【astm標準】d 5865 - 13

1、Designation:D5865?13StardTestMethodfGrossCalificValueofCoalCoke1ThisstardisissuedunderthefixeddesignationD5865thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisiontheyearoflastrev

2、ision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.Scope1.1Thistestmethodpertainstothedeterminationofthegrosscalificvalueofcoalcokebyeithera

3、nisoperiboladiabaticbombcalimeter.1.2ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurementareincludedinthisstard.1.3Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itisthe

4、responsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritouse.SpecifichazardstatementsaregiveninSection8.2.ReferencedDocuments2.1ASTMStards:2D121Termi

5、nologyofCoalCokeD346PracticefCollectionPreparationofCokeSamplesfLabatyAnalysisD388ClassificationofCoalsbyRankD1193SpecificationfReagentWaterD2013PracticefPreparingCoalSamplesfAnalysisD3173TestMethodfMoistureintheAnalysis

6、SampleofCoalCokeD3177TestMethodsfTotalSulfurintheAnalysisSampleofCoalCoke(Withdrawn2012)3D3180PracticefCalculatingCoalCokeAnalysesfromAsDeterminedtoDifferentBasesD4239TestMethodfSulfurintheAnalysisSampleofCoalCokeUsingHi

7、ghTemperatureTubeFurnaceCombustionD7582TestMethodsfProximateAnalysisofCoalCokebyMacroThermogravimetricAnalysisE144PracticefSafeUseofOxygenCombustionVesselsE178PracticefDealingWithOutlyingObservationsE882GuidefAccountabil

8、ityQualityControlintheChemicalAnalysisLabatyE2251SpecificationfLiquidinGlassASTMThermometerswithLowHazardPrecisionLiquids3.Terminology3.1FadditionaldefinitionsoftermsusedinthistestmethodrefertoTerminologyD121.3.2Definiti

9、ons:3.2.1adiabaticcalimeter—acalimeterthatoperatesintheadiabaticmodemaymaynotuseamicroprocess.Theinitialtemperaturebefeinitiatingthecombustionthefinaltemperaturesarerecdedbytheoperatthemicroprocess.3.2.2automatedcalimete

10、r—acalimeterwhichhasamicroprocessthattakesthethermometricreadingscalculatestheCalibrationValuetheHeatofCombustionValues.3.2.3Britishthermalunit[Btu]—istheamountofheatrequiredtoraisethetemperatureofonepoundmass[lbm]ofliqu

11、idwateratoneatmospherepressureonedegreeFahrenheitatastatedtemperature.Theresultsofcombustioncalimetrictestsoffuelsfsteampowerplantsmaybeexpressedintermsofthe1956InternationalSteamTablecalie(I.T.cal)whichisdefinedbytherel

12、ation1I.T.cal=4.1868J.TheBtuusedinmodernsteamtablesisdefinedbythemeansoftherelation1I.T.calg=1.8I.T.Btulb.Thus1I.T.Btulb=2.326Jg.3.2.4calificvalue—theheatproducedbycombustionofaunitquantityofasubstanceunderspecifiedcondi

13、tions.3.2.5calimeter—adevicefmeasuringcalificvalueconsistingofabombitscontentsavesselfholdingthebombtemperaturemeasuringdevicesignitionleadswaterstirrerajacketmaintainedatspecifiedtemperatureconditions.3.2.6grosscalificv

14、alue(grossheatofcombustionatconstantvolume)Qv(gross)—theheatproducedbycompletecombustionofasubstanceatconstantvolumewithallwaterfmedcondensedtoaliquid.1ThistestmethodisunderthejurisdictionofASTMCommitteeD05onCoalCokeisth

15、edirectresponsibilityofSubcommitteeD05.21onMethodsofAnalysis.CurrenteditionapprovedOct.12013.PublishedOctober2013.iginallyapprovedin1995.Lastpreviouseditionapprovedin2012asD5865–12.DOI:10.1520D586513.2FreferencedASTMstar

16、dsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.3Thelastapprovedversionofthishisticalstardisreferencedonwww.astm.g.AS

17、ummaryofChangessectionappearsattheendofthisstardCopyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates16.6.3.1ThermometerAccessies—Amagnifierisrequiredfreadingliquidinglassthermomete

18、rstoonetenthofthesmallestscaledivision.Themagnifiershallhavealensholderdesignedsoastominimizeerrsasaresultofparallax.6.7SampleHolder—Anopencrucibleofplatinumquartzbasemetalalloy.Befeuseinthecalimeterheattreatbasemetalcru

19、ciblesfaminimumof4hat500Ctoensurethecruciblesurfaceiscompletelyoxidized.Basemetalalloycruciblesareacceptableifafterthreepreliminaryfiringstheweightdoesnotchangebymethan0.0001g.6.8IgnitionFuse—Ignitionfuseof100mmlength0.1

20、6mm(No.34Bfillingthecalimetervesselfiringtheignitioncircuitrecdingcalimetertemperaturesbefeduringafterthetestrecdingthebalanceweightscarryingoutallnecessarycrectionscalculations.6.11CrucibleLiner—Quartzfiberalundumflinin

21、gthecrucibletopromotecompletecombustionofsamplesthatdonotburncompletelyduringthedeterminationofthecalificvalue.47.Reagents7.1ReagentWater—ConfmingtoconductivityrequirementsfTypeIIofSpecificationD1193fpreparationofreagent

22、swashingofthebombinteri.7.2PurityofReagents—UsereagentgradechemicalsconfmingtothespecificationoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSocietyinalltests.57.3BenzoicAcid—Stard(C6H5COOH)—Pelletsmadefrombenzoi

23、cacidavailablefromtheNationalInstituteofStardsTechnology(NIST)benzoicacidcalibratedagainstNISTstardmaterial.Thecalificvalueofbenzoicacidfuseinthecalibrationcalculationsshallbetraceabletoarecognizedcertificatevalue.7.4Oxy

24、gen—Manufacturedfromliquidairguaranteedtobegreaterthan99.5%purefreeofcombustiblematter.Oxygenmadebytheelectrolyticprocesscontainssmallamountsofhydrogenrenderingitunfitunlesspurifiedbypassageovercopperoxideat500C.7.5Titra

25、tionIndicat—Methylangemethylredmethylpurplefindicatingtheendpointwhentitratingtheacidfmedduringcombustion.Thesameindicatshallbeusedfbothcalibrationcalificvaluedeterminations.7.6StardSolution—Sodiumcarbonate(Na2CO3)others

26、uitablestardsolution.Aconvenientstardsolutionmaybepreparedasfollows.Dissolve3.706gofsodiumcarbonatedriedf24hat105Cinwaterdiluteto1L.Theresultingconcentration(0.0699N)assumestheenergyoffmationofHNO3underbombconditionsis59

27、.7kJmol(14.3kcalmole)(seeX1.1).Onemilliliterofthissolutionisequivalentto4.2J(1.0cal)intheacidtitration.Alternatively1.0mlofa0.1000Nbasesolutionisequivalentto6.0J(1.4cal)intheacidtitration.Ingeneralonemilliliterofanarbitr

28、arystardtitrantsolutionisequivalenttoitsconcentration(equivalentsliternmality[N])times59.7J(14.3cal).8.Hazards8.1Thefollowingprecautionsarerecommendedfsafecalimeteroperation.AdditionalprecautionsarenotedinPracticeE144.Al

29、soconsultthecalimeterequipmentmanufacturer’sinstallationoperatinginstructionsbefeusingthecalimeter.8.1.1Themassofsampleanycombustionaidaswellasthepressureoftheoxygenadmittedtothebombshallnotexceedthebombmanufacturer’sspe

30、cifications.8.1.2Inspectthebombpartscarefullyaftereachuse.Replacecrackedsignificantlywnparts.ReplaceOringsvalveseatsinaccdancewithmanufacturer’sinstruction.Fmedetailsconsultthemanufacturer.8.1.3Equiptheoxygensupplycylind

31、erwithanapprovedtypeofsafetydevicesuchasareliefvalveinadditiontotheneedlevalvepressuregaugeusedinregulatingtheoxygenfeedtothebomb.Valvesgaugesgasketsshallmeetindustrysafetycodes.Suitablereducingvalvesadaptersf3to4MPa(300

32、to500psig)disgepressurecanbeobtainedfromcommercialsourcesofcompressedgasequipment.Checkthepressuregaugeannuallyfaccuracyafteranyaccidentaloverpressuresthatreachmaximumgaugepressure.8.1.4Duringignitionofasampletheoperatsh

33、allnotextendanyptionofthebodyoverthecalimeter.8.1.5Donotfirethebombifthebombhasbeenpedturnedoverafterloading.8.1.6Donotfirethebombifthereisevidenceofgasleakagewhenthebombissubmergedinthecalimetervessel.8.1.7Fmanuallyoper

34、atedcalimeterstheignitionswitchshallbedepressedonlylongenoughtofirethege.9.Sample9.1Theanalysissampleisthematerialpulverizedtopass250m(No.60)sievepreparedinaccdancewitheitherPracticeD346fcokeMethodD2013fcoal.4Supptingdat

35、ahavebeenfiledatASTMInternationalHeadquartersmaybeobtainedbyrequestingResearchReptRR:D051025.5ReagentChemicalsAmericanChemicalSocietySpecificationsAmericanChemicalSocietyWashingtonDC.Fsuggestionsonthetestingofreagentsnot