EPA METHOD 3540C Soxhlet Extraction

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1、METHOD3540CSOXHLETEXTRACTION1.0SCOPEANDAPPLICATION1.1Method3540isaprocedureforextractingnonvolatileandsemivolatileorganiccompoundsfromsolidssuchassoils,sludges,andwastes.TheSoxhletextractionprocessensuresintimatecontactofthesamplematrixwiththeextractionsolvent.1.2Thismethodi

2、sapplicabletotheisolationandconcentrationofwater-insolubleandslightlywatersolubleorganicsinpreparationforavarietyofchromatographicprocedures.1.3Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilitytogenerateacceptableresults

3、withthismethod.2.0SUMMARYOFMETHOD2.1Thesolidsampleismixedwithanhydroussodiumsulfate,placedinanextractionthimbleorbetweentwoplugsofglasswool,andextractedusinganappropriatesolventinaSoxhletextractor.2.2Theextractisthendried,concentrated(ifnecessary),and,asnecessary,exchangedin

4、toasolventcompatiblewiththecleanupordeterminativestepbeingemployed.3.0INTERFERENCESRefertoMethod3500.4.0APPARATUSANDMATERIALS4.1Soxhletextractor-40mmID,with500-mLroundbottomflask.4.2Dryingcolumn-20mmIDPyrex®chromatographiccolumnwithPyrex®glasswoolatbottom.NOTE:Frittedglassdi

5、scsaredifficulttodecontaminateafterhighlycontaminatedextractshavebeenpassedthrough.Columnswithoutfritsmaybepurchased.UseasmallpadofPyrex®glasswooltoretaintheadsorbent.Prewashtheglasswoolpadwith50mLofacetonefollowedby50mLofelutionsolventpriortopackingthecolumnwithadsorbent.4.

6、3Kuderna-Danish(K-D)apparatus4.3.1Concentratortube-10-mL,graduated(KontesK-570050-1025orequivalent).Aground-glassstopperisusedtopreventevaporationofextracts.CD-ROM3540C-1Revision3December19964.3.2Evaporationflask-500-mL(KontesK-570001-500orequivalent).Attachtoconcentratortub

7、ewithsprings,clamps,orequivalent.4.3.3Snydercolumn-Three-ballmacro(KontesK-503000-0121orequivalent).4.3.4Snydercolumn-Two-ballmicro(KontesK-569001-0219orequivalent).4.3.5Springs-1/2inch(KontesK-662750orequivalent).NOTE:Thefollowingglasswareisrecommendedforthepurposeofsolvent

8、recoveryduringtheconcentrationproceduresrequiringtheuseofKuderna-Danishevap