500Cr,Chromium.2009.TableIB.
(xxvi)3500Cu,Copper.1999.TableIB.
(xxvii)3500Fe,Iron.1997.TableIB.
(xxviii)3500Pb,Lead.1997.TableIB.
(xxix)3500Mn,Manganese.1999.TableIB.
(xxx)3500K,Potassium.1997.TableIB.
(xxxi)3500Na,Sodium.1997.TableIB.
(xxxii)3500V,Vanadium.1997.TableIB.
(xxxiii)3500Zn,Zinc.1997.TableIB.
(xxxiv)4110,DeterminationofAnionsbyIonChromatography.2000.TableIB.
(xxxv)4140,InorganicAnionsbyCapillaryIonElectrophoresis.1997.TableIB.
(xxxvi)4500B,Boron.2000.TableIB.
(xxxvii)4500Cl,Chloride.1997.TableIB.
(xxxviii)4500Cl,Chlorine(Residual).2000.TableIB.
(xxxix)4500CN,Cyanide.1999.TableIB.
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(xl)4500F ,Fluoride.1997.TableIB.
(xli)4500H+,pHValue.2000.TableIB.
(xlii)4500NH3,Nitrogen(Ammonia).1997.TableIB.
(xliii)4500NO2,Nitrogen(Nitrite).2000.TableIB.
(xliv)4500NO3,Nitrogen(Nitrate).2000.TableIB.
(xlv)4500Norg,Nitrogen(Organic).1997.TableIB.
(xlvi)4500O,Oxygen(Dissolved).2001.TableIB.
(xlvii)4500P,Phosphorus.1999.TableIB.
(xlviii)4500SiO2,Silica.1997.TableIB.
(xlix)4500S2,Sulfide.2000.TableIB.
(l)4500SO32,Sulfite.2000.TableIB.
(li)4500SO42,Sulfate.1997.TableIB.
(lii)5210,BiochemicalOxygenDemand(BOD).2001.TableIB.
(liii)5220,ChemicalOxygenDemand(COD).1997.TableIB.
(liv)5310,TotalOrganicCarbon(TOC).2000.TableIB.
(lv)5520,OilandGrease.2001.TableIB.
(lvi)5530,Phenols.2005.TableIB.
(lvii)5540,Surfactants.2000.TableIB.
(lviii)6200,VolatileOrganicCompounds.1997.TableIC.
(lix)6410,ExtractableBase/NeutralsandAcids.2000.TablesIC,ID.
(lx)6420,Phenols.2000.TableIC.
(lxi)6440,PolynuclearAromaticHydrocarbons.2000.TableIC.
(lxii)6630,OrganochlorinePesticides.2000.TableID.
(lxiii)6640,AcidicHerbicideCompounds.2001.TableID.
(lxiv)7110,GrossAlphaandGrossBetaRadioactivity(Total,Suspended,andDissolved).2000.Table
IE.
(lxv)7500,Radium.2001.TableIE.
(lxvi)9213,RecreationalWaters.2007.TableIH.
(lxvii)9221,MultipleTubeFermentationTechniqueforMembersoftheColiformGroup.2006.TableIA,
Notes12and14TableIH,Notes11and13.
(lxviii)9222,MembraneFilterTechniqueforMembersoftheColiformGroup.1997.TableIATableIH,
Note18.
(lxix)9223,EnzymeSubstrateColiformTest.2004.TableIATableIH.
(lxx)9230,Fecal Enterococcus / Streptococcus Groups.2007.TableIATableIH.
(11)TheAnalyst,TheRoyalSocietyofChemistry,RSCPublishing,RoyalSocietyofChemistry,
ThomasGrahamHouse,SciencePark,MiltonRoad,CambridgeCB40WF,UnitedKingdom.(Also
availablefrommostpubliclibraries.)
(i)SpectrophotometricDeterminationofAmmonia:AStudyofaModifiedBerthelotReactionUsing
SalicylateandDichloroisocyanurate.Krom,M.D.105:305316,April1980.TableIB,Note60.
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(ii)[Reserved]
(12)AnalyticalChemistry,ACSPublications,1155SixteenthSt.NW.,WashingtonDC20036.(Also
availablefrommostpubliclibraries.)
(i)SpectrophotometricandKineticsInvestigationoftheBerthelotReactionfortheDeterminationof
Ammonia.Patton,C.J.andS.R.Crouch.49(3):464469,March1977.TableIB,Note60.
(ii)[Reserved]
(13)AOACInternational,481NorthFrederickAvenue,Suite500,Gaithersburg,MD208772417.
(i)OfficialMethodsofAnalysisofAOACInternational.16thEdition,4thRevision,1998.
(A)920.203,ManganeseinWater,PersulfateMethod.TableIB,Note3.
(B)925.54,SulfateinWater,GravimetricMethod.TableIB,Note3.
(C)973.40,SpecificConductanceofWater.TableIB,Note3.
(D)973.41,pHofWater.TableIB,Note3.
(E)973.43,AlkalinityofWater,TitrimetricMethod.TableIB,Note3.
(F)973.44,BiochemicalOxygenDemand(BOD)ofWater,IncubationMethod.TableIB,Note3.
(G)973.45,Oxygen(Dissolved)inWater,TitrimetricMethods.TableIB,Note3.
(H)973.46,ChemicalOxygenDemand(COD)ofWater,TitrimetricMethods.TableIB,Note3.
(I)973.47,OrganicCarboninWater,InfraredAnalyzerMethod.TableIB,Note3.
(J)973.48,Nitrogen(Total)inWater,KjeldahlMethod.TableIB,Note3.
(K)973.49,Nitrogen(Ammonia)inWater,ColorimetricMethod.TableIB,Note3.
(L)973.50,Nitrogen(Nitrate)inWater,BrucineColorimetricMethod.TableIB,Note3.
(M)973.51,ChlorideinWater,MercuricNitrateMethod.TableIB,Note3.
(N)973.52,HardnessofWater.TableIB,Note3.
(O)973.53,PotassiuminWater,AtomicAbsorptionSpectrophotometricMethod.TableIB,Note3.
(P)973.54,SodiuminWater,AtomicAbsorptionSpectrophotometricMethod.TableIB,Note3.
(Q)973.55,PhosphorusinWater,PhotometricMethod.TableIB,Note3.
