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1、METHOD3545PRESSURIZEDFLUIDEXTRACTION(PFE)1.0SCOPEANDAPPLICATION1.1Method3545isaprocedureforextractingwaterinsolubleorslightlywatersolublesemivolatileorganiccompoundsfromsoils,clays,sediments,sludges,andwastesolids.Themethoduseselevatedtemperature(100EC)andpressure(1500-2000psi)toachie
2、veanalyterecoveriesequivalenttothosefromSoxhletextraction,usinglesssolventandtakingsignificantlylesstimethantheSoxhletprocedure.Thisprocedurewasdevelopedandvalidatedonacommercially-available,automatedextractionsystem.1.2Thismethodisapplicabletotheextractionofsemivolatileorganiccompoun
3、ds,organophosphoruspesticides,organochlorinepesticides,chlorinatedherbicides,andPCBs,whichmaythenbeanalyzedbyavarietyofchromatographicprocedures.1.3Thismethodhasbeenvalidatedforsolidmatricescontaining250to12,500µg/kgofsemivolatileorganiccompounds,250to2500µg/kgoforganophosphoruspestic
4、ides,5to250µg/kgoforganochlorinepesticides,50to5000µg/kgofchlorinatedherbicides,and1to1400µg/kgofPCBs.Themethodmaybeapplicabletosamplescontainingtheseanalytesathigherconcentrationsandmaybeemployedafteradequateperformancehasbeendemonstratedfortheconcentrationsofinterest(seeMethod3500,S
5、ec.8.0).1.4Thismethodisapplicabletosolidsamplesonly,andismosteffectiveondrymaterialswithsmallparticlesizes.Therefore,wastesamplesmustundergophaseseparation,asdescribedinChapterTwo,andonlythesolidphasematerialistobeextractedbythisprocedure.Ifpossible,soil/sedimentsamplesmaybeair-drieda
6、ndgroundtoafinepowderpriortoextraction.Alternatively,ifthelossofanalytesduringdryingisaconcern,soil/sedimentsamplesmaybemixedwithanhydroussodiumsulfateorpelletizeddiatomaceousearth.Thetotalmassofmaterialtobeprepareddependsonthespecificationsofthedeterminativemethodandthesensitivityreq
7、uiredfortheanalysis,but10-30gofmaterialareusuallynecessaryandcanbeaccommodatedbythisextractionprocedure.1.5Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Samplesarep
8、repar
