EPA method 8032a ACRYLAMIDE BY GAS CHROMATOGRAPHY

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1、METHOD8032AACRYLAMIDEBYGASCHROMATOGRAPHY1.0SCOPEANDAPPLICATION1.1Method8032isusedtodeterminetraceamountsofacrylamidemonomer(CASNo.79-06-1)inaqueousmatrices.Thismethodmaybeapplicabletoothermatricesandtoothersimilaranalytes.1.2Themethoddetectionlimit(MDL)inanaqueousmatrixis0.032µg/L.1.3Thismeth

2、odisrestrictedforuseby,orunderthesupervisionof,analystsexperiencedintheuseofgaschromatographsandskilledintheinterpretationofgaschromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Method8032isbasedonbrominationoftheacrylamidedoublebo

3、nd.Thereactionproduct(2,3-dibromopropionamide)isextractedfromthereactionmixturewithethylacetate,aftersaltingoutwithsodiumsulfate.TheextractiscleanedupusingaFlorisilcolumn,andanalyzedbygaschromatographywithelectroncapturedetection(GC/ECD).2.2Compoundidentificationshouldbesupportedbyatleastonea

4、dditionalqualitativetechnique.Analysisusingasecondgaschromatographiccolumnorgaschromatography/massspectrometrymaybeusedforcompoundconfirmation.3.0INTERFERENCES3.1Nointerferenceisobservedfromseawaterorinthepresenceof8.0%ofammoniumionsderivedfromammoniumbromide.3.2Impuritiesfrompotassiumbromide

5、areremovedbytheFlorisilcleanupprocedure.4.0APPARATUSANDMATERIALS4.1Gaschromatographicsystem4.1.1Gaschromatographsuitableforon-columninjectionswithallrequiredaccessories,includingdetector,analyticalcolumns,recorder,gases,andsyringes.Adatasystemformeasuringpeakheightsand/orpeakareasisrecommende

6、d.4.1.2GCColumn-2mx3mmglasscolumn,5%FFAP(freefattyacidpolyester)on60-80meshacidwashedChromosorbW,orequivalent.4.1.3Detector-electroncapturedetector.4.2Separatoryfunnel-150-mL.CD-ROM8032A-1Revision1December19964.3Volumetricflask(ClassA)-100-mL,withground-glassstopper;25-mL,amber,withground-gla

7、ssstopper.4.4Syringe-5-mL.4.5Microsyringes-5-µL,100-µL.4.6Pipets(ClassA).4.7Glasschromatographycolumn(30cmx2cm).4.8Mechanicalshaker.5.0REAGENTS5.1Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,itisintendedthatallreagentss