(R)973.56,PhosphorusinWater,AutomatedMethod.TableIB,Note3.
(S)974.27,Cadmium,Chromium,Copper,Iron,Lead,Magnesium,Manganese,Silver,ZincinWater,
AtomicAbsorptionSpectrophotometricMethod.TableIB,Note3.
(T)977.22,MercuryinWater,FlamelessAtomicAbsorptionSpectrophotometricMethod.TableIB,Note
3.
(U)991.15.TotalColiformsand Escherichiacoli inWaterDefinedSubstrateTechnology(Colilert)
Method.TableIA,Note10TableIH,Note10.
(V)993.14,TraceElementsinWatersandWastewaters,InductivelyCoupledPlasmaMass
SpectrometricMethod.TableIB,Note3.
(W)993.23,DissolvedHexavalentChromiuminDrinkingWater,GroundWater,andIndustrial
WastewaterEffluents,IonChromatographicMethod.TableIB,Note3.
(X)993.30,InorganicAnionsinWater,IonChromatographicMethod.TableIB,Note3.
(ii)[Reserved]
(14)AppliedandEnvironmentalMicrobiology,AmericanSocietyforMicrobiology,1752NStreetNW.,
WashingtonDC20036.(Alsoavailablefrommostpubliclibraries.)
(i)NewMediumfortheSimultaneousDetectionofTotalColiformsand Escherichiacoli inWater.
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Brenner,K.P.,C.C.Rankin,Y.R.Roybal,G.N.Stelma,Jr.,P.V.Scarpino,andA.P.Dufour.59:3534
3544,November1993.TableIH,Note21.
(ii)[Reserved]
(15)ASTMInternational,100BarrHarborDrive,P.O.BoxC700,WestConshohocken,PA194282959,
oronlineat http://www.astm.org.
(i)AnnualBookofASTMStandards,Water,andEnvironmentalTechnology,Section11,Volumes11.01
and11.02.1994.TablesIA,IB,IC,ID,IE,andIH.
(ii)AnnualBookofASTMStandards,Water,andEnvironmentalTechnology,Section11,Volumes11.01
and11.02.1996.TablesIA,IB,IC,ID,IE,andIH.
(iii)AnnualBookofASTMStandards,Water,andEnvironmentalTechnology,Section11,Volumes
11.01and11.02.1999.TablesIA,IB,IC,ID,IE,andIH.
(iv)AnnualBookofASTMStandards,Water,andEnvironmentalTechnology,Section11,Volumes
11.01and11.02.2000.TablesIA,IB,IC,ID,IE,andIH.
(v)ASTMD51108,StandardTestMethodsforCalciumandMagnesiuminWater.November2008.
TableIB.
(vi)ASTMD51204,StandardTestMethodsforChlorideIoninWater.July2004.TableIB.
(vii)ASTMD51588,TestMethodsforPhosphorusinWater,March1989.TableIB.
(viii)ASTMD51607,StandardTestMethodforSulfateIoninWater,September2007.TableIB.
(ix)ASTMD85807,StandardTestMethodsforManganeseinWater.August2007.TableIB.
(x)ASTMD85905,StandardTestMethodforSilicainWater.February2005.TableIB.
(xi)ASTMD88809,StandardTestMethodsforDissolvedOxygeninWater.December2009.TableIB.
(xii)ASTMD106706,StandardTestMethodsforAcidityorAlkalinityofWater.January2007.TableIB.
(xiii)ASTMD106805e1,StandardTestMethodsforIroninWater.July2005.TableIB.
(xiv)ASTMD112595(Reapproved1999),StandardTestMethodsforElectricalConductivityand
ResistivityofWater.December1995.TableIB.
(xv)ASTMD112602(Reapproved2007)e1,StandardTestMethodforHardnessinWater.August2007.
TableIB.
(xvi)ASTMD117904,StandardTestMethodsforFluorideIoninWater.July2004.TableIB.
(xvii)ASTMD124605,StandardTestMethodforBromideIoninWater.February2005.TableIB.
(xviii)ASTMD125206,StandardTestMethodsforChemicalOxygenDemand(DichromateOxygen
Demand)ofWater.February2006.TableIB.
(xix)ASTMD125308,StandardTestMethodforResidualChlorineinWater.October2008.TableIB.
(xx)ASTMD129399,StandardTestMethodsforpHofWater.March2000.TableIB.
(xxi)ASTMD142608,StandardTestMethodsforAmmoniaNitrogeninWater.September2008.Table
IB.
(xxii)ASTMD168702(Reapproved2007)e1,StandardTestMethodsforChromiuminWater.August
2007.TableIB.
(xxiii)ASTMD168807,StandardTestMethodsforCopperinWater.August2007.TableIB.
(xxiv)ASTMD169102(Reapproved2007)e1,StandardTestMethodsforZincinWater.August2007.
TableIB.
(xxv)ASTMD178301(Reapproved2007),StandardTestMethodsforPhenolicCompoundsinWater.
January2008).TableIB.
(xxvi)ASTMD188608,StandardTestMethodsforNickelinWater.October2008.TableIB.
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(xxvii)ASTMD188900,StandardTestMethodforTurbidityofWater.October2000.TableIB.
(xxviii)ASTMD189096,StandardTestMethodforBetaParticleRadioactivityofWater.April1996.
TableIE.
(xxix)ASTMD194396,StandardTestMethodforAlphaParticleRadioactivityofWater.April1996.
TableIE.
(xxx)ASTMD197607,StandardTestMethodforElementsinWaterbyInductivelyCoupledArgon
PlasmaAtomicEmissionSpectroscopy.August2007.TableIB.
(xxxi)ASTMD203609,StandardTestMethodsforCyanidesinWater.October2009.TableIB.
(xxxii)ASTMD233002,StandardTestMethodforMethyleneBlueActiveSubstances.August2002.
TableIB.
(xxxiii)ASTMD246097,StandardTestMethodforAlphaParticleEmittingIsotopesofRadiuminWater.
October1997.TableIE.
(xxxiv)ASTMD297208,StandardTestsMethodforArsenicinWater.October2008.TableIB.
(xxxv)ASTMD322302(Reapproved2007)e1,StandardTestMethodforTotalMercuryinWater.August
2007.TableIB.
(xxxvi)ASTMD337195,StandardTestMethodforNitrilesinAqueousSolutionbyGasLiquid
Chromatography,February1996.TableIF.
