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1、METHOD3546MICROWAVEEXTRACTION1.0SCOPEANDAPPLICATION1.1Method3546isaprocedureforextractingwaterinsolubleorslightlywatersolubleorganiccompoundsfromsoils,clays,sediments,sludges,andsolidwastes.Themethodwasdevelopedandvalidatedoncommercially-availablesolventex
2、tractionsystems.Theprocedureusesmicrowaveenergytoproduceelevatedtemperatureandpressureconditions(i.e.,100-115ECand50-175psi)inaclosedvesselcontainingthesampleandorganicsolvent(s)toachieveanalyterecoveriesequivalenttothosefromSoxhletextraction(Method3540),u
3、singlesssolventandtakingsignificantlylesstimethantheSoxhletprocedure.Othersystemsandothertypesofvesselsmaybeused,providedthattheanalystcandemonstrateappropriateperformanceforaspecificapplication.1.2Thismethodisapplicabletotheextractionofsemivolatileorganic
4、compounds,organophosphoruspesticides,organochlorinepesticides,chlorinatedherbicides,phenoxyacidherbicides,substitutedphenols,PCBs,andPCDDs/PCDFs,whichmaythenbeanalyzedbyavarietyofchromatographicprocedures.Themethodmayalsobeapplicablefortheextractionofaddit
5、ionaltargetanalytes,providedthattheanalystdemonstratesadequateperformancefortheintendedapplication(seeMethod3500andChapterTwo).1.3Thismethodhasbeenvalidatedforsolidmatricescontaining50to10,000µg/kgofsemivolatileorganiccompounds,250to2,500µg/kgoforganophosp
6、horuspesticides,10to5,000µg/kgoforganochlorinepesticidesandchlorinatedherbicides,50to2,500µg/kgofsubstitutedphenols,100to5,000µg/kgofphenoxyacidherbicides,1to5,000µg/kgofPCBs,and10to6000ng/kgofPCDDs/PCDFs.Themethodmaybeapplicabletosamplescontainingtheseana
7、lytesathigherconcentrationsandmaybeemployedafteradequateperformancehasbeendemonstratedfortheconcentrationsofinterest(seeMethod3500).1.4Thismethodonlyisapplicabletosolidsampleswithsmallparticlesizes.Ifpractical,soil/sedimentsamplesmaybeair-driedandgroundtoa
8、finepowderpriortoextraction.Alternatively,ifworkersafetyorthelossofanalytesduringdryingisaconcern,soil/sedimentsamplesmaybemixedwithanhydroussodiumsulfateorpelletizeddiatomaceousearth.Thetotalmassofmaterialto