1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS 6043-1.11:2000 ISO 129
2、79:1999 ICS 71.100.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Methods of sampling and test for carbonaceous materials used in aluminium manufacture Part 1: Electrode pitch Section 1.11: Determination of the atomic C/H ratio of the quinoline-insoluble materialThis Briti
3、sh Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 January 2000 BSI 01-2000 ISBN 0 580 35777 5 BS 6043-1.11:2000 Amendments issued since publication Amd. N
4、o. Date Comments National foreword This British Standard reproduces verbatim ISO 12979:1999 and implements it as the UK national standard. It supersedes BS 6043-1.11:1994 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee CII/24, Raw materials for the al
5、uminium industry, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developmen
6、ts and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue
7、under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correc
8、t application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 11 and a back cover. The BSI copyright notice displayed in this d
9、ocument indicates when the document was last issued.Reference number ISO 12979:1999(E) ISO 1999 INTERNATIONAL STANDARD ISO 12979 First edition 1999-12-01 Carbonaceous materials used in the production of aluminium Pitch for electrodes Determination of C/H ratio in the quinoline-insoluble fraction Pro
10、duits carbons utiliss pour la production de laluminium Brais pour lectrodes Dtermination du rapport C/H dans la fraction insoluble dans la quinolineii blankISO12979:1999(E)iii Contents Page 1 Scope1 2 Normativereferences1 3 Principle1 4 Isolationofquinoline-insolublematerialforanalysis2 4.1 Reagents
11、.2 4.2 Apparatus.2 4.3 Samplingandpreparationofthetestsample.2 4.4 Procedure.2 4.5 Calculationandexpressionofresults.5 5 Analysisofquinoline-insolublematerialforcarbonandhydrogencontent.5 5.1 Reagents.5 5.2 Apparatus.5 5.3 Preparationoftheapparatus7 5.4 Procedure.9 5.5 Calculationandexpressionofresu
12、lts.9 5.6 Ashcontent10 6 Precision.11 6.1 Repeatability.11 6.2 Reproducibility.11 7 Testreport11ISO12979:1999(E) iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedo
13、utthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElec
14、trotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandar
15、drequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO12979waspreparedbyTechnicalCommitteeI
16、SO/TC47, Chemistry, Subcommittee SC7, Aluminium oxide, cryolite, aluminium fluoride, sodium fluoride, carbonaceous products for the aluminium industry.INTERNATIONALSTANDARD ISO12979:1999(E)1 Carbonaceousmaterialsusedintheproductionofaluminium PitchforelectrodesDeterminationofC/Hratiointhe quinoline-
17、insolublefraction 1 Scope ThisInternationalStandarddescribesamethodforthedeterminationoftheatomiccarbon/hydrogenratioof quinoline-insolublematerialisolatedfromcoal-tarpitches.Aprocedurefortheisolationofthequinoline-insoluble materialinaformsuitablefortheanalysisisdescribed. NOTE Theisolationprocedur
18、eisnotanalternativetoISO6971 1) ,whichistobeusedinallcaseswheretheamountof quinoline-insolublematterpresentinapitchistobedetermined. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferenc
19、es,subsequentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocum
20、entreferredtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards. ISO565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings. ISO4788, Laboratory glassware Graduated measuring cylinders. ISO6257, Carbonaceous material
21、s used in the production of aluminium Pitch for electrodes Sampling. 3Principle Thequinoline-insolublematerialisisolatedfromafinelydividedsampleofthecoal-tarpitchbydigestionwithhot quinolinefollowedbypressure-filtrationthroughamembranefilter.Theisolatedmaterialiswashedonthefilterwith hotquinolinethe
22、nwithhottolueneanddried. Thecarbonandhydrogencontentsoftheisolatedquinoline-insolublematerialaredeterminedbycombustionofa weighedaliquotportionofthatmaterialinastreamofoxygenandtrappingandweighingthecarbondioxideand waterwhichareformed.Theatomiccarbon/hydrogenratioofthequinoline-insolublematerialisc
