【astm標(biāo)準(zhǔn)】d 7065 - 11

1、Designation:D7065?11StardTestMethodfDeterminationofNonylphenolBisphenolAptertOctylphenolNonylphenolMonoethoxylateNonylphenolDiethoxylateinEnvironmentalWatersbyGasChromatographyMassSpectrometry1Thisstardisissuedunderthefi

2、xeddesignationD7065thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditia

3、lchangesincethelastrevisionreapproval.1.Scope1.1Thistestmethodcoversdeterminationofnonylphenol(NP)nonylphenolethoxylate(NP1EO)nonylphenoldiethoxylate(NP2EO)octylphenol(OP)bisphenolA(BPA)thatarepartitionedintoganicsolvent

4、separatedusinggaschromatographydetectedwithmassivedetection.Thesecompoundsisomermixturesarequalitativelyquantitativelydeterminedbythismethod.Thismethodadherestoedionmonitingmassspectrometrybutfullscanmassspectrometryhasa

5、lsobeenshowntowkwellundertheseconditions.Eitheranalysismaybeused.1.2Themethoddetectionlimit(MDL)reptinglimit(RL)fNPNP1EONP2EOOPBPAarelistedinTable1.1.3ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurem

6、entareincludedinthisstard.1.4Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticestodeterminetheapplicabilityof

7、regulatylimitationspritouse.2.ReferencedDocuments2.1ASTMStards:2D1193SpecificationfReagentWaterD3694PracticesfPreparationofSampleContainersfPreservationofganicConstituentsD3856GuidefManagementSystemsinLabatiesEngagedinAn

8、alysisofWaterD5847PracticefWritingQualityControlSpecificationsfStardTestMethodsfWaterAnalysisD5905PracticefthePreparationofSubstituteWastewaterE691PracticefConductinganInterlabatyStudytoDeterminethePrecisionofaTestMethod

9、3.Terminology3.1Definitions:3.1.1NonylphenolNPn—nonylphenolismixedisomersofbranchedpnonylphenol.3.1.1.1Discussion—Commercialnonylphenolisproducedbythereactionofphenolwithcommercialnonene.Commercialnoneneisnotsimplyalinea

10、rC9H18alphaolefinitisacomplexmixtureofpredominantlyninecarbonolefinscalledpropylenetrimercontainingnolinearisomers.Thissynthesisresultsinamixtureofvariousbranchednonylphenolisomersratherthanadiscretechemicalstructure.The

11、branchednonylgroupispositionedpredominantlyintheparapositiononthephenolring.3.1.2OctylphenolOPn—OPrepresents4(1133tetramethylbutyl)phenol.3.1.2.1Discussion—Commercialoctylphenolisproducedbythereactionofphenoldiisobutylen

12、etoproducepredominantlythe4(1133tetramethylbutyl)phenolisomer.3.1.3BisphenolABPAnBPArepresents44’dihydroxy22diphenylpropane.3.1.3.1Discussion—CommercialbisphenolAisproducedbythecondensationreactionofphenolacetonetoproduc

13、epredominantlythe44’dihydroxy22diphenylpropane.3.1.4Environmentalwatern—itshallrefertowatertestedusingthismethod.SeeSection5.3.2Abbreviations:3.2.1NP1EO—branchednonylphenolmonoethoxylate.3.2.2NP2EO—branchednonylphenoldie

14、thoxylate.3.2.3nNP—nmalstraightchainnonylphenol.3.2.3.1Discussion—nNPisusedinthismethodasasurrogatefNPOPBPA.nNPisnotproducedcommerciallyisnotexpectedtobefoundinenvironmentalwaters.1ThistestmethodisunderthejurisdictionofA

15、STMCommitteeD19onWateristhedirectresponsibilityofSubcommitteeD19.06onMethodsfAnalysisfganicSubstancesinWater.CurrenteditionapprovedJune152011.PublishedJuly2011.iginallypublishedin2006.Lastpreviousversionapprovedin2006asD

16、7065–06.DOI:10.1520D706511.2FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.Copyright?ASTMInternat

17、ional100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates17.1.2AnalyticalColumn—Ananalyticalcolumn(DB5MS30m0.25mmi.dfilmthickness—0.25mequivalent(5%phenyl)methylpolysiloxane)suitableftheanalysisoftargetalkyl

18、phenols.67.1.3MassSpectrometer(MS)System—AnMSsystemcapableofscanning45to500amuevery2slessusing70eVintheelectronimpactmodeproducingamassspectrumwhichmeetsallthecriteriawhen50ngofdecafluorotriphenylphosphine(DFTPP)isinject

19、edthroughtheGCinlet.7.2CLLEApparatus.7.3ganicSolventEvapationDevice.8.ReagentsMaterials8.1PurityofReagents—Reagentgradechemicalsshallbeusedinalltests.Unlessindicatedotherwiseitisintendedthatallreagentsshallconfmtothespec

