EPA METHOD 3620B Florisil Cleanup

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1、METHOD3620BFLORISILCLEANUP1.0SCOPEANDAPPLICATION1.1Florisil,aregisteredtradenameofU.S.SilicaCo.,isamagnesiumsilicatewithbasicproperties.Itisusedtoseparateanalytesfrominterferingcompoundspriortosampleanalysisbyachromatographicmethod.1.2Florisilhasbeenusedforthecleanupofpesticideresiduesandotherchlori

2、natedhydrocarbons;theseparationofnitrogencompoundsfromhydrocarbons;theseparationofaromaticcompoundsfromaliphatic-aromaticmixtures;andsimilarapplicationsforusewithfats,oils,andwaxes.Additionally,Florisilisconsideredgoodforseparationswithsteroids,esters,ketones,glycerides,alkaloids,andsomecarbohydrate

3、s.1.3FlorisilcleanupmaybeaccomplishedusingaglasschromatographiccolumnpackedwithFlorisilorusingsolid-phaseextractioncartridgescontainingFlorisil.1.4Thismethodincludesproceduresforcleanupofsampleextractscontainingthefollowinganalytegroups:PhthalateestersChlorinatedhydrocarbonsNitrosaminesOrganochlorin

4、epesticidesNitroaromaticsOrganophosphatesHaloethersOrganophosphoruspesticidesAnilineandanilinederivativesPCBs1.5Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Thismethoddescribespr

5、oceduresforFlorisilcleanupofsolventextractsofenvironmentalsamples.Itprovidestheoptionofusingeithertraditionalcolumnchromatographytechniquestosolid-phaseextractioncartridges.Generally,thetraditionalcolumnchromatographytechniqueuseslargeramountsofadsorbentand,therefore,hasagreatercleanupcapacity.2.2In

6、thecolumncleanupprotocol,thecolumnispackedwiththerequiredamountofadsorbent,toppedwithawateradsorbent,andthenloadedwiththesampleextract.Elutionoftheanalytesiseffectedwithasuitablesolvent(s),leavingtheinterferingcompoundsonthecolumn.Theeluatemaybefurtherconcentratedpriortogaschromatographicanalysis.2.

7、3Thecartridgecleanupprotocolusessolid-phaseextractioncartridgescontaining40µmparticlesofFlorisil(60Dpores).Eachcartridgeiswashedwithsolventimmediatelypriortouse.Thesampleextractisloadedontothecartridg