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1、CDROM83161Revision0September1994METHOD8316ACRYLAEACRYLONITRILEACROLEINBYHIGHPERFMANCELIQUIDCHROMATOGRAPHY(HPLC)1.0SCOPEAPPLICATION1.1Thefollowingcompoundscanbedeterminedbythismethod:______________________________________

2、______________________________CompoundNameCASNo.aAcrylae79061Acrylonitrile107131Acrolein(Propenal)107028____________________________________________________________________ChemicalAbstractServicesRegistryNumber.a1.2Theme

3、thoddetectionlimits(MDLs)fthetargetanalytesinganicfreereagentwaterarelistedinTable1.Themethodmaybeapplicabletoothermatrices.1.3Thismethodisrestrictedtousebyunderthesupervisionofanalystsexperiencedintheuseofhighperfmancel

4、iquidchromatographsskilledintheinterpretationofhighperfmanceliquidchromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Watersamplesareanalyzedbyhighperfmanceliq

5、uidchromatography(HPLC).A200LaliquotisinjectedontoaC18reversephasecolumncompoundsintheeffluentaredetectedwithanultraviolet(UV)detect.3.0INTERFERENCES3.1Contaminationbycarryovercanoccurwheneverhighconcentrationlowconcentr

6、ationsamplesaresequentiallyanalyzed.Toreducecarryoverthesamplesyringemustberinsedoutbetweensampleswithsolvent.Wheneveranunusuallyconcentratedsampleisencountereditshouldbefollowedbytheanalysisofsolventtocheckfcrosscontami

7、nation.CDROM83163Revision0September19945.5ganicfreereagentwater.AllreferencestowaterinthismethodrefertoganicfreereagentwaterasdefinedinChapterOne.SpargewithHetoeliminateOtopreventsignificantabsptioninterferencefromOatthe

8、19522nmwavelength.5.6StockstardsolutionsCanbepreparedfrompurestardmaterialscanbepurchasedascertifiedsolutions.Commerciallypreparedstockstardscanbeusediftheyarecertifiedbythemanufacturerverifiedagainstastardmadefrompurema

9、terial.5.6.1Acrylae5.6.1.1Weigh0.0100gofacrylaeneatstardintoa100mLvolumetricflaskdilutetothemarkwithganicfreereagentwater.Calculatetheconcentrationofthestardsolutionfromtheactualweightused.Whencompoundpurityisassayedtobe

10、96%greatertheweightcanbeusedwithoutcrectiontocalculatetheconcentrationofthestockstard.5.6.1.2TransferthestocksolutionintovialswithTeflonlinedscrewcapscrimptops.Steat4Cprotectedfromlight.o5.6.1.3Stocksolutionsmustbereplac

11、edaftersixmonthssoonerifcomparisonwiththecheckstardsindicatesaproblem.5.6.2AcrylonitrileAcroleinPrepareseparatestocksolutionsfacrylonitrileacrolein.5.6.2.1Placeabout9.8mLofganicfreereagentwaterintoa10mLvolumetricflaskbef

12、eweighingtheflaskstopper.Weightheflaskrecdtheweighttothenearest0.0001g.Addtwosofneatstardusinga50Lsyringetotheflask.Theliquidmustfalldirectlyintothewaterwithoutcontactingtheinsidewalloftheflask.CAUTION:Acrylonitrileacrol

13、einaretoxic.Stardpreparationshouldbeperfmedinanlabatyfumehood.5.6.2.2Stoppertheflaskthenreweigh.Dilutetovolumewithganicfreereagentwater.Calculatetheconcentrationfromthegaininweight.Whencompoundpurityisassayedtobe96%great

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