EPA Method 554 Determination of Carbonyl Compounds in Drinking Water

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1、METHOD554DETERMINATIONOFCARBONYLCOMPOUNDSINDRINKINGWATERBYDINITROPHENYLHYDRAZINEDERIVATIZATIONANDHIGHPERFORMANCELIQUIDCHROMATOGRAPHYRevision1.0August1992JamesW.EichelbergerW.J.Bashe(TechnologyApplications,Incorporated)ENVIRONMENTALMONITORINGSYSTEMSLABORATORYOFFICEOFRES

2、EARCHANDDEVELOPMENTU.S.ENVIRONMENTALPROTECTIONAGENCYCINCINNATI,OHIO45268554-1METHOD554DETERMINATIONOFCARBONYLCOMPOUNDSINDRINKINGWATERBYDINITROPHENYLHYDRAZINEDERIVATIZATIONANDHIGHPERFORMANCELIQUIDCHROMATOGRAPHY(HPLC)1.0SCOPEANDAPPLICATION1.1Thisisahighperformanceliquidc

3、hromatographic(HPLC)methodoptimizedforthedeterminationofselectedcarbonylcompoundsinfinisheddrinkingwaterandrawsourcewater.TheanalytesapplicabletothismethodarepartitionedfromthewaterontoareversephaseCbondedsilicapacked18cartridge,thenelutedwithethanol.Liquid-solidextrac

4、tiondisksmayalsobeusedforthispurpose.Single-laboratoryaccuracyandprecisiondatahavebeengeneratedforthefollowingcompounds:ChemicalAbstractServicesAnalyteRegistryNumberFormaldehyde50-00-0Acetaldehyde75-07-0Propanal123-38-6Butanal123-72-8Pentanal110-62-3Hexanal66-25-1Hepta

5、nal111-71-7Octanal124-13-0Nonanal124-19-6Decanal112-31-2Cyclohexanone108-94-1Crotonaldehyde123-73-91.2Themethoddetectionlimits(MDLs)fortheanalytesarelistedinTables1and2.TheMDLisdefinedasthestatisticallycalculatedminimumamountthatcanbemeasuredwith99%confidencethattherep

6、ortedvalueisgreaterthan1zero.TheMDLsforaspecificsamplemaydifferfromthatofthestandardmatrixandbythevolumeofsampleusedintheprocedure.Forthelistedanalytes,MDLsrangefrom3.0-69.0µg/L.1.3ThismethodisrestrictedtousebyorunderthesupervisionofanalystsexperiencedintheuseofHPLCand

7、intheinterpretationofchromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod,usingtheproceduredescribedinSection11.0.554-22.0SUMMARYOFMETHOD2.1Ameasuredvolumeofaqueoussample,approximately100mL,isbufferedtopH3andtheanalytesarederivati

8、zedat40°Cforonehourwith2,4-dinitrophenylhydrazine(DNPH).Thederivativesareextractedfromthewaterbypassingthesamplethrou