【astm標(biāo)準(zhǔn)】d 7575 - 11

1、Designation:D7575?11StardTestMethodfSolventFreeMembraneRecoverableOilGreasebyInfraredDetermination1ThisstardisissuedunderthefixeddesignationD7575thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoption

2、inthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.Scope1.1Thistestmethodcoversthedeterminationofoilgreas

3、einproducedwastewatersamplesovertheconcentrationrangeoutlinedinTable1thatcanbeextractedwithaninfraredamenablemembranemeasuredbyinfraredtransmissionthroughthemembrane.1.2Thismethoddefinesoilgreaseinwaterasthatwhichisextra

4、ctableinthetestmethodmeasuredbyinfraredtransmission.1.3Themethoddetectionlimit(MDL)recommendedreptingrangearelistedinTable1.1.4ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurementareincludedinthisstar

5、d.1.5Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritous

6、e.2.ReferencedDocuments2.1ASTMStards:2D1129TerminologyRelatingtoWaterD1193SpecificationfReagentWaterD2777PracticefDeterminationofPrecisionBiasofApplicableTestMethodsofCommitteeD19onWaterD5847PracticefWritingQualityContro

7、lSpecificationsfStardTestMethodsfWaterAnalysisE168PracticesfGeneralTechniquesofInfraredQuantitativeAnalysisE178PracticefDealingWithOutlyingObservations2.2EPAStards3EPAMethod1664RevisionA:NHexaneExtractableMaterial(HEMOil

8、Grease)SilicaGelTreatedNHexaneExtractableMaterial(SGTHEMNonpolarMaterial)ByExtractionGravimetry40CFR49CFR3.Terminology3.1Definitions—FdefinitionsoftermsusedinthistestmethodrefertoTerminologyD1129PracticesE168.3.2Definiti

9、onsofTermsSpecifictoThisStard:3.2.1oilgreasen—“membranerecoverableoilgrease”isamethoddefinedanalytethatisthedefinitionofmembranerecoverableoilgreaseisdependentontheprocedureused.3.2.1.1Discussion—Thenatureoftheoilsgrease

10、s(both)thepresenceofrecoverablenonoilymatterinthesamplewillinfluencethematerialmeasuredinterpretationofresults.3.2.2extractn—adevicethatcontainsaninfraredamenableoilgreasesolidphaseextractionmembranedirectswaterflowthrou

11、ghthemembraneunderappliedpressure.4.SummaryofTestMethod4.1Thisisaperfmancebasedmethodmodificationsareallowedtoimproveperfmance.4.2Asampleofwaterisprocessedthroughanextract.4.3Theextractisthensufficientlydriedofwatersoast

12、oallowinfraredanalysis.4.4Theextractisexaminedbyaninfraredanalyzerfanoilgreasemeasurement.4.5Calibrationsdataareprocessedmanuallywithappropriatesoftware.1ThistestmethodisunderthejurisdictionofASTMCommitteeD19onWateristhe

13、directresponsibilityofSubcommitteeD19.06onMethodsfAnalysisfganicSubstancesinWater.CurrenteditionapprovedNov.12011.PublishedNovember2011.iginallyapproved2010.Lastcurrentversionapprovedin2010asD7575–10ε1.DOI:10.1520D757511

14、.2FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.3AvailablefromUnitedStatesEnvironmentalProtectio

15、nAgency(EPA)ArielRiosBldg.1200PennsylvaniaAve.NWWashingtonDC20460:www.epa.gov.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates18.5Acetone—ACSresiduelessthan1mgL.8.6Hexadecane—9

16、8%minimumpurity.8.7StearicAcid—98%minimumpurity.9.Hazards9.1Nmallabatysafetyappliestothismethod.Analystsshouldwearsafetyglassesgloveslabcoatswhenwkingwithacids.AnalystsshouldreviewtheMaterialSafetyDataSheets(MSDS)fallrea

17、gentsusedinthismethod.Additionalhazardsmaybepresentedbytheparticularsamplebeingtestedsopropercaremustbetaken.10.Sampling10.1Fillthesamplecontainer.Donotfillthecontainertothebrimsufficientheadspaceisrequiredtoallowvigoush

18、omogenization.Donotrinsethesamplecontainerwiththesampletobeanalyzed.Donotallowthesampletooverflowthecontainerduringcollection.Preventingoverflowmaynotbepossibleinallsamplingsituationshowevermeasuresshouldbetakentominimiz

19、eoverflowatalltimes.NOTE3—About5–10%ofvolumeheadspacehasbeenfoundtobesuitablefhomogenization.10.2Addasufficientquantityofeithersulfuric(seeSection8.4)hydrochlicacid(seeSection8.3)toapHof2.Ifanalysisistobedelayedfmethanfo

20、urhoursrefrigerateto6Clesswithoutfreezingfromthetimeofcollectionuntilextraction.TheamountofacidrequiredwillbedependentuponthepHbuffercapacityofthesampleatthetimeofcollection.IftheamountofacidrequiredisnotknownmakethepHme

21、asurementonaseparatesamplethatwillnotbeanalyzed.IntroductionofpHpapertoanactualsamplesamplecapmayremovesomeoilfromthesample.Tomeaccuratelycalculatethefinaloilgreaseconcentrationthefollowingequationcanbeused:CS5Ci3~VS1VA!

22、VS(1)whereCiisthemeasuredconcentrationVSisthesamplevolumeVAisthevolumeofacidaddedtothesampleCSisthesampleconcentrationbefetheacidwasadded.10.3IfthesampleistobeshippedbycommercialcarrierU.S.DepartmentofTransptationregulat

23、ions(see49CFRpart172)limitthepHtoaminimumof1.96ifHClisused1.15ifH2SO4isused.(see40CFRPart136TableIIFootnote3).NOTE4—Fthosecircumstancesrequiringthecollectionofmultiplealiquotsofonesampleeachaliquotistobecollectedineither

24、ofthefollowingways:(1)collectsimultaneouslyinparallelifpossible(2)collectasgrabsamplesinrapidsuccessionfilling1?3ofeachcontaineratatimecontinuinguntilallcontainersare90–95%fullconsistentwithNote3.11.PreparationofApparatu

25、s11.1HexadecaneStearicAcid(11)SpikingSolution—Place400mg64mghexadecane400mg64mgstearicacidina100mLvolumetricflaskfilltothebottomofthenecknottothemarkwithacetone.NOTE5—Thesolutionmayrequirewarmingfcompletedissolutionofste

26、aricacid.11.2Afterthehexadecanestearicacidhasdissolvedallowtocooltoroomtemperatureaddacetonetothemark.Stopperthevolumetricflasktransferthesolutiontoa100–150mLvialwithfluopolymerlinedcap.Markthesolutionlevelonthevialstein

27、thedarkatroomtemperature.11.3Immediatelypritothefirstuseverifythelevelonthevialbringtovolumewithacetoneifrequired.Warmtoredissolveallvisibleprecipitateifrequired.Ifthereisdoubtoftheconcentrationremove10.060.1mLwithavolum

28、etricpipetplaceinataredweighingpanevapatetodrynessinafumehood.Theweightmustbe8061mg.Ifnotprepareafreshsolution(Section11.1).11.4ThespikingsolutionsshouldbecheckedfrequentlyfsignsofdegradationevapationusingthetestinSectio

29、n11.3.11.5Ifnecessarythissolutioncanbemademelessconcentratedtosuittheconcentrationneededfthematrixspike.Afreshspikingsolutionshouldbepreparedweeklybiweekly.12.CalibrationStardization12.1Toensureanalyticalvaluesobtainedus

30、ingthistestmethodarevalidaccuratewithintheconfidencelimitsofthetesttheinstrumentmanufacturer’sinstructionsthefollowingproceduresmustbefollowedwhenperfmingthetestmethod.NOTE6—InstrumentsotherthanFTIRspectrometersmayhavedi

31、fferentproceduresthatshouldbefollowedaccdingtothemanufacturer’sinstructions.12.2Calibrationiscarriedoutusingthesetofcalibrationstarddevices(CSD).12.2.1TakeabackgroundreferencefilethroughtheCSDlabeled“Background”accdingto

32、theinstrumentmanufacturer’sinstructions.12.2.2ScaneachoftheotherCSDsaccdingtotheinstrumentmanufacturer’sinstructions.12.2.3Measurerecdtheabsbanceofthepeakcenterednear2920cm–1(3.42micron)accdingtoPracticesE168.Theinstrume

33、ntmayincludeautomaticmeasurementsoftwareifsofollowinstrumentmanufacturer’sinstructionsfusingthesoftware.NOTE7—OtherpeaksassociatedwiththemethylenemoietymayalsobeuseddetectionlimitswillbeaffectedsotheoperatshouldfollowSec

34、tion12.4todeterminethedetectionlimitftheabsbancepeakschosen.12.2.4Linearcalibrationmaybeusedifthecoefficientofdeterminationr2is0.95ftheanalyte.Ifoneofthecalibrationstardsotherthanthehighlowpointcausesther2tobe0.95calibra