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1、METHOD547DETERMINATIONOFGLYPHOSATEINDRINKINGWATERBYDIRECT-AQUEOUS-INJECTIONHPLC,POST-COLUMNDERIVATIZATION,ANDFLUORESCENCEDETECTIONJuly1990T.W.WinfieldW.J.Bashe(TechnologyApplicationsInc.)T.V.Baker(TechnologyApplicationsInc.)ENVIRONMENTALMONITORINGSYSTEMSLABORATORYOFFICEOFRESEARCHANDD
2、EVELOPMENTU.S.ENVIRONMENTALPROTECTIONAGENCYCINCINNATI,OHIO45268METHOD547DETERMINATIONOFGLYPHOSATEINDRINKINGWATERBYDIRECT-AQUEOUS-INJECTIONHPLC,POST-COLUMNDERIVATIZATION,ANDFLUORESCENCEDETECTION1.0SCOPEANDAPPLICATION1.1ThismethoddescribesaprocedurefortheidentificationandmeasurementofG
3、lyphosate(N-phosphonomethylglycine)indrinkingwatermatrices.Singlelaboratoryaccuracyandprecisiondatahavebeendeterminedforthismethod.11.2Glyphosatewasfoundtorapidlydecomposeinchlorinatedwaters.ItisthereforeunlikelythattheanalytewillbeevidencedintapwaterexceptasseparateglycineandN-phosp
4、honomethylmoieties,neitherofwhichisapplicabletothismethod.ChemicalAbstractServicesAnalyteRegistryNumberGlyphosate1071-83-61.3Themethoddetectionlimits(MDL,definedinSection13.0)forglyphosateare2listedinTable1.TheMDLsforaspecificsamplemaydifferfromthoselisted.2.0SUMMARYOFMETHOD2.1Awater
5、sampleisfilteredanda200μLaliquotinjectedintoacationexchangeHPLCcolumn.Separationisachievedbyusinganisocraticelution.Afterelutionfromtheanalyticalcolumnat65°C,theanalyteisoxidizedwithcalciumhypochlorite.Theproduct(glycine)isthencoupledwitho-phthalaldehyde-2-mercaptoethanolcomplexat38°
6、Ctogiveafluorophor,whichisdetectedbyafluorometerwithexcitationat340nmanddetectionof1,3emissionmeasuredat>455nm.3.0DEFINITIONS3.1LaboratoryDuplicates(LD1andLD2)--Twosamplealiquotstakenintheanalyticallaboratoryandanalyzedseparatelywithidenticalprocedures.AnalysesofLD1andLD2giveameasure
7、oftheprecisionassociatedwithlaboratoryprocedures,butnotwithsamplecollection,preservation,orstorageprocedures.3.2FieldDuplicates(FD1andFD2)--Twoseparatesamplescollectedatthesametimeandplaceunderidenticalcircumstancesandtreatedexactlythesamethroughoutfieldandlaboratoryprocedures.Analys
8、esofFD1andFD
