EPA Method 549.1 Determination of Diquat and Paraquat in Drinking Water

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1、METHOD549.1DETERMINATIONOFDIQUATANDPARAQUATINDRINKINGWATERBYLIQUID-SOLIDEXTRACTIONANDHIGHPERFORMANCELIQUIDCHROMATOGRAPHYWITHULTRAVIOLETDETECTIONRevision1.0August1992J.W.HodgesonW.J.Bashe(TechnologyApplicationsInc.)JamesW.EichelbergerENVIRONMENTALMONITORIN

2、GSYSTEMSLABORATORYOFFICEOFRESEARCHANDDEVELOPMENTU.S.ENVIRONMENTALPROTECTIONAGENCYCINCINNATI,OHIO45268549.1-1METHOD549.1DETERMINATIONOFDIQUATANDPARAQUATINDRINKINGWATERBYLIQUID-SOLIDEXTRACTIONANDHIGHPERFORMANCELIQUIDCHROMATOGRAPHYWITHULTRAVIOLETDETECTION1.0

3、SCOPEANDAPPLICATION1.1Thisisahighperformanceliquidchromatography(HPLC)methodforthedeterminationofdiquat(1,1©-ethylene-2,2©-bipyridiliumdibromidesalt)andparaquat(1,1©-dimethyl-4,4©-bipyridiliumdichloridesalt)indrinkingwater1,2sourcesandfinisheddrinkingwate

4、r.ChemicalAbstractServicesRegistryAnalyteNumberDiquat85-00-7Paraquat1910-42-51.2Whenthismethodisusedtoanalyzeunfamiliarsamples,compoundidentificationshouldbesupportedbyatleastoneadditionalqualitativetechnique.Theuseofaphotodiodearraydetectorprovidesultrav

5、ioletspectrathatcanbeusedforthequalitativeconfirmation.1.3Themethoddetectionlimits(MDL,definedinSect.13)(3)fordiquatandparaquatarelistedinTable1.1.4ThismethodisrestrictedtousebyorunderthesupervisionofanalystsexperiencedintheuseofHPLC.Eachanalystmustdemons

6、tratetheabilitytogenerateacceptableresultswiththismethodusingtheproceduredescribedinSect.9.3.2.SUMMARYOFMETHOD2.1Ameasuredvolumeofliquidsample,approximately250mL,isadjustedtopH10.5.ThesampleisextractedusingaCsolidsorbentcartridgeoraC-88diskwhichhasbeenspe

7、ciallypreparedforthereversed-phase,ion-pairmode.Thediskorcartridgeiselutedwith4.5mLofanacidicaqueoussolvent.Aftertheion-pairreagentisaddedtotheeluate,thefinalvolumeisadjustedto5.0mL.Liquidchromatographicconditionsaredescribedwhichpermittheseparationandmea

8、surementofdiquatandparaquatintheextractbyabsorbancedetectionat308nmand257nm,respectively.Aphotodiodearraydetectorisutilizedtoprovidesimultaneousdetectionandconfirmationofthe1,2methodanalytes.549.1-22.2Analysisofdiqu