(xxxvii)ASTMD337303(Reapproved2007)e1,StandardTestMethodforVanadiuminWater.September
2007.TableIB.
(xxxviii)ASTMD345497,StandardTestMethodforRadium226inWater.February1998.TableIE.
(xxxix)ASTMD355702(Reapproved2007)e1,StandardTestMethodforCadmiuminWater.September
2007.TableIB.
(xl)ASTMD355808,StandardTestMethodforCobaltinWater.November2008.TableIB.
(xli)ASTMD355908,StandardTestMethodsforLeadinWater.October2008.TableIB.
(xlii)ASTMD359002(Reapproved2006),StandardTestMethodsforTotalKjeldahlNitrogeninWater.
February2007.TableIB.
(xliii)ASTMD364508,StandardTestMethodsforBerylliuminWater.October2008.TableIB.
(xliv)ASTMD369595,StandardTestMethodforVolatileAlcoholsinWaterbyDirectAqueousInjection
GasChromatography.April1995.TableIF.
(xlv)ASTMD385908,StandardTestMethodsforSeleniuminWater.October2008.TableIB.
(xlvi)ASTMD386704,StandardTestMethodforNitriteNitrateinWater.July2004.TableIB.
(xlvii)ASTMD419008,StandardTestMethodforElementsinWaterbyDirectCurrentPlasmaAtomic
EmissionSpectroscopy.October2008.TableIB.
(xlviii)ASTMD428202,StandardTestMethodforDeterminationofFreeCyanideinWaterand
WastewaterbyMicrodiffusion.August2002.TableIB.
(xlix)ASTMD432703,StandardTestMethodforAnionsinWaterbyChemicallySuppressedIon
Chromatography.January2003.TableIB.
(l)ASTMD438202(Reapproved2007)e1,StandardTestMethodforBariuminWater,AtomicAbsorption
Spectrophotometry,GraphiteFurnace.September2007.TableIB.
(li)ASTMD465792(Reapproved1998),StandardTestMethodforPolynuclearAromaticHydrocarbons
inWater.January1993.TableIC.
(lii)ASTMD465808,StandardTestMethodforSulfideIoninWater.August2008.TableIB.
(liii)ASTMD476388(Reapproved2001),StandardPracticeforIdentificationofChemicalsinWaterby
FluorescenceSpectroscopy.September1988.TableIF.
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(liv)ASTMD483903,StandardTestMethodforTotalCarbonandOrganicCarboninWaterby
Ultraviolet,orPersulfateOxidation,orBoth,andInfraredDetection.January2003.TableIB.
(lv)ASTMD525703,StandardTestMethodforDissolvedHexavalentChromiuminWaterbyIon
Chromatography.January2003.TableIB.
(lvi)ASTMD525992,StandardTestMethodforIsolationandEnumerationofEnterococcifromWaterby
theMembraneFilterProcedure.October1992.TableIH,Note9.
(lvii)ASTMD539293,StandardTestMethodforIsolationandEnumerationof Escherichiacoli inWater
bytheTwoStepMembraneFilterProcedure.September1993.TableIH,Note9.
(lviii)ASTMD567305,StandardTestMethodforElementsinWaterbyInductivelyCoupledPlasma
MassSpectrometry.July2005.TableIB.
(lix)ASTMD590703,StandardTestMethodforFilterableandNonfilterableMatterinWater.July2003.
TableIB.
(lx)ASTMD650399,StandardTestMethodforEnterococciinWaterUsingEnterolert.April2000.Table
IANote9,TableIH,Note9.
(lxi)ASTM.D650800(Reapproved2005)E2,StandardTestMethodforDeterminationofDissolved
InorganicAnionsinAqueousMatricesUsingCapillaryIonElectrophoresisandChromateElectrolyte.
April2005.TableIB.
(lxii)ASTM.D688809,StandardTestMethodforAvailableCyanidewithLigandDisplacementandFlow
InjectionAnalysis(FIA)UtilizingGasDiffusionSeparationandAmperometricDetection.October2009.
TableIB,Note59.
(lxiii)ASTM.D691909,StandardTestMethodforDeterminationofDissolvedAlkaliandAlkalineEarth
CationsandAmmoniuminWaterandWastewaterbyIonChromatography.May2009.TableIB.
(lxiv)ASTM.D706506,StandardTestMethodforDeterminationofNonylphenol,BisphenolA,ptert
Octylphenol,NonylphenolMonoethoxylateandNonylphenolDiethoxylateinEnvironmentalWatersby
GasChromatographyMassSpectrometry.January2007.TableIC.
(lxv)ASTM.D723710,StandardTestMethodforFreeCyanidewithFlowInjectionAnalysis(FIA)
UtilizingGasDiffusionSeparationandAmperometricDetection.June2010.TableIB.
(lxvi)ASTM.D728408,StandardTestMethodforTotalCyanideinWaterbyMicroDistillationfollowed
byFlowInjectionAnalysiswithGasDiffusionSeparationandAmperometricDetection.April2008).
TableIB.
(lxvii)ASTM.D736509a,StandardPracticeforSampling,Preservation,andMitigatingInterferencesin
WaterSamplesforAnalysisofCyanide.October2009.TableII,Notes5and6.
(lxviii)ASTM.D751109E2,StandardTestMethodforTotalCyanidebySegmentedFlowInjection
Analysis,InLineUltravioletDigestionandAmperometricDetection.March2009.TableIB.
(lxix)ASTM.D757309,StandardTestMethodforTotalCarbonandOrganicCarboninWaterbyHigh
TemperatureCatalyticCombustionandInfraredDetection.November2009.TableIB.
(16)Bran&LuebbeAnalyzingTechnologies,Inc.,ElmsfordNY10523.
(i)IndustrialMethodNumber37875WA,HydrogenIon(pH)AutomatedElectrodeMethod,Bran&
Luebbe(Technicon)AutoAnalyzerII.October1976.TableIB,Note21.
(ii)[Reserved]
(17)CEMCorporation,P.O.Box200,MatthewsNC281060200.
(i)ClosedVesselMicrowaveDigestionofWastewaterSamplesforDeterminationofMetals.April16,
1992.TableIB,Note36.
(ii)[Reserved]
(18)CraigR.Chinchilla,900JorieBlvd.,Suite35,OakBrookIL60523.Telephone:6306450600.
