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1、METHOD8316ACRYLAMIDE,ACRYLONITRILEANDACROLEINBYHIGHPERFORMANCELIQUIDCHROMATOGRAPHY(HPLC)1.0SCOPEANDAPPLICATION1.1Thefollowingcompoundscanbedeterminedbythismethod:____________________________________________________________________aCompoundNameCASNo.Acrylamide79-06-1Acrylonitri
2、le107-13-1Acrolein(Propenal)107-02-8____________________________________________________________________aChemicalAbstractServicesRegistryNumber.1.2Themethoddetectionlimits(MDLs)forthetargetanalytesinorganic-freereagentwaterarelistedinTable1.Themethodmaybeapplicabletoothermatri
3、ces.1.3Thismethodisrestrictedtousebyorunderthesupervisionofanalystsexperiencedintheuseofhighperformanceliquidchromatographsandskilledintheinterpretationofhighperformanceliquidchromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARY
4、OFMETHOD2.1Watersamplesareanalyzedbyhighperformanceliquidchromatography(HPLC).A200µLaliquotisinjectedontoaC-18reverse-phasecolumn,andcompoundsintheeffluentaredetectedwithanultraviolet(UV)detector.3.0INTERFERENCES3.1Contaminationbycarryovercanoccurwheneverhigh-concentrationandl
5、ow-concentrationsamplesaresequentiallyanalyzed.Toreducecarryover,thesamplesyringemustberinsedoutbetweensampleswithsolvent.Wheneveranunusuallyconcentratedsampleisencountered,itshouldbefollowedbytheanalysisofsolventtocheckforcrosscontamination.CD-ROM8316-1Revision0September19944
6、.0APPARATUSANDMATERIALS4.1HPLCsystem4.1.1Onehighpressurepump.4.1.2OctadecylSilane(ODS,C-18)reversephaseHPLCcolumn,25cmx4.6mm,10µm,(Zorbax,orequivalent).4.1.3VariablewavelengthUVdetector.4.1.4Datasystem.4.2Otherapparatus4.2.1Waterdegassingunit-1literfilterflaskwithstopperandpre
7、ssuretubing.4.2.2Analyticalbalance-+0.0001g.4.2.3Magneticstirrerandmagneticstirringbar.4.2.4Samplefiltrationunit-syringefilterwith0.45µmfiltermembrane,orequivalentdisposablefilterunit.4.3Materials4.3.1Syringes-10,25,50and250µLand10mL.4.3.2Volumetricpipettes,ClassA,glass-1,5and
8、10mL.4.3.3Volumetricflasks-5,10,50and100mL.4.3.4Vials-25mL,gl