23、alculatedfromits carbonandhydrogencontentsandtherelativeatomicmassesofcarbonandhydrogen. 1)ISO6971, Carbonaceous materials for the production of aluminium Pitch for electrodes Determination of contents of quinoline-insoluble material.ISO12979:1999(E) 2 4 Isolationofquinoline-insolublematerialforanal
24、ysis 4.1 Reagents WARNINGRefertothereagentsuppliersHealthandSafetydatasheetsfortheprecautionswhichareto betakenforthesafeuseofquinolineandtoluene. 4.1.1 Quinoline,ofpurityatleast97%,freshlydistilled,boilingbetween235Cand237Cat0,1013MPa. Storethedistilledquinolinebetween5Candambienttemperatureinastop
25、peredbottleofdarkglass.Useitwithin twoweeks;afterthistimeperiodeitherredistillordiscardthequinoline. 4.1.2 Toluene,generalpurposereagentgrade. 4.1.3 Nitrogenorotherinertgas,suppliedviaatwo-stagepressureregulatorwithamaximumoutletpressure of0,45MPa. 4.2 Apparatus WARNINGBeforeusingpressure-filtration
26、equipmentensurethatitisprovidedwithadequatesafety devicesandthattheequipmenthasbeentestedtoensurecompliancewithrelevantHealthandSafety legislation. Ordinarylaboratoryapparatusandthefollowing. 4.2.1 Thermostaticallycontrolledelectrichotplate,capableofmaintainingliquidsinbeakersat70Cto 80C. 4.2.2 Pres
27、sure-filtrationapparatus,acceptingfilterdiscsof47mmdiameteranddesignedforsafeoperationat upto120Cwithappliedgaspressuresofupto1MPa.Atypicalpressure-filtrationapparatusisshowninFigure1. 4.2.3 Membranefilterdiscs,ofpolytetrafluoroethylene(PTFE),47mmindiameterandhavinganominalpore sizeof0,2 m. 4.2.4 Ha
28、nd-heldhot-airblower,general-purposelaboratorytype,typicallyof500Wpowerratingandgivingan airexittemperatureofapproximately300C. 4.2.5 Testsieve,of250 mnominalaperture,conformingtotherequirementsofISO565,andhavingalidand receiver. 4.2.6 Watchglass,approximately70mmindiameter,driedat105Cto110Cfor1hand
29、cooledina desiccator. 4.2.7 Measuringcylinder,ofborosilicateglass,of50mlcapacitywithpouringspout,conformingtothe requirementsofISO4788. 4.3 Samplingandpreparationofthetestsample Preparearepresentativesampleofapproximately10gofthepitchbythemethoddescribedinISO6257.Grindthe samplewithapestleandmortaru
30、ntilitallpassesthetestsieve(4.2.5). 4.4 Procedure 4.4.1 Weigha100mlborosilicateglassbeakertothenearest0,1mg.Transferapproximately1gofthetest sample(4.3)tothebeakerandweighittothenearest0,1mg.Usingthemeasuringcylinder(4.2.7),add25mlof thequinoline(4.1.1)andstirthemixturewithaglassrodtobreakupanyagglo
31、merates.Coverthebeakerwitha watchglassandplaceitonthehotplate(4.2.1).Allowthemixturetodigestat70Cto80Cfor20min.DuringtheISO12979:1999(E)3 digestionstirthecontentsofthebeakeratapproximately5minintervals.Whilethedigestionisproceeding,heatthe liquidreservoirandfilter-supportassemblyofthepressure-filtra
32、tionapparatus(4.2.2;seeFigure1)toapproximately 100C,eitherinanovenorbyuseofthehot-airblower(4.2.4). Whenthedigestionisapproachingcompletion,weighamembranefilterdisc(4.2.3)tothenearest0,1mgand insertitintotheheatedfilter-supportassembly.Assemblethefiltrationunitensuringthatitissatisfactorilygas-tight
33、. NOTE Themembranefilterdisctendstocurlupwhenplacedontheheatedfilter-supportassembly.Itishelpfultoplace themembranefilterdiscandthesiliconerubberO-ringsealwhichliesaboveitontotheheatedfilter-supportassemblyina singleoperation,thusholdingthemembranefilterdiscflatduringthesubsequentassemblyoftheappara
34、tus. 4.4.2 Placethemeasuringcylinder(4.2.7)undertheoutletofthepressurefiltration-assembly.Transferthe digestedmixtureofpitchandquinolinefromthebeakertotheliquidreservoirofthepressure-filtrationapparatus, usingasmallglassfunneltopreventanyoftheliquidfromenteringthegasline.Closethefilterunitandpressur
35、ize itwiththeinertgas(4.1.3),graduallyincreasingtheappliedpressureuntilthefiltratebeginstoflowintothe graduatedreceiver. NOTE1 Thefiltratetypicallybeginstoflowwhentheappliedgaspressurereaches0,12MPato0,14MPa. Allowthefiltrationtoproceedusingtheminimumappliedgaspressurewhichisconsistentwithasatisfact
36、oryflow rate.Usethevolumeofthecollectedfiltrateasaguidetotheprogressoffiltration.Iffiltrationisslow,maintainthe temperatureoftheliquid-containingpartofthepressure-filtrationapparatusatapproximately70Cto80Cbyuse ofthehot-airblower. NOTE2 Thefiltrationratewhichisachieveddependsverymarkedlyonthecharact
