美国环保局-EPA--试验--方法-551-1

551.1-1METHOD551.1DETERMINATIONOFCHLORINATIONDISINFECTIONBYPRODUCTS,CHLORINATEDSOLVENTS,ANDHALOGENATEDPESTICIDES/HERBICIDESINDRINKINGWATERBYLIQUID-LIQUIDEXTRACTIONANDGASCHROMATOGRAPHYWITHELECTRON-CAPTUREDETECTIONRevision1.0J.W.Hodgeson,A.L.Cohen-Method551,(1990)D.J.Munch(USEPA,OfficeofWater)andD.P.Hautman(InternationalConsultants,Inc.)-Method551.1,(1995)NATIONALEXPOSURERESEARCHLABORATORYOFFICEOFRESEARCHANDDEVELOPMENTU.S.ENVIRONMENTALPROTECTIONAGENCYCINCINNATI,OHIO45268551.1-2METHOD551.1DETERMINATIONOFCHLORINATIONDISINFECTIONBYPRODUCTS,CHLORINATEDSOLVENTS,ANDHALOGENATEDPESTICIDES/HERBICIDESINDRINKINGWATERBYLIQUID-LIQUIDEXTRACTIONANDGASCHROMATOGRAPHYWITHELECTRON-CAPTUREDETECTION1.0SCOPEANDAPPLICATION1.1Thismethodisapplicabletothedeterminationofthefollowinganalytesin1-9finisheddrinkingwater,drinkingwaterduringintermediatestagesoftreatment,andrawsourcewater.Theparticularchoiceofanalytesfromthislistshouldbeafunctionofthespecificprojectrequirements.AnalyteCASNo.DisinfectionByproducts(DBPs):TrihalomethanesChloroform67-66-3Bromodichloromethane75-27-4Bromoform75-25-2Dibromochloromethane124-48-1HaloacetonitrilesBromochloroacetonitrile83463-62-1Dibromoacetonitrile3252-43-5Dichloroacetonitrile3018-12-0Trichloroacetonitrile545-06-2OtherDBPsChloralHydrate75-87-6Chloropicrin76-06-21,1-Dichloro-2-propanone513-88-21,1,1-Trichloro-2-propanone918-00-3ChlorinatedSolvents:CarbonTetrachloride56-23-51,2-Dibromo-3-chloropropane[DBCP]96-12-81,2-Dibromoethane[EDB]106-93-4Tetrachloroethylene127-18-41,1,1-Trichloroethane71-55-61,1,2-Trichloroethane79-00-5Trichloroethylene79-01-61,2,3-Trichloropropane96-18-4Pesticides/Herbicides:Alachlor15972-60-8Atrazine1912-24-9Bromacil314-40-9Cyanazine21725-46-2Endrin72-20-8AnalyteCASNo.551.1-3EndrinAldehyde7421-93-4EndrinKetone53494-70-5Heptachlor76-44-8HeptachlorEpoxide1024-57-3Hexachlorobenzene118-74-1Hexachlorocyclopentadiene77-47-4Lindane(gamma-BHC)58-89-9Metolachlor51218-45-2Metribuzin21087-64-9Methoxychlor72-43-5Simazine122-34-9Trifluralin1582-09-81.2Thisanalytelistincludes12commonlyobservedchlorinationdisinfectionbyproducts,eightcommonlyusedchlorinatedorganicsolventsand3,416halogenatedpesticidesandherbicides.1.3Thismethodisintendedasastand-aloneprocedureforeithertheanalysisofonlythetrihalomethanes(THMs)orforallthechlorinationdisinfectionby-products(DBPs)withthechlorinatedorganicsolventsorasaprocedureforthetotalanalytelist.Thedechlorination/preservationtechniquepresentedinSection8.0detailstwodifferentdechlorinatingagents.ResultsfortheTHMsandtheeightsolventsmaybeobtainedfromtheanalysisofsamplesemployingeitherdechlorinatingagent.(Section8.1.2)1.4AfterananalytehasbeenidentifiedandquantitatedinanunknownsamplewiththeprimaryGCcolumn(Section6.9.2.1)qualitativeconfirmationofresultsisstronglyrecommendedbygaschromatography/massspectrometry(GC/MS),orbyGCanalysisusingadissimilarcolumn(Section6.9.2.2).10,111.5Theexperimentallydeterminedmethoddetectionlimits(MDLs)fortheabove12listedanalytesareprovidedinTables2and8.ActualMDLvalueswillvaryaccordingtotheparticularmatrixanalyzedandthespecificinstrumentationemployed.1.6ThismethodisrestrictedtousebyorunderthesupervisionofanalystsexperiencedintheuseofGCandintheinterpretationofgaschromatograms.EachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethodusingtheproceduredescribedinSection9.4.1.7Methyl-t-butylether(MTBE)isrecommendedastheprimaryextractionsolventinthismethodsinceiteffectivelyextractsallofthetargetanalyteslistedinSection1.1.However,duetosafetyconcernsassociatedwithMTBEandthecurrentuseofpentanebysomelaboratoriesforcertainmethodanalytes,pentaneisofferedasanoptionalextractionsolventforallanalytesexcept551.1-4chloralhydrate.Ifprojectrequirementsspecifytheanalysisofchloralhydrate,MTBEmustbeusedastheextractingsolvent.Thismethodincludessectionsspecificforpentaneasanoptionalsolvent.2.0SUMMARYOFMETHOD2.1A50mLsamplealiquotisextractedwith3mLofMTBEor5mLofpentane.TwoμLoftheextractistheninjectedintoaGCequippedwithafusedsilicacapillarycolumnandlinearizedelectroncapturedetectorforseparationandanalysis.Proceduralstandardcalibrationisusedtoquantitatemethodanalytes.2.2Atypicalsamplecanbeextractedandanalyzedbythismethodin50minutesforthechlorinationby-products/chlorinatedsolventsandtwohoursforthetotalanalytelist.Confirmationoftheelutedcompoundsmaybeobtainedusingadissimilarcolumn(Section6.9.2.2)orbytheuseofGC-MS.Simultaneousconfirmationcanbeperformedusingdualprimary/confirmationcolumnsinstalledinasingleinjectionport(Section6.9.3)oraseparateconfirmationanalysis.3.0DEFINITIONS3.1InternalStandard(IS)--Apureanalyte(s)addedtoasample,extract,orstandardsolutioninknownamount(s)andusedtomeasuretherelativeresponsesofothermethodanalytesandsurrogatesthatarecomponentsofthesamesampleorsolution.Theinternalstandardmustbeananalytethatisnotasamplecomponent.3.2SurrogateAnalyte(SA)--Apureanalyte(s),whichisextremelyunlikelytobefoundinanysample,andwhichisaddeddirectlytoasamplealiquotinknownamount(s)beforeextractionorotherprocessingandismeasuredwiththesameproceduresusedtomeasure