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1、METHOD3665ASULFURICACID/PERMANGANATECLEANUP1.0SCOPEANDAPPLICATION1.1Thismethodissuitablefortherigorouscleanupofsampleextractspriortoanalysisforpolychlorinatedbiphenyls.ThismethodshouldbeusedwheneverelevatedbaselinesoroverlycomplexchromatogramspreventaccuratequantitationofPCBs.Thismet
2、hodcannotbeusedtocleanupextractsforothertargetanalytes,asitwilldestroymostorganicchemicalsincludingthepesticidesAldrin,Dieldrin,Endrin,Endosulfan(IandII),andEndosulfansulfate.1.2Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilityto
3、generateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Anextractissolventexchangedtohexane,thenthehexaneissequentiallytreatedwith(1)concentratedsulfuricacidand,ifnecessary,(2)5%aqueouspotassiumpermanganate.Appropriatecautionmustbetakenwiththesecorrosivereagents.2.2Blanksandrepl
4、icateanalysissamplesmustbesubjectedtothesamecleanupasthesamplesassociatedwiththem.2.3Itisimportantthatalltheextractsbeexchangedtohexanebeforeinitiatingthefollowingtreatments.3.0INTERFERENCES3.1Thistechniquewillnotdestroychlorinatedbenzenes,chlorinatednaphthalenes(Halowaxes),andanumbe
5、rofchlorinatedpesticides.4.0APPARATUS4.1SyringeorClassAvolumetricpipet,glass;1.0,2.0and5.0mL.4.2Vials-1,2and10mL,glasswithpolytetrafluoroethylene(PTFE)-linedscrewcapsorcrimptops.4.3Vortexmixer.5.0REAGENTS5.1Reagentgradeinorganicchemicalsshallbeusedinalltests.Unlessotherwiseindicated,
6、itisintendedthatallreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.OthergradesCD-ROM3665A-1Revision1December1996maybeused,provideditisfirstascertainedthatthereagentisofsufficientlyhighpuritytope
7、rmititsusewithoutlesseningtheaccuracyofthedetermination.5.2Organic-freereagentwater.Allreferencestowaterinthismethodrefertoorganic-freereagentwater,asdefinedinChapterOne.5.3Sulfuricacid/Water,H2SO4/H2O(1:1,v/v).5.4Hexane,C6H14-Pesticidegradeorequivalent.5.5Potassiumpermanganate,KMnO4
8、,5percentaqu