(i)NitratebyDiscreteAnalysisEasy(1Reagent)NitrateMethod,(Colorimetric,Automated,1Reagent).
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Revision1,November12,2011.TableIB,Note62.
(ii)[Reserved]
(19)HachCompany,P.O.Box389,LovelandCO80537.
(i)Method8000,ChemicalOxygenDemand.HachHandbookofWaterAnalysis.1979.TableIB,Note
14.
(ii)Method8008,1,10PhenanthrolineMethodusingFerroVerIronReagentforWater.1980.TableIB,
Note22.
(iii)Method8009,ZinconMethodforZinc.HachHandbookforWaterAnalysis.1979.TableIB,Note33.
(iv)Method8034,PeriodateOxidationMethodforManganese.HachHandbookforWaterAnalysis.
1979.TableIB,Note23.
(v)Method8506,BicinchoninateMethodforCopper.HachHandbookofWaterAnalysis.1979.TableIB,
Note19.
(vi)Method8507,Nitrogen,NitriteLowRange,DiazotizationMethodforWaterandWastewater.1979.
TableIB,Note25.
(vii)HachMethod10360,LuminescenceMeasurementofDissolvedOxygeninWaterandWastewater
andforUseintheDeterminationofBOD5andcBOD5.Revision1.2,October2011.TableIB,Note63.
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(i)MitchellMethodM5271,DeterminationofTurbiditybyNephelometry.Revision1.0,July31,2008.
TableIB,Note66.
(ii)MitchellMethodM5331,DeterminationofTurbiditybyNephelometry.Revision1.0,July31,2008.
TableIB,Note65.
(25)NationalCouncilofthePaperIndustryforAirandStreamImprovements,Inc.(NCASI),260
MadisonAvenue,NewYorkNY10016.
(i)NCASITechnicalBulletinNo.253,AnInvestigationofImprovedProceduresforMeasurementofMill
EffluentandReceivingWaterColor.December1971.TableIB,Note18.
(ii)[Reserved]
(26)OceanographyInternationalCorporation,512WestLoop,P.O.Box2980,CollegeStationTX77840.
(i)OICChemicalOxygenDemandMethod.1978.TableIB,Note13.
(ii)[Reserved]
(27)OIAnalytical,Box9010,CollegeStationTX778209010.
(i)MethodOIA167709,AvailableCyanidebyLigandExchangeandFlowInjectionAnalysis(FIA).
Copyright2010.TableIB,Note59.
(ii)MethodPAIDK01,Nitrogen,TotalKjeldahl,BlockDigestion,SteamDistillation,Titrimetric
Detection.RevisedDecember22,1994.TableIB,Note39.
(iii)MethodPAIDK02,Nitrogen,TotalKjeldahl,BlockDigestion,SteamDistillation,Colorimetric
Detection.RevisedDecember22,1994.TableIB,Note40.
(iv)MethodPAIDK03,Nitrogen,TotalKjeldahl,BlockDigestion,AutomatedFIAGasDiffusion.Revised
December22,1994.TableIB,Note41.
(28)ORIONResearchCorporation,840MemorialDrive,Cambridge,Massachusetts02138.
(i)ORIONResearchInstructionManual,ResidualChlorineElectrodeModel9770.1977.TableIB,Note
16.
(ii)[Reserved]
(29)TechniconIndustrialSystems,TarrytownNY10591.
(i)IndustrialMethodNumber37975WEAmmonia,AutomatedElectrodeMethod,TechniconAuto
AnalyzerII.February19,1976.TableIB,Note7.
(ii)[Reserved]
(30)ThermoJarrellAshCorporation,27ForgeParkway,FranklinMA02038.
(i)MethodAES0029.DirectCurrentPlasma(DCP)OpticalEmissionSpectrometricMethodforTrace
ElementalAnalysisofWaterandWastes.1986,Revised1991.TableIB,Note34.
(ii)[Reserved]
(31)ThermoScientific,166CummingsCenter,BeverlyMA01915.Telephone:18002251480.
www.thermoscientific.com.
(i)ThermoScientificOrionMethodAQ4500,DeterminationofTurbiditybyNephelometry.Revision5,
March12,2009.TableIB,Note67.
(ii)[Reserved]
(32)3MCorporation,3MCenterBuilding2209E10,St.PaulMN551441000.
(i)OrganochlorinePesticidesandPCBsinWastewaterUsingEmporeTMDiskTestMethod3M0222.
RevisedOctober28,1994.TableIC,Note8TableID,Note8.
(ii)[Reserved]
(33)U.S.GeologicalSurvey(USGS),U.S.DepartmentoftheInterior,Reston,Virginia.Availablefrom
https://www.gpo.gov/fdsys/pkg/CFR2014title40vol23/xml/CFR2014title40vol23sec1363.xml 57/64
1/26/2016 CodeofFederalRegulations
USGSBooksandOpenFileReports(OFR)Section,FederalCenter,Box25425,Denver,CO80225.
(i)OFR76177,SelectedMethodsoftheU.S.GeologicalSurveyofAnalysisofWastewaters.1976.
TableIE,Note2.
(ii)OFR91519,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofOrganonitrogenHerbicidesinWaterbySolidPhaseExtractionandCapillaryColumn
GasChromatography/MassSpectrometryWithSelectedIonMonitoring.1992.TableID,Note14.
(iii)OFR92146,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofTotalPhosphorusbyaKjeldahlDigestionMethodandanAutomatedColorimetric
FinishThatIncludesDialysis.1992.TableIB,Note48.
(iv)OFR93125,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofInorganicandOrganicConstituentsinWaterandFluvialSediments.1993.TableIB,
Note51TableIC,Note9.
(v)OFR93449,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofChromiuminWaterbyGraphiteFurnaceAtomicAbsorptionSpectrophotometry.
1993.TableIB,Note46.
(vi)OFR9437,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofTriazineandOtherNitrogencontainingCompoundsbyGasChromatographywith
NitrogenPhosphorusDetectors.1994.TableID,Note9.
(vii)OFR95181,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofPesticidesinWaterbyC18SolidPhaseExtractionandCapillaryColumnGas
Chromatography/MassSpectrometryWithSelectedIonMonitoring.1995.TableID,Note11.
(viii)OFR97198,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofMolybdenuminWaterbyGraphiteFurnaceAtomicAbsorptionSpectrophotometry.
