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1、METHOD3545APRESSURIZEDFLUIDEXTRACTION(PFE)1.0SCOPEANDAPPLICATION1.1Method3545isaprocedureforextractingwaterinsolubleorslightlywatersolubleorganiccompoundsfromsoils,clays,sediments,sludges,andwastesolids.Themethoduseselevatedtemperature(100-180EC)andpressure(1500-2000psi)toachieveanalyterecoverie
2、sequivalenttothosefromSoxhletextraction,usinglesssolventandtakingsignificantlylesstimethantheSoxhletprocedure.Thisprocedurewasdevelopedandvalidatedonacommercially-available,automatedextractionsystem.1.2Thismethodisapplicabletotheextractionofsemivolatileorganiccompounds,organophosphoruspesticides
3、,organochlorinepesticides,chlorinatedherbicides,PCBs,andPCDDs/PCDFs,whichmaythenbeanalyzedbyavarietyofchromatographicprocedures.1.3Thismethodhasbeenvalidatedforsolidmatricescontaining250to12,500µg/kgofsemivolatileorganiccompounds,250to2500µg/kgoforganophosphoruspesticides,5to250µg/kgoforganochlo
4、rinepesticides,50to5000µg/kgofchlorinatedherbicides,1to1400µg/kgofPCBs,and1to2500ng/kgofPCDDs/PCDFs.Themethodmaybeapplicabletosamplescontainingtheseanalytesathigherconcentrationsandmaybeemployedafteradequateperformancehasbeendemonstratedfortheconcentrationsofinterest(seeMethod3500,Sec.8.0).1.4Th
5、ismethodisapplicabletosolidsamplesonly,andismosteffectiveondrymaterialswithsmallparticlesizes.Therefore,wastesamplesmustundergophaseseparation,asdescribedinChapterTwo,andonlythesolidphasematerialistobeextractedbythisprocedure.Ifpossible,soil/sedimentsamplesmaybeair-driedandgroundtoafinepowderpri
6、ortoextraction.Alternatively,ifthelossofanalytesorduringdryingisaconcern,soil/sedimentsamplesmaybemixedwithanhydroussodiumsulfateorpelletizeddiatomaceousearth.(DryingandgrindingsamplescontainingPCDDs/PCDFsisnotrecommended,duetosafetyconcerns).Thetotalmassofmaterialtobeprepareddependsonthespecifi
7、cationsofthedeterminativemethodandthesensitivityrequiredfortheanalysis,but10-30gofmaterialareusuallynecessaryandcanbeaccommodatedbythisextractionprocedure.1.5Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalyst
