EPA Method 548 Determination of Endothall in Drinking Water

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1、Method548DeterminationofEndothallinDrinkingWaterbyAqueousDerivatization,Liquid-SolidExtraction,andGasChromatographywithElectron-CaptureDetectionJuly1990ÐEPAEMSL-CiJ.W.HodgesonMethod548DeterminationofEndothallinDrinkingWaterbyAqueousDerivatization,Liquid-SolidExt

2、raction,andGasChromatographywithElectron-CaptureDetection1.ScopeandApplication1.1Thismethodcoversthedeterminationofendothallindrinkingwatersourcesandfinisheddrinkingwater.Thefollowinganalytecanbedeterminebythismethod:AnalyteCASNo.Endothall145-73-31.2Thisisagasch

3、romatographic(GC)methodapplicabletothedeterminationofthecompoundlistedabove.Whenthismethodisusedtoanalyzeunfamiliarsamples,compoundidentificationshouldbesupportedbyatleastoneadditionalqualitativetechnique.Agaschromatograph/massspectrometer(GC/MS)maybeusedfortheq

4、ualitativeconfirmationofresultsforEndothallusingtheextractproducedbythismethod.11.3Themethoddetectionlimit(MDL,definedinSection12)forendothallislistedinTable1.TheMDLforaspecificsamplemaydifferfromthelistedvalue,dependinguponthenatureofinterferencesinthesamplemat

5、rixandtheamountofsampleusedintheprocedure.1.4Anymodificationofthismethodbeyondthoseexpresslypermitted,shallbeconsideredamajormodificationsubjecttoapplicationandapprovalofalternatetestproceduresunder40CFR136.4and136.5.1.5Thismethodisrestrictedtousebyorunderthesup

6、ervisionofanalystsexperiencedintheuseofgaschromatographyandintheinterpretationofgaschromatograms.EachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethodusingtheproceduredescribedinSection11.2.SummaryofMethod2.1A5.0mLvolumeofliquidsampleispl

7、acedinaKuderna-Danishtubeandthevolumeisreducedtolessthan0.75mLusingaheatingblock.Thetubeischargedwithglacialaceticacidandsodiumacetate,followedbyasolutionofthederivatizationreagent,pentafluorophenylhydrazine(PFPH),inglacialaceticacid.Afterheatingat150°Cfor90minu

8、testhederivativeisextractedbyasolidsorbentfromthereactionsolution,followedbyelutionwith5.0mLofmethyl-tert-butylether(MTBE).TheMTBEextractisanalyzedbygaschromatography