1997.TableIB,Note47.
(ix)OFR98165,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofElementsinWholeWaterDigestsUsingInductivelyCoupledPlasmaOptical
EmissionSpectrometryandInductivelyCoupledPlasmaMassSpectrometry.1998.TableIB,Note50.
(x)OFR98639,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofArsenicandSeleniuminWaterandSedimentbyGraphiteFurnaceAtomic
AbsorptionSpectrometry.1999.TableIB,Note49.
(xi)OFR00170,MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory
DeterminationofAmmoniumPlusOrganicNitrogenbyaKjeldahlDigestionMethodandanAutomated
PhotometricFinishthatIncludesDigestCleanupbyGasDiffusion.2000.TableIB,Note45.
(xii)WaterResourcesInvestigationReport014098,MethodsofAnalysisbytheU.S.GeologicalSurvey
NationalWaterQualityLaboratoryDeterminationofModerateUsePesticidesandSelectedDegradates
inWaterbyC18SolidPhaseExtractionandGasChromatography/MassSpectrometry.2001.TableID,
Note13.
(xiii)WaterResourcesInvestigationsReport014132,MethodsofAnalysisbytheU.S.Geological
SurveyNationalWaterQualityLaboratoryDeterminationofOrganicPlusInorganicMercuryinFiltered
andUnfilteredNaturalWaterWithColdVaporAtomicFluorescenceSpectrometry.2001.TableIB,Note
71.
(xiv)WaterResourcesInvestigationReport014134,MethodsofAnalysisbytheU.S.Geological
SurveyNationalWaterQualityLaboratoryDeterminationofPesticidesinWaterbyGraphitizedCarbon
BasedSolidPhaseExtractionandHighPerformanceLiquidChormatography/MassSpectrometry.2001.
TableID,Note12.
(xv)MethodsforDeterminationofInorganicSubstancesinWaterandFluvialSediments,editors,
TechniquesofWaterResourcesInvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA1.
1979.TableIB,Note8.
(xvi)MethodsforDeterminationofInorganicSubstancesinWaterandFluvialSediments,Techniquesof
WaterResourcesInvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA1.1989.TableIB,
Note2.
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(xvii)MethodsfortheDeterminationofOrganicSubstancesinWaterandFluvialSediments.Techniques
ofWaterResourcesInvestigationsoftheU.S.GeologicalSurvey,Book5,ChapterA3.1987.TableIB,
Note24TableID,Note4.
(xviii)TechniquesandMethodsBook5B1,DeterminationofElementsinNaturalWater,Biota,
SedimentandSoilSamplesUsingCollision/ReactionCellInductivelyCoupledPlasmaMass
Spectrometry.Chapter1,SectionB,MethodsoftheNationalWaterQualityLaboratory,Book5,
LaboratoryAnalysis.2006.TableIB,Note70.
(xix)U.S.GeologicalSurveyTechniquesofWaterResourcesInvestigations,Book5,Laboratory
Analysis,ChapterA4,MethodsforCollectionandAnalysisofAquaticBiologicalandMicrobiological
Samples.1989.TableIA,Note4TableIH,Note4.
(xx)WaterTemperatureInfluentialFactors,FieldMeasurementandDataPresentation,Techniquesof
WaterResourcesInvestigationsoftheU.S.GeologicalSurvey,Book1,ChapterD1.1975.TableIB,
Note32.
(34)WatersCorporation,34MapleStreet,MilfordMA01757,Telephone:5084822131,Fax:508482
3625.
(i)MethodD6508,TestMethodforDeterminationofDissolvedInorganicAnionsinAqueousMatrices
UsingCapillaryIonElectrophoresisandChromateElectrolyte.Revision2,December2000.TableIB,
Note54.
(ii)[Reserved]
(c)Undercertaincircumstances,theRegionalAdministratorortheDirectorintheRegionorStatewhere
thedischargewilloccurmaydetermineforaparticulardischargethatadditionalparametersorpollutants
mustbereported.Undersuchcircumstances,additionaltestproceduresforanalysisofpollutantsmay
bespecifiedbytheRegionalAdministrator,ortheDirectoruponrecommendationoftheAlternateTest
ProcedureProgramCoordinator,Washington,DC.
(d)Undercertaincircumstances,theAdministratormayapproveadditionalalternatetestproceduresfor
nationwideuse,uponrecommendationbytheAlternateTestProcedureProgramCoordinator,
Washington,DC.
(e)Samplepreservationprocedures,containermaterials,andmaximumallowableholdingtimesfor
parametersarecitedinTablesIA,IB,IC,ID,IE,IF,IG,andIHareprescribedinTableII.Informationin
thetabletakesprecedenceoverinformationinspecificmethodsorelsewhere.Anypersonmayapplyfor
achangefromtheprescribedpreservationtechniques,containermaterials,andmaximumholdingtimes
applicabletosamplestakenfromaspecificdischarge.Applicationsforsuchlimitedusechangesmay
bemadebyletterstotheRegionalAlternativeTestProcedure(ATP)ProgramCoordinatororthe
permittingauthorityintheRegioninwhichthedischargewilloccur.Sufficientdatashouldbeprovidedto
assuresuchchangesinsamplepreservation,containersorholdingtimesdonotadverselyaffectthe
integrityofthesample.TheRegionalATPCoordinatororpermittingauthoritywillreviewtheapplication
andthennotifytheapplicantandtheappropriateStateagencyofapprovalorrejectionoftheuseofthe
alternatetestprocedure.Adecisiontoapproveordenyanyrequestondeviationsfromtheprescribed
TableIIrequirementswillbemadewithin90daysofreceiptoftheapplicationbytheRegional
Administrator.Ananalystmaynotmodifyanysamplepreservationand/orholdingtimerequirementsof
anapprovedmethodunlesstherequirementsofthissectionaremet.
TableIIRequiredContainers,PreservationTechniques,andHoldingTimes
Container Maximum
Parameternumber/name Preservation23
1 holdingtime4
TableIABacterialTests:
Cool,<10C,0.0008%
15.Coliform,total,fecal,and E.coli PA,G Na2S2O35 8hours.2223
Cool,<10C,0.0008%
6.Fecalstreptococci PA,G Na2S2O35 8hours.22
Cool,<10C,0.0008%
7.Enterococci PA,G Na2S2O35 8hours.22
Cool,<10C,0.0008%
8. Salmonella PA,G 8hours.22
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Na2S2O35
TableIAAquaticToxicityTests:
TableIBInorganicTests:
Cool,6C18,H2SO4to
4.Ammonia P,FP,G 28days.
pH<2
P,FP,or HNO3topH<2
10.Boron 6months.
