【astm標準】d 5739 - 06 (2013)

1、Designation:D5739?06(Reapproved2013)StardPracticefOilSpillSourceIdentificationbyGasChromatographyPositiveIonElectronImpactLowResolutionMassSpectrometry1ThisstardisissuedunderthefixeddesignationD5739thenumberimmediatelyfo

2、llowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.S

3、cope1.1Thispracticecoverstheuseofgaschromatographymassspectrometrytoanalyzecomparepetroleumoilspillssuspectedsources.1.2Theprobablesourcefaspillcanbeertainedbytheexaminationofcertainuniquecompoundclassesthatalsodemonstra

4、tethemostweatheringstability.Toagreaterlesserdegreecertainchemicalclassescanbeanticipatedtochemicallyalterinproptiontotheweatheringexposuretimeseveritysubsequentanalyticalchangescanbepredicted.Thispracticerecommendsvario

5、usclassestobeanalyzedalsoprovidesaguidetoexpectedweathering—inducedanalyticalchanges.1.3ThispracticeisapplicablefmoderatelytoseverelydegradedpetroleumoilsinthedistillaterangefromdieselthroughBunkerCitisalsoapplicablefall

6、crudeoilswithcomparabledistillationranges.Thispracticemayhavelimitedapplicabilityfsomekerosenesbutitisnotusefulfgasolines.1.4ThevaluesstatedinSIunitsaretoberegardedasthestard.1.5Thisstarddoesnotpurpttoaddressallofthesafe

7、tyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritouse.2.ReferencedDocuments2.1ASTMStards:2D1129Term

8、inologyRelatingtoWaterD3325PracticefPreservationofWaterbneOilSamplesD3326PracticefPreparationofSamplesfIdentificationofWaterbneOilsD3328TestMethodsfComparisonofWaterbnePetroleumOilsbyGasChromatographyD3414TestMethodfComp

9、arisonofWaterbnePetroleumOilsbyInfraredSpectroscopyD3415PracticefIdentificationofWaterbneOilsD3650TestMethodfComparisonofWaterbnePetroleumOilsByFluescenceAnalysisD5037TestMethodfComparisonofWaterbnePetroleumOilsbyHighPer

10、fmanceLiquidChromatography(Withdrawn2002)3E355PracticefGasChromatographyTermsRelationships3.SummaryofPractice3.1Therecommendedchromatographycolumnisacapillarydirectlyinterfacedtothemassspectrometer(eitherquadrupolemagic)

11、.3.2Thelowresolutionmassspectrometerisoperatedinthepositiveionelectronimpactmode70eVnominal.3.3Massspectraldataareacquiredstedprocessedwiththeaidofcommerciallyavailablecomputerbaseddatasystems.4.SignificanceUse4.1Thispra

12、cticeisusefulfassessingthesourcefanoilspill.Otherlesscomplexanalyticalprocedures(TestMethodsD3328D3414D3650D5037)mayprovideallofthenecessaryinfmationfertaininganoilspillsourcehowevertheuseofamecomplexanalyticalstrategyma

13、ybenecessaryincertaindifficultcasesparticularlyfsignificantlyweatheredoils.Thispracticeprovidestheuserwithameanstothisend.4.1.1Thispracticepresumesthata“screening”ofpossiblesuspectsourceshasalreadyoccurredusinglessintens

14、ive1ThispracticeisunderthejurisdictionofASTMCommitteeD19onWateristhedirectresponsibilityofSubcommitteeD19.06onMethodsfAnalysisfganicSubstancesinWater.CurrenteditionapprovedFeb.152013.PublishedMarch2013.iginallyapprovedin

15、1995.Lastpreviouseditionapprovedin2006asD5739–06.DOI:10.1520D573906R13.2FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummar

16、ypageontheASTMwebsite.3Thelastapprovedversionofthishisticalstardisreferencedonwww.astm.g.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates1(me69at100%ofbasepeak)(me219at35to40%A

17、ofbasepeak)B(me502at1to2%ofbasepeak)CAThesensitivityfalmostalloftheionsmonited(Table1)canbeimprovedsomewhatbyadjustingthispercentagetobetween6065howevertheresultingmassspectramaybedisttedsignificantlysothatMScomputersear

18、chroutinesftheidentificationofunknownsbycomparisontoconventionallyacquiredmassspectrallibrariesmaybeimpairedsignificantly.BAdjusttheentrancelensvoltage.CAdjusttheionfocusvoltage.7.2.2Retuneevery12hofmassspectrometeropera

19、tion.7.3ResolutionCheck—Undertheinstrumentalconditionslisted(7.1)pristanephytaneusuallydisplay80%greaterresolutionfromC17C18respectively.Iftheresolutionislessthan50%takecrectiveactionsuchasreplacementoftheinjectlinerseal

