EPA METHOD 3611B Alumina Column Cleanup and Separation of Petroleum Wastes

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1、METHOD3611BALUMINACOLUMNCLEANUPANDSEPARATIONOFPETROLEUMWASTES1.0SCOPEANDAPPLICATION1.1Aluminaisahighlyporousandgranularformofaluminumoxide.ItisavailableinthreepHranges(basic,neutral,andacidic)foruseinchromatographiccleanupprocedures.Method3611utilizesneutralpHaluminatosepara

2、tepetroleumwastesintoaliphatic,aromatic,andpolarfractions.1.2Method3611wasformerlyMethod3570intheSecondEditionofthismanual.1.3Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0

3、SUMMARYOFMETHOD2.1Thecolumnispackedwiththerequiredamountofadsorbent,toppedwithawateradsorbent,andthenloadedwiththesampletobeanalyzed.Elutionoftheanalytesiseffectedwithasuitablesolvent(s),leavingtheinterferingcompoundsonthecolumn.Theeluateisthenconcentrated(ifnecessary).3.0IN

4、TERFERENCES3.1Areagentblankshouldbeperformedforthecompoundsofinterestpriortotheuseofthismethod.Thelevelofinterferencesmustbebelowthemethoddetectionlimitbeforethismethodisperformedonactualsamples.3.2Moreextensiveproceduresthanthoseoutlinedinthismethodmaybenecessaryforreagentp

5、urification.3.3Cautionmustbetakentopreventoverloadingofthechromatographiccolumn.Asthecolumnloadingforanyofthesetypesofwastesapproaches0.300gofextractableorganics,separationrecoverieswillsuffer.Ifoverloadingissuspected,analiquotofthebase-neutralextractpriortocleanupmaybeweigh

6、edandthenevaporatedtodryness.Agravimetricdeterminationonthealiquotwillindicatetheweightofextractableorganicsinthesample.3.4Mixturesofpetroleumwastescontainingpredominantlypolarsolvents,i.e.,chlorinatedsolventsoroxygenatedsolvents,arenotappropriateforthismethod.4.0APPARATUSAN

7、DMATERIALS4.1Chromatographycolumn:300mmx10mmID,withPyrex®glasswoolatbottomandapolytetrafluoroethylene(PTFE)stopcock.NOTE:Frittedglassdiscsaredifficulttodecontaminateafterhighlycontaminatedextractshavebeenpassedthrough.Columnswithoutfritsmaybepurchased.UseasmallpadofPyrex®gla

8、sswooltoretaintheadsorbent.PrewashtheCD-ROM3611B-1Revision2December1996glas