Quartz
Cool,6C18,H2SO4to
15.Chemicaloxygendemand P,FP,G 28days.
pH<2
Analyzewithin15
17.Chlorine,totalresidual P,G Nonerequired
minutes.
Cool,6C18,NaOHto
2324.Cyanide,totaloravailable(orCATC)andfree P,FP,G pH>1056,reducingagent 14days.
ifoxidizerpresent
Analyzewithin15
28.Hydrogenion(pH) P,FP,G Nonerequired
minutes.
Cool,6C18,H2SO4to
31,43.KjeldahlandorganicN P,FP,G 28days.
pH<2
TableIBMetals:7
Cool,6C18,pH=9.3
18.ChromiumVI P,FP,G 28days.
9.720
FP,Gand
5mL/L12NHClor5mL/L
35.Mercury(CVAFS) FPlined 90days.17
BrCl17
cap17
3,58,12,13,19,20,22,26,29,30,3234,36,37,45, HNO3topH<2,oratleast
47,51,52,5860,62,63,7072,74,75.Metals,except P,FP,G 6months.
boron,chromiumVI,andmercury 24hourspriortoanalysis19
Cool,6C18,H2SO4to
39.Nitratenitrite P,FP,G 28days.
pH<2
Coolto6C18,HClor
41.Oilandgrease G H2SO4topH<2 28days.
Coolto6C18,HCl,
42.OrganicCarbon P,FP,G H2SO4,orH3PO4topH<2 28days.
Filterwithin15
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44.Orthophosphate P,FP,G Cool,to6C1824 minutesAnalyze
within48hours.
G,Bottle Analyzewithin15
46.Oxygen,DissolvedProbe Nonerequired
andtop minutes.
G,Bottle
47.Winkler Fixonsiteandstoreindark 8hours.
andtop
Cool,6C18,H2SO4to
48.Phenols G 28days.
pH<2
Cool,6C18,H2SO4to
50.Phosphorous,total P,FP,G 28days.
pH<2
Cool,6C18,addzinc
66.Sulfide P,FP,G acetateplussodium 7days.
hydroxidetopH>9
Analyzewithin15
67.Sulfite P,FP,G Nonerequired
minutes.
TableICOrganicTests:8
G,FPlined Cool,6C18,0.008%
6,57,106.Purgeablearomatichydrocarbons Na2S2O35,HCltopH29 14days.9
septum
G,FPlined Cool,6C18,0.008%
3,4.Acroleinandacrylonitrile Na2S2O3,pHto4510 14days.10
septum
Cool,6C18,0.008% 7daysuntil
G,FPlined
23,30,44,49,53,77,80,81,98,100,112.Phenols11 Na2S2O3 extraction,40days
cap
afterextraction.
7daysuntil
G,FPlined
14,17,48,5052.Phthalateesters11 Cool,6C18 extraction,40days
cap
afterextraction.
1yearuntil
G,FPlined
8894.PCBs11 Cool,6C18 extraction,1year
cap
afterextraction.
7daysuntil
G,FPlined Cool,6C18,storein
54,55,75,79.Nitroaromaticsandisophorone11 extraction,40days
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cap dark,0.008%Na2S2O35 afterextraction.
Cool,6C18,storein 7daysuntil
1,2,5,812,32,33,58,59,74,78,99,101.Polynuclear G,FPlined
dark,0.008%Na2S2O35 extraction,40days
aromatichydrocarbons11 cap
afterextraction.
Cool,6C18,0.008% 7daysuntil
G,FPlined
15,16,21,31,87.Haloethers11 Na2S2O35 extraction,40days
cap
afterextraction.
7daysuntil
G,FPlined
29,3537,6365,107.Chlorinatedhydrocarbons11 Cool,6C18 extraction,40days
cap
afterextraction.
6062,6672,85,86,9597,102,103.CDDs/CDFs11
Cool,6C18,0.008%
AqueousSamples:FieldandLabPreservation G Na2S2O35,pH<9 1year.
Solids,MixedPhase,andTissueSamples:Lab
G Freeze,10C 1year.
Preservation
Cool,<6C,H2SO4topH 28daysuntil
114118.Alkylatedphenols G extraction,40days
<2 afterextraction.
Cool,<6C,0.008% 30daysuntil
120.ChlorinatedPhenolics Na2S2O3H2SO4topH<2 acetylation,30days
afteracetylation.
TableIDPesticidesTests:
7daysuntil
G,FPlined
170.Pesticides11 Cool,6C18,pH5915 extraction,40days
cap
afterextraction.
TableIERadiologicalTests:
TableIHBacterialTests:
Cool,<10C,0.0008%
1. E.coli PA,G Na2S2O35 8hours.22
Cool,<10C,0.0008%
2.Enterococci PA,G Na2S2O35 8hours.22
TableIHProtozoanTests:
LDPEfield
8. Cryptosporidium 110C 96hours.21
filtration
LDPEfield
9. Giardia 110C 96hours.21
filtration
1PisforpolyethyleneFPisfluoropolymer(polytetrafluoroethylene(PTFE)Teflon),orotherfluoropolymer,unless
statedotherwiseinthisTableIIGisglassPAisanyplasticthatismadeofasterilizablematerial(polypropyleneorother
autoclavableplastic)LDPEislowdensitypolyethylene.