20、ificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety.7Otherreagentgradesmaybeusedprovideditisfirstertainedthattheyareofsufficientlyhighpuritytopermittheirusewithoutaffectingtheaccuracyofthemeasurement

21、.8.2PurityofWater—UnlessotherwiseindicatedreferencestowatershallbeunderstoodtomeanreagentwaterconfmingtoTypeIofspecificationD1193.Itmustbedemonstratedthatthiswaterdoesnotcontaincontaminantsatconcentrationssufficienttoint

22、erferewiththeanalysis.8.3Gases—Researchgradenitrogenheliumofhighestpurityareused.8.4MethyleneChlidechromatographygrade.8.5Methanolpurgetrapgrade.8.6BranchedNonylphenolMonoethoxylate(NP1EO)availableasahighpuritycustomstar

23、d.8.7BranchedNonylphenolDiethoxylate(NP2EO)availableasahighpuritycustomstard.8.8BranchedNonylphenolEthoxylateBlend(NP1EO–NP3EO)wherethecompositionisdeterminedbygaschromatography.88.9Nonylphenol(NP)95%paraisomer(CAS#84852

24、153).8.10Octylphenol(OP)99%4(1133tetramethylbutyl)phenol(CAS#140669).8.11BisphenolA(BPA)99%44ispropylidenediphenol(CAS#80057).8.12ConcentratedH2SO4(CAS#7664939).8.13InternalStardMixcontainingacenaphthened10phenanthrened1

25、0.8.14nnonylphenol(CAS#104405).8.15nNPmonoethoxylate(nNP1EOCAS#104358).8.16AcetoneReagentGrade(CAS#67641).8.17PerfluotributylaminePFTBA(CAS#311897).9.Hazards9.1Nmallabatysafetyappliestothismethod.Analystsshouldwearsafety

26、glassesgloveslabcoatswhenwkingwithacids.Methylenechlideisusedasanextractionsolventfthismethod.AnalystsshouldreviewtheMSDSfallreagentsusedinthismethod.10.SampleCollectionPreservationStage10.1Sampling:10.1.1Grabsamplesmust

27、becollectedinglasssamplecontainers.Conventionalsamplingpracticesshouldbefollowed.RefertoGuideD3856PracticeD3694.AutomaticsamplingequipmentshouldbeasfreeaspossibleofTygontubingotherpotentialsourcesofcontamination.Samplesm

28、ustbeicedkeptat0to4C.Samplesmustbepreventedfromfreezing.10.2Preservation:10.2.1AdjusttopH2withH2SO4.Stesamplesbetween04Cfromthetimeofcollectionuntilextraction.Extractthesamplewithin28daysofcollectioncompletelyanalyzewith

29、in40daysofextraction.10.2.2Sampleextractsmaybestedinsealedglasscontainersat0Cindefinitely.11.PreparationofGCMS11.1ChromatographOperatingConditions(approximatevaluesyourinstrumentmayrequiredifferentsettings):CarrierGas:He

30、liumCarrierFlow:Variable(1.3to0.4mLmin)ConstantPressure(11.16psiapproximately)AverageVelocity42cmsInjectionPtParameters:SplitlessInjectionInjectionPressure:10to12psiInjectionpttemperature:290CPurgeflowtosplitvent:30mLmin

31、at0.75minTotalFlow34.2mLminColumnoventemperature:50Cinitiallyhold2min50to320Cat10Cmin320C–hold5minInjectionVolume:1LInjectionLiner:SingletaperlinerMSTransferLineTemperature:290C11.2MassSpectrometerParameters:Mode:Electro

32、nIonizationElectronMultiplier:Setelectronmultipliertoachieveoptimalperfmance.Tune:AutotuneusingPFTBAmasses69219502.DwellTime:30msSIMIons:RefertoTable2.6ThesolesourceofsupplyofthecolumnsknowntothecommitteeatthistimeisJ&WC

33、olumnsAgilentTechnologiesInc.2850CentervilleRd.WilmingtonDE19808.IfyouareawareofalternativesupplierspleaseprovidethisinfmationtoASTMInternationalHeadquarters.Yourcommentswillreceivecarefulconsiderationatameetingoftheresp

34、onsibletechnicalcommittee1whichyoumayattend.7ReagentChemicalsAmericanChemicalSocietySpecificationsAmericanChemicalSocietyWashingtonDC.FSuggestionsonthetestingofreagentsnotlistedbytheAmericanChemicalSocietyseeAnnualStards

35、fLabatyChemicalsBDHLtd.PooleDsetU.K.theUnitedStatesPharmacopeiaNationalFmularyU.S.PharmacopeialConventionInc.(USPC)RockvilleMD.8ThesolesourceofsupplyoftheblendknowntothecommitteeatthistimeisSchenectadyInternationalInc.27

36、50BalltownRoadSchenectadyNY12309.IfyouareawareofalternativesupplierspleaseprovidethisinfmationtoASTMInternationalHeadquarters.Yourcommentswillreceivecarefulconsiderationatameetingoftheresponsibletechnicalcommittee1whichy