37、eristicsofthepitchbeingtested. Electrodebinderpitcheswhichhavehadlittleornothermalpolymerizationusuallygivesolutionswhichfilterreadilyinunder 1minwithanappliedgaspressureof0,13MPa.However,solutionsofpitcheswhichhavehadextensivethermaltreatment usuallyfiltermoreslowly,withfiltrationtimesupto1hbeingco
38、mmon.Inthesecases,itisessentialtokeepthefilterunithot duringfiltrationandoccasionaldepressurizationandrepressurizationofthefilterunitmayprovehelpful.Theuseofapplied pressuresaboveapproximately0,2MPadoesnotnormallyproduceanyusefulimprovementintherateoffiltration. 4.4.3 Whenthefiltrationofthequinoline
39、solutioniscomplete,depressurizethefiltrationapparatus,rinsethe beakerwithapproximately5mlofquinolineat70Cto80Candtransferthewashingsviatheglassfunneltothe filtrationapparatus.Closetheapparatusandgraduallyrepressurizeituntilfiltrationcommences.Thiswilltypically occuratapproximately0,1MPa.Adjusttheapp
40、liedpressuretoachieveasatisfactoryflowrate.Repeattherinsing ofthebeakerandthewashingoftheinsolublematteronthefilterafurtherninetimesusingapproximately5mlof quinolineat70Cto80Cforeachoperation,bywhichstagethewashingspassingintothegraduatedreceiver shouldbeverylittledarkerthanthedistilledquinoline(4.1
41、.1).Ifthewashingsarestilldeeplycoloured,continue washingwithfurtherportionsofhotquinolineuntiltheyshownofurtherlighteningofcolour.Washtheinsoluble matterinthepressure-filtrationapparatuswithtensuccessiveapproximately5mlportionsofthetoluene(4.1.2)at 70Cto80C,usinganappliedgaspressurereducedtoapproxim
42、ately0,01MPato0,02MPatoachievea controllableflowrate.Allowthefinalwashingstodrainfor1minto2min. 4.4.4 Weighthewatchglass(4.2.6)tothenearest0,1mg.Transferthemembranefilterdiscfromthepressure- filtrationapparatustothewatchglass.Ifanysignificantamountofthequinoline-insolublematteradherestothe O-ringsea
43、l,placethisonthewatchglassalso.Placethewatchglassandcontentsinanovenmaintainedat 105Cto110Cfor2h,thentransferthemtoadesiccatortocool. Ifquinoline-insolublematerialhasadheredtotheO-ringseal,gentlybrushthisontothewatchglass.Weighthe watchglasswiththemembranefilterdiscandthequinoline-insolublemattertot
44、henearest0,1mg.Usingforceps, holdthemembranefilterdisc,whichwillhaverolledintoatube,overthewatchglassanddetachasmuchadhering quinoline-insolublematteraspossiblebysharplytappingtheforceps.Holdthemembranefilterdiscflatonaclean, smoothpieceofpaperandremoveanyresidualquinoline-insolublematerialbycareful
45、lybrushing. Transfertherecoveredquinoline-insolublematerialtoacleanvialofsuitablesizetoawaitanalysis. NOTE Anartistssablebrush,size5hasbeenfoundtobesuitableforbrushingoffthequinoline-insolublematerial.ISO12979:1999(E) 4 Key 1Cap 2 Clampingrod 3 SiliconeO-ring 4 Pressurehoseconnector 5 SiliconeO-ring
46、 6 Perforatedsupportplate 7 Coarsemeshsupport 8 Outletconnector Figure1Typicalpressure-filtrationapparatus 4.4.5 Iftheamountofrecoveredquinoline-insolublematerialisinsufficientfortheensuinganalysis,repeatthe extractionwithamountsofpitchandquinolineincreasedproportionatelyuptoamaximumof5gofpitchand12
47、5ml ofquinolineforasingleextraction.Intheeventthattheincreasedamountsstillyieldaninadequatequantityof quinoline-insolublematter,repeattheentireextractionprocedureusingfurther5gportionsofthetestsampleuntil therequiredamountisobtained.ISO12979:1999(E)5 4.5 Calculationandexpressionofresults Calculateth
48、eyieldofquinoline-insolublematerial,w qi ,expressedasapercentagebymass,usingtheequation: 123 qi 45 100mmm w mm (1) where m 1 isthecombinedmassofthewatchglass,themembranefilterdiscandtheisolatedquinoline-insoluble material,ingrams; m 2 isthemassofthewatchglass,ingrams; m 3 isthemassofthemembranefilte
49、rdisc,ingrams; m 4 isthemassofthebeakercontainingthepitchsample,ingrams; m 5 isthemassoftheemptybeaker,ingrams. Expresstheresultofthecalculationtotwosignificantfigures. NOTE Thisresultshouldnotbequotedasthecontentofquinoline-insolublematterpresentinthepitchbecausethe quinoline-insolublematterisempirical.ISO6791shouldbeusedforthedeterminationofquinoline-insolublematter. 5 Analysisofquinoline-insolublematerialforcarbonandhydrogencontent 5.1 Reagents WarningRefertothereagentsuppliersHealthandSafetydatasheetsforth