2ExceptwherenotedinthisTableIIandthemethodfortheparameter,preserveeachgrabsamplewithin15minutesof
collection.Foracompositesamplecollectedwithanautomatedsample(e.g.,usinga24hourcompositesamplesee40
CFR122.21(g)(7)(i)or40CFRPart403,AppendixE),refrigeratethesampleat6Cduringcollectionunlessspecified
otherwiseinthisTableIIorinthemethod(s).Foracompositesampletobesplitintoseparatealiquotsforpreservation
and/oranalysis,maintainthesampleat6C,unlessspecifiedotherwiseinthisTableIIorinthemethod(s),untilcollection,
splitting,andpreservationiscompleted.Addthepreservativetothesamplecontainerpriortosamplecollectionwhenthe
preservativewillnotcompromisetheintegrityofagrabsample,acompositesample,oraliquotsplitfromacompositesample
within15minutesofcollection.Ifacompositemeasurementisrequiredbutacompositesamplewouldcompromisesample
integrity,individualgrabsamplesmustbecollectedatprescribedtimeintervals(e.g.,4samplesoverthecourseofaday,at
6hourintervals).Grabsamplesmustbeanalyzedseparatelyandtheconcentrationsaveraged.Alternatively,grabsamples
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maybecollectedinthefieldandcompositedinthelaboratoryifthecompositingprocedureproducesresultsequivalentto
resultsproducedbyarithmeticaveragingofresultsofanalysisofindividualgrabsamples.Forexamplesoflaboratory
compositingprocedures,seeEPAMethod1664Rev.A(oilandgrease)andtheproceduresat40CFR141.34(f)(14)(iv)
and(v)(volatileorganics).
3WhenanysampleistobeshippedbycommoncarrierorsentviatheU.S.PostalService,itmustcomplywiththe
DepartmentofTransportationHazardousMaterialsRegulations(49CFRpart172).Thepersonofferingsuchmaterialfor
transportationisresponsibleforensuringsuchcompliance.ForthepreservationrequirementofTableII,theOfficeof
HazardousMaterials,MaterialsTransportationBureau,DepartmentofTransportationhasdeterminedthattheHazardous
MaterialsRegulationsdonotapplytothefollowingmaterials:Hydrochloricacid(HCl)inwatersolutionsatconcentrationsof
0.04%byweightorless(pHabout1.96orgreaterNitricacid(HNO3)inwatersolutionsatconcentrationsof0.15%by
weightorless(pHabout1.62orgreater)Sulfuricacid(H2SO4)inwatersolutionsatconcentrationsof0.35%byweightor
less(pHabout1.15orgreater)andSodiumhydroxide(NaOH)inwatersolutionsatconcentrationsof0.080%byweightor
less(pHabout12.30orless).
4Samplesshouldbeanalyzedassoonaspossibleaftercollection.Thetimeslistedarethemaximumtimesthatsamples
maybeheldbeforethestartofanalysisandstillbeconsideredvalid.Samplesmaybeheldforlongerperiodsonlyifthe
permitteeormonitoringlaboratoryhasdataonfiletoshowthat,forthespecifictypesofsamplesunderstudy,theanalytes
arestableforthelongertime,andhasreceivedavariancefromtheRegionalAdministratorunderSec.136.3(e).Foragrab
sample,theholdingtimebeginsatthetimeofcollection.Foracompositesamplecollectedwithanautomatedsampler(e.g.,
usinga24hourcompositesamplersee40CFR122.21(g)(7)(i)or40CFRpart403,AppendixE),theholdingtimebegins
atthetimeoftheendofcollectionofthecompositesample.Forasetofgrabsamplescompositedinthefieldorlaboratory,
theholdingtimebeginsatthetimeofcollectionofthelastgrabsampleintheset.Somesamplesmaynotbestableforthe
maximumtimeperiodgiveninthetable.Apermitteeormonitoringlaboratoryisobligatedtoholdthesampleforashorter
timeifitknowsthatashortertimeisnecessarytomaintainsamplestability.See136.3(e)fordetails.Thedateandtimeof
collectionofanindividualgrabsampleisthedateandtimeatwhichthesampleiscollected.Forasetofgrabsamplestobe
composited,andthatareallcollectedonthesamecalendardate,thedateofcollectionisthedateonwhichthesamplesare
collected.Forasetofgrabsamplestobecomposited,andthatarecollectedacrosstwocalendardates,thedateof
collectionisthedatesofthetwodayse.g.,November1415.Foracompositesamplecollectedautomaticallyonagiven
date,thedateofcollectionisthedateonwhichthesampleiscollected.Foracompositesamplecollectedautomatically,and
thatiscollectedacrosstwocalendardates,thedateofcollectionisthedatesofthetwodayse.g.,November1415.For
staticrenewaltoxicitytests,eachgraborcompositesamplemayalsobeusedtopreparetestsolutionsforrenewalat24h,
48h,and/or72hafterfirstuse,ifstoredat06C,withminimumheadspace.
5ASTMD736509aspecifiestreatmentoptionsforsamplescontainingoxidants(e.g ., chlorine).Also,Section9060Aof
StandardMethodsfortheExaminationofWaterandWastewater(20thand21steditions)addressesdechlorination
procedures.
6Sampling,preservationandmitigatinginterferencesinwatersamplesforanalysisofcyanidearedescribedinASTM
D736509a.TheremaybeinterferencesthatarenotmitigatedbytheanalyticaltestmethodsorD736509a.Anytechnique
forremovalorsuppressionofinterferencemaybeemployed,providedthelaboratorydemonstratesthatitmoreaccurately
measurescyanidethroughqualitycontrolmeasuresdescribedintheanalyticaltestmethod.Anyremovalorsuppression
techniquenotdescribedinD736509aortheanalyticaltestmethodmustbedocumentedalongwithsupportingdata.
7Fordissolvedmetals,filtergrabsampleswithin15minutesofcollectionandbeforeaddingpreservatives.Foracomposite
samplecollectedwithanautomatedsampler(e.g.,usinga24hourcompositesamplersee40CFR122.21(g)(7)(i)or40
CFRPart403,AppendixE),filterthesamplewithin15minutesaftercompletionofcollectionandbeforeadding
preservatives.Ifitisknownorsuspectedthatdissolvedsampleintegritywillbecompromisedduringcollectionofacomposite
samplecollectedautomaticallyovertime(e.g.,byinterchangeofametalbetweendissolvedandsuspendedforms),collect
andfiltergrabsamplestobecomposited(footnote2)inplaceofacompositesamplecollectedautomatically.
8GuidanceappliestosamplestobeanalyzedbyGC,LC,orGC/MSforspecificcompounds.
9IfthesampleisnotadjustedtopH2,thenthesamplemustbeanalyzedwithinsevendaysofsampling.
10ThepHadjustmentisnotrequiredifacroleinwillnotbemeasured.SamplesforacroleinreceivingnopHadjustmentmust
beanalyzedwithin3daysofsampling.
