Designation:D7599−16(Reapproved2017)StandardTestMethodforDeterminationofDiethanolamine,Triethanolamine,N-MethyldiethanolamineandN-EthyldiethanolamineinWaterbySingleReactionMonitoringLiquidChromatography/TandemMassSpectrometry(LC/MS/MS)1ThisstandardisissuedunderthefixeddesignationD7599;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.1.Scope1.1Thisprocedurecoversthedeterminationofdiethanolamine,triethanolamine,N-methyldiethanolamineandN-ethyldiethanolamine(referredtocollectivelyasethano-laminesinthistestmethod)insurfacewaterbydirectinjectionusingliquidchromatography(LC)anddetectedwithtandemmassspectrometry(MS/MS).Theseanalytesarequalitativelyandquantitativelydeterminedbythistestmethod.Thistestmethodadherestosinglereactionmonitoring(SRM)massspectrometry.1.2ThistestmethodhasbeendevelopedbyU.S.EPARegion5ChicagoRegionalLaboratory(CRL).1.3ThevaluesstatedinSIunitsaretoberegardedasstandard.Nootherunitsofmeasurementareincludedinthisstandard.1.4TheDetectionVerificationLevel(DVL)andReportingRangefortheethanolaminesarelistedinTable1.1.4.1TheDVLisrequiredtobeataconcentrationatleast3timesbelowtheReportingLimit(RL)andhaveasignal/noiseratiogreaterthan3:1.Fig.1displaysthesignal/noiseratiosattheDVLsandathigherconcentrationsforN-methyldiethanolamine.1.4.2ThereportinglimitistheconcentrationoftheLevel1calibrationstandardasshowninTable2fordiethanolamine,triethanolamine,andN-ethyldiethanolamineandLevel2forN-methyldiethanolamine.ThereportinglimitforN-methyldiethanolamineissetat50µg/Lduetopoorsensi-tivityata5µg/LconcentrationwhichdidnotmeettheDVLcriteria.TheDVLforN-methyldiethanolamineisat10µg/L,whichforcesaraisedreportinglimit(chromatogramsareshowninFig.1).However,themulti-laboratoryvalidationrequiredaspikeofalltargetanalytesat25µg/L.ThemeanrecoveryforN-methyldiethanolamineatth...
