Designation:D7597−09´2StandardTestMethodforDeterminationofDiisopropylMethylphosphonate,EthylHydrogenDimethylamidophosphate,EthylMethylphosphonicAcid,IsopropylMethylphosphonicAcid,MethylphosphonicAcidandPinacolylMethylphosphonicAcidinWaterbyLiquidChromatography/TandemMassSpectrometry1ThisstandardisissuedunderthefixeddesignationD7597;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.ε1NOTE—ThistestmethodwaschangededitoriallyinFebruary2012.ε2NOTE—AddedresearchreportfootnotetoSection16editoriallyinJune2013.1.Scope1.1Thisprocedurecoversthedeterminationofdiisopropylmethylphosphonate(DIMP),ethylhydrogendimethylami-dophosphate(EHDMAP),ethylmethylphosphonicacid(EMPA),isopropylmethylphosphonicacid(IMPA),methyl-phosphonicacid(MPA)andpinacolylmethylphosphonicacid(PMPA)(referredtocollectivelyasorganophosphonatesinthistestmethod)insurfacewaterbydirectinjectionusingliquidchromatography(LC)anddetectedwithtandemmassspec-trometry(MS/MS)usingelectrosprayionization(ESI).Theseanalytesarequalitativelyandquantitativelydeterminedbythismethod.Thismethodadherestosinglereactionmonitoring(SRM)massspectrometry.1.2ThistestmethodhasbeendevelopedbyUSEPARegion5ChicagoRegionalLaboratory(CRL).1.3ThevaluesstatedinSIunitsaretoberegardedasstandard.Nootherunitsofmeasurementareincludedinthisstandard.1.4Thedetectionverificationlevel(DVL)andreportingrangefortheorganophosphonatesarelistedinTable1.1.4.1TheDVLisrequiredtobeataconcentrationatleastthreetimesbelowthereportinglimit(RL)andhaveasignal/noiseratiogreaterthan3:1.Fig.1displaysthesignal/noiseratiosattheDVLsfortheorganophosphonatesintheESIpositivemodeandFig.2intheESInegativemode.1.4.2ThereportinglimitistheconcentrationoftheLevel1calibrationstandardasshowninTable2fortheorganophos-phonatesexceptforMPAintheESInegativemodewhichisatLevel2duetonotme...