20、sremovalofthefrontoftheanalyticalcolumn.ReptthedegreeofresolutioninSection10.RefertoPracticeE355fcalculationofresolutionvalues.7.4MassDiscriminationCheck:7.4.1Usethegaschromatographicinstrumentalparametersenumeratedin8.3

21、.1operatethemassspectrometerbutinthelinearscanmodefromme45to360in1s.7.4.2Injecta1Lsolutionofnaphthalenefluanthenebenzo(ghi)peryleneinequalconcentrations(from50to150ngL)incyclohexane.7.4.3Integratethetotalionchromatogram(

22、TIC).7.4.4Calculatethefollowingratios:(1)Areaofnaphthalenetoareaoffluanthene(2)Areaofbenzo(ghi)perylenetoareaoffluanthene.7.4.5Theratioof(1)mustbelessthanequalto2theratioof(2)mustbegreaterthanequalto0.2.ReptthisvalueinSe

23、ction10.7.4.6Ahighmolecularweightresponsecansometimesbeimprovedbychangingtheperationofthechromatographiccolumnintotheinjectbodyusingsilanizedglasswoolquartzasinjectpackingmaterialboth.Electronicflowcontrol(insteadofconst

24、antcolumnheadpressure)hasrecentlybecomeavailablefCapillaryGC.Itcanbeusedtoprovideahighmolecularweightresponsebyincreasedflowduringsplitlessinjection.7.5RetentionTimeCheck—Theabsoluteretentiontimesfthemassdiscriminationch

25、eckcompounds(7.4.2)mustberecded.Thebatchtobatchretentiontimereproducibilitycanbedocumentedinthisway.RepttheseretentiontimesinSection10.8.Procedure8.1RefertoTerminologyD1129ftermsrelatingtowaterPracticeD3415fidentificatio

26、nofwaterbneoils.RefertoPracticeD3325fthepreservationofoilsamplesPracticeD3326fpreparationoftheneatoilsample.(PracticeD3326includesProcedureFfrecoveringoilfromthinfilmsonwaterProcedureGfrecoveringoilfromsdebris.)Itisthere

27、sponsibilityoftheusertovalidatethismethodfusewiththesetypesofmatricessinceoilrecoveredfromthemmaycontaincontaminationderivedfromthesubstratematerial.8.2SamplePreparation—Weigh100to200mgofoilintoascrewcapglassvialadd10mLc

28、yclohexane.Sonicationmaybenecessaryaswellascentrifugationtoremoveparticulatesifthesampledoesnotdissolvecompletely.8.3InstrumentalParameters:8.3.1GasChromatograph—Usethefollowingparameters:1Lsplitlessinjectionf45saninitia

29、lcolumntemperatureof55Cf2minatemperaturerampat6Cminto270Catemperaturerampof3Cminto300Cafinalcolumntemperatureof300Cf17minaninjectiontemperatureof290Camassspectrometer(MS)interfacetemperatureof300C.Atotalruntimeofapproxim

30、ately65minwillbeachievedusingtheseparameters.8.3.2MassSpectrometerDataAcquisitionParameters—Operatethemassspectrometerinedionmoniting(SIM)fthe24ionslistedinTable2.Sincealloftheionswillbescannedeverysecondthedwelltimefeac

31、his70ms.Allowasolventdelaytimeof4minbefethestartofMSscanning.NOTE1—Itisrecognizedthatthedifferentmonitedclassesofanalyteseluteonlyincertainregionsofthechromatogramconsequentlynotallionsneedbemonitedcontinuously.Howeverno

32、effthasbeenmadetosegmentthechromatogrambyusingdifferentSIMmassesatdifferenttimesfthesakeofmaintainingsimplicity.Itisalsorecognizedthatthesignaltonoiseratioisimprovedbyanincreaseinthedwelltimehoweverthisimprovementisdirec

33、tlyproptionaltothesquarerootoftheproptionaldwelltimeincrease.Asignaltonoiseratioincreaseofonlytwowouldthusresultfromafourfoldincreaseinthedwell(from70to280ms).Thisincreaseddwelltimewouldpermitonly3ionsstobemonited.Nevert

34、helesstheexperiencedanalystwhoiswkingwithawellacterizedoilsourcesuchasmonitingdegradationovertimemaychoosetomonitfewerionsindertomaximizethesignaltonoiseratiosconsequentlyimprovethesensitivityfasubsetoftheionslistedinthe

35、table.SimilarlyusersofcertainoldermodelmassspectrometersmayalsochoosetomodifySIMacquisitionbymonitingfewerionssimultaneouslyindertooffsetloweredMSsensitivity.8.4SampleAnalysisBatchingRequirements—Everytimethemassspectrom

36、eterisusedbracketallsamplesbyaTABLE2SIMAcquisitionmeDwellmsElutionrangemin85704to60113704to60156704to60166704to60170704to60177704to60178704to60183704to60184704to60191704to60192704to60198704to60202704to60205704to60206704t