【astm標準】d 3695 - 95 (2013)

1、Designation:D3695?95(Reapproved2013)StardTestMethodfVolatileAlcoholsinWaterbyDirectAqueousInjectionGasChromatography1ThisstardisissuedunderthefixeddesignationD3695thenumberimmediatelyfollowingthedesignationindicatestheye

2、arofiginaladoptioninthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.Scope1.1Thistestmethodcoversawideran

3、geofalcoholswithvariousstructuresboilingpointsthatcanbeseparateddetectedquantitativelyinwaterwastewaterataminimumdetectionlimitofapproximately1mgLbyaqueousinjectiongasliquidchromatography.2Thistestmethodcanalsobeusedtode

4、tectothervolatileganiccompoundsqualitatively.ganicacidsamineshighboilinghighlypolarcompoundsarenotreadilydetectableunderthissetofconditions.FanalysisofganicswithsimilarfunctionalitiesrefertoothertestmethodsinVolumes11.01

5、11.02oftheAnnualBookofASTMStards.1.2ThistestmethodutilizestheproceduresprecautionsasdescribedinPracticeD2908.Utilizetheproceduresprecautionsasdescribedtherein.1.3ThistestmethodhasbeenusedsuccessfullywithreagentgradeTypeI

6、Inaturalchlinatedtapwaters.Itistheuser’sresponsibilitytoassurethevalidityofthistestmethodfanyuntestedmatrices.1.4Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuse

7、rofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritouse.2.ReferencedDocuments2.1ASTMStards:3D1129TerminologyRelatingtoWaterD1193SpecificationfReagentWaterD2908Practic

8、efMeasuringVolatileganicMatterinWaterbyAqueousInjectionGasChromatographyD3856GuidefManagementSystemsinLabatiesEngagedinAnalysisofWaterD4210PracticefIntralabatyQualityControlProceduresaDiscussiononReptingLowLevelData(With

9、drawn2002)4E355PracticefGasChromatographyTermsRelationships3.Terminology3.1Definitions—FdefinitionsoftermsusedinthistestmethodrefertoTerminologyD1129PracticeE355.4.SummaryofTestMethod4.1Analiquotofanaqueoussampleisdirect

10、lyinjectedintoagaschromatographbymeansofamicrolitresyringe.Theganiccompoundsinthesampleareseparatedelutedfromachromatographiccolumnintoaflameionizationdetect.ThecompoundsareidentifiedbyrelativeretentiontimeKovatsIndexmea

11、suredbydirectcomparisonwithcrespondingstardresponses.5.SignificanceUse5.1Themajganicconstituentsinindustrialwastewaterneedtobeidentifiedfsupptofeffectiveinplantpollutioncontrolprograms.Currentlythemostpracticalmeansftent

12、ativelyidentifyingmeasuringarangeofvolatileganiccompoundsisgasliquidchromatography.6.Interferences6.1Sincethespecifiedcolumnconditionsareapplicabletonumerousganicsthepossibilityofonemecomponentshavingidenticalretentionti

13、mesisalwayspresent.Therefetheanalystmustdeterminethequalitativeidentityofthecomponentsofeachpeakbyspectrometrictechniquesamulticolumnapproachbothsothatproperquantitationfthosecompoundsofinterestmaybemade.RefertoTable1fre

14、lativeretentiondata.1ThistestmethodisunderthejurisdictionofASTMCommitteeD19onWateristhedirectresponsibilityofSubcommitteeD19.06onMethodsfAnalysisfganicSubstancesinWater.CurrenteditionapprovedFeb.152013.PublishedMarch2013

15、.iginallyapprovedin1978.Lastpreviouseditionapprovedin2007asD3695–95(2007).DOI:10.1520D369595R13.2SugarJ.W.ConwayR.A.“GasLiquidChromatographicTechniquesfPetrochemicalWasteWaterAnalysis’’JournaloftheWaterPollutionControlFe

16、derationVol401968pp.1622–1631.3FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.4Thelastapprovedver

17、sionofthishisticalstardisreferencedonwww.astm.g.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates17.2ColumnCarbowax20M(trademark)5(5%)on80100AcidWashedChromosbW(trademark)66.1m(

18、20ft)3.2mm(1?8in.)inoutsidediameter0.508mm(0.020in.)wallthicknessstainlesssteel.8.Reagents8.1PurityofReagents—Reagentgradechemicalsshallbeused.Unlessotherwiseindicateditisintendedthatallreagentsshallconfmtothespecificati

19、onsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSocietywheresuchspecificationsareavailable.7Othergradesmaybeusedprovideditisfirstertainedthatthereagentisofsufficientlyhighpuritytopermititsusewithoutlesseningthe

20、accuracyofthedetermination.8.2PurityofWater—UnlessotherwiseindicatedreferencestowatershallbeunderstoodtomeanreagentwaterconfmingtoSpecificationD1193TypeII.8.3CalibrationStardization—Prepareastocksolutionofthematerialsofi

21、nterestbyweighingaknownamountofeach1.00glessdilutingwithwaterto1Lmixing.Subsequentdilutionsshouldbepreparedasdeemednecessary.9.Sampling9.1CollectthesampleinaccdancewithSection9ofPracticeD2908.10.Procedure10.1Usetheproced

22、uresdescribedinPracticeD2908.11.TypicalChromatogram11.1InstrumentParameters:ColumnCarbowax20M(5%)80100AWChromasbW6.1m(20ft)3.2mm(1?8in.)inoutsidediameterstainlesssteelDetectflameionizationTemperaturesinjectionpt–165to260

23、Cdetect–250Ccolumn–50to250Cat8CminGasescarrier–Heat45mLminSampleSize10LRecdertspeed1.3cmmin(0.5in.min)fullscaleresponse1mV(23.3cm)11.2SeethechromatograminFig.1frelativeretentiontimesseparationofcompoundsusedintheroundrob

24、intesting.12.PrecisionBias812.1Sixlabatiesdeterminedtheprecisionbiasoftheprocedureperfmingtriplicateanalysesatthreelevelsinbothnaturalreagentwater(seeTable2Table3).12.2Theprecisionbiasdatapresentedin12.112.2werebasedonan

25、interlabatycollabativestudywithsamplescontainingalcoholsonly.Theprecisionbiasofthisprocedureftheothercompoundscoveredbytheproceduremayvaryfromthesedata.5ThesolesourceofsupplyoftheapparatusknowntothecommitteeatthistimeisU

26、nionCarbideCp.IfyouareawareofalternativesupplierspleaseprovidethisinfmationtoASTMInternationalHeadquarters.Yourcommentswillreceivecarefulconsiderationatameetingoftheresponsibletechnicalcommittee1whichyoumayattend.6Thesol

27、esourceofsupplyoftheapparatusknowntothecommitteeatthistimeisJohnsManvilleProductsCo.IfyouareawareofalternativesupplierspleaseprovidethisinfmationtoASTMInternationalHeadquarters.Yourcommentswillreceivecarefulconsideration

28、atameetingoftheresponsibletechnicalcommittee1whichyoumayattend.7ReagentChemicalsAmericanChemicalSocietySpecificationsAmericanChemicalSocietyWashingtonDC.FsuggestionsonthetestingofreagentsnotlistedbytheAmericanChemicalSoc

29、ietyseeAnalarStardsfLabatyChemicalsBDHLtd.PooleDsetU.K.theUnitedStatesPharmacopeiaNationalFmularyU.S.PharmaceuticalConventionInc.(USPC)RockvilleMD.8SupptingdatahavebeenfiledatASTMInternationalHeadquartersmaybeobtainedbyr