11Whentheextractableanalytesofconcernfallwithinasinglechemicalcategory,thespecifiedpreservativeandmaximum
holdingtimesshouldbeobservedforoptimumsafeguardofsampleintegrity( i.e., useallnecessarypreservativesandhold
fortheshortesttimelisted).Whentheanalytesofconcernfallwithintwoormorechemicalcategories,thesamplemaybe
preservedbycoolingto6C,reducingresidualchlorinewith0.008%sodiumthiosulfate,storinginthedark,andadjusting
thepHto69samplespreservedinthismannermaybeheldforsevendaysbeforeextractionandforfortydaysafter
extraction.Exceptionstothisoptionalpreservationandholdingtimeprocedurearenotedinfootnote5(regardingthe
requirementforthiosulfatereduction),andfootnotes12,13(regardingtheanalysisofbenzidine).
12If1,2diphenylhydrazineislikelytobepresent,adjustthepHofthesampleto4.00.2topreventrearrangementto
benzidine.
13Extractsmaybestoredupto30daysat<0C.
14Fortheanalysisofdiphenylnitrosamine,add0.008%Na2S2O3andadjustpHto710withNaOHwithin24hoursof
sampling.
15ThepHadjustmentmaybeperformeduponreceiptatthelaboratoryandmaybeomittedifthesamplesareextracted
within72hoursofcollection.Fortheanalysisofaldrin,add0.008%Na2S2O3.
16Placesufficienticewiththesamplesintheshippingcontainertoensurethaticeisstillpresentwhenthesamplesarriveat
thelaboratory.However,evenificeispresentwhenthesamplesarrive,immediatelymeasurethetemperatureofthe
samplesandconfirmthatthepreservationtemperaturemaximumhasnotbeenexceeded.Intheisolatedcaseswhereitcan
bedocumentedthatthisholdingtemperaturecannotbemet,thepermitteecanbegiventheoptionofonsitetestingorcan
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requestavariance.Therequestforavarianceshouldincludesupportivedatawhichshowthatthetoxicityoftheeffluent
samplesisnotreducedbecauseoftheincreasedholdingtemperature.Aqueoussamplesmustnotbefrozen.Hand
deliveredsamplesusedonthedayofcollectiondonotneedtobecooledto0to6Cpriortotestinitiation.
17Samplescollectedforthedeterminationoftracelevelmercury(<100ng/L)usingEPAMethod1631mustbecollectedin
tightlycappedfluoropolymerorglassbottlesandpreservedwithBrClorHClsolutionwithin48hoursofsamplecollection.
Thetimetopreservationmaybeextendedto28daysifasampleisoxidizedinthesamplebottle.Asamplecollectedfor
dissolvedtracelevelmercuryshouldbefilteredinthelaboratorywithin24hoursofthetimeofcollection.However,if
circumstancesprecludeovernightshipment,thesampleshouldbefilteredinadesignatedcleanareainthefieldin
accordancewithproceduresgiveninMethod1669.Ifsampleintegritywillnotbemaintainedbyshipmenttoandfiltrationin
thelaboratory,thesamplemustbefilteredinadesignatedcleanareainthefieldwithinthetimeperiodnecessaryto
maintainsampleintegrity.Asamplethathasbeencollectedfordeterminationoftotalordissolvedtracelevelmercurymust
beanalyzedwithin90daysofsamplecollection.
18Aqueoussamplesmustbepreservedat6C,andshouldnotbefrozenunlessdatademonstratingthatsamplefreezing
doesnotadverselyimpactsampleintegrityismaintainedonfileandacceptedasvalidbytheregulatoryauthority.Also,for
purposesofNPDESmonitoring,thespecificationofCisusedinplaceofthe4Cand<4Csampletemperature
requirementslistedinsomemethods.Itisnotnecessarytomeasurethesampletemperaturetothreesignificantfigures
(1/100thof1degree)rather,threesignificantfiguresarespecifiedsothatroundingdownto6Cmaynotbeusedtomeet
the6Crequirement.Thepreservationtemperaturedoesnotapplytosamplesthatareanalyzedimmediately(lessthan
15minutes).
19Anaqueoussamplemaybecollectedandshippedwithoutacidpreservation.However,acidmustbeaddedatleast24
hoursbeforeanalysistodissolveanymetalsthatadsorbtothecontainerwalls.Ifthesamplemustbeanalyzedwithin24
hoursofcollection,addtheacidimmediately(seefootnote2).Soilandsedimentsamplesdonotneedtobepreservedwith
acid.Theallowancesinthisfootnotesupersedethepreservationandholdingtimerequirementsintheapprovedmetals
methods.
20Toachievethe28dayholdingtime,usetheammoniumsulfatebuffersolutionspecifiedinEPAMethod218.6.The
allowanceinthisfootnotesupersedespreservationandholdingtimerequirementsintheapprovedhexavalentchromium
methods,unlessthissupersessionwouldcompromisethemeasurement,inwhichcaserequirementsinthemethodmustbe
followed.
21Holdingtimeiscalculatedfromtimeofsamplecollectiontoelutionforsamplesshippedtothelaboratoryinbulkand
calculatedfromthetimeofsamplefiltrationtoelutionforsamplesfilteredinthefield.
22Sampleanalysisshouldbeginassoonaspossibleafterreceiptsampleincubationmustbestartednolaterthan8hours
fromtimeofcollection.
23Forfecalcoliformsamplesforsewagesludge(biosolids)only,theholdingtimeisextendedto24hoursforthefollowing
sampletypesusingeitherEPAMethod1680(LTBEC)or1681(A1):ClassAcomposted,ClassBaerobicallydigested,and
ClassBanaerobicallydigested.
24Theimmediatefiltrationrequirementinorthophosphatemeasurementistoassessthedissolvedorbioavailableformof
orthophosphorus( i.e., thatwhichpassesthrougha0.45micronfilter),hencetherequirementtofilterthesample
immediatelyuponcollection( i.e., within15minutesofcollection).
[38FR28758,Oct.16,1973]
EditorialNote: ForFederalRegistercitationsaffecting136.3,seetheListof
CFRSectionsAffected,whichappearsintheFindingAidssectionoftheprinted
volumeandat www.fdsys.gov.
https://www.gpo.gov/fdsys/pkg/CFR2014title40vol23/xml/CFR2014title40vol23sec1363.xml 64/64