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1、TranslatedEnglishofChineseStandard:GBT1574-2007WWW.ChineseSSaIeSChineSeStandardnetGBNationalStandardofthePeople,sRepublicofChinaICS73.040D21GB/T1574-2007ReplacingGB/T1574-1995,GB/T4634-1996,GB/T18856.13-2002TestMethodforAnalysisofCoalAshGB/T1574-2007HowtoB喉灰fiih5旃PGETafull-copyofthisstandard?1. www.
2、ChineseS;2. Search-AddtoCart-Checkout(3-steps);3. Noactionisrequired-Full-copyofthisstandardwillbeautomatically&immediatelydeliveredtoyourEMAILaddressin025minutes.4. Support:SalesChineseS.Wayne,SalesmanagerIssuedon:November1,2007Implementedon:June1,2008Jointlyissuedby:GeneralAdministrationofQualityS
3、upervision,InspectionandQuarantine(AQSIQ);StandardizationAdministration(SAC)ofthePeoplesRepublicofChina.TableofContent1 Scope42 NormativeReferences43 Reagents44 InstrumentsandEquipment45 PreparationofAshSample56 Semi-microanalysisMethodofSilica,FerricOxide,TitaniumDioxide,AluminumOxide,CalciumOxidea
4、ndMagnesiumOxide56.1 PreparationofTestSolution56.2 DeterminationofSiliconDioxide(SiliconMolybdenumBlueSpectrophotometricMethod)66.3 ContinuousDeterminationofFerricOxideandTitaniumDioxide(SpectrophotometricMethodwithFerrotitaniumReagent)96.4 SeparateDeterminationofTitaniumDioxide(DiantipyrylMethaneSp
5、ectrophotometricMethod)126.5 DeterminationofAluminumOxide(ComplexometricTitrationwithVilliaumiteReplacingEDTA)146.6 DeterminationofCalciumOxide(EGTAComplexometricTitration)166.7 DeterminationofMagnesiumOxide(EDTAComplexometricTitration)187 Macro-analysisMethodofSiliconDioxide,FerricOxide,AluminumOxi
6、de,CalciumOxide,MagnesiumOxideandTitaniumDioxide207.1 DeterminationofSiliconDioxide(AnimalGlueCondensingMassMethod)207.2 ContinuousDeterminationofFerricOxideandAluminumOxide(ComplexometricTitrationwithEDTA)227.3 DeterminationofCalciumOxide(EDTAComplexometricTitration)267.4 DeterminationofMagnesiumOx
7、ide(ComplexometricTitrationwithEDTA,SubtractionMethod)287.5 DeterminationofTitaniumDioxide(SpectrophotometricMethodwithHydrogenPeroxide)308 DeterminationofSulfurTrioxide328.1 BariumSulfateMassMethod328.2 CombustionNeutralizationMethod348.3 CoulombTitration389 DeterminationofPhosphorusPentoxide(Phosp
8、horusMolybdenumBlueSpectrophotometricMethod)419.1 Method1419.2 Method24310 DeterminationofPotassiumOxideandSodiumOxide(FlamePhotometry).4611MethodforDeterminationofPotassium,Sodium,Ferrum,Calcium,MagnesiumandManganese(AtomicAbsorptionMethod)4812 TestReport53ForewordThisstandardreplacesGB/T1574-1995A
9、nalysisofCoalAsh,GBZT4634-1996DeterminationofPotassium,Sodium,Iron,Calcium,MagnesiumandManganeseinCoalAshbyAtomicAbsorptionSpectrometricMethod,andGB/T18856.13-2002TestMethodsforQualityofCoalWaterMixture-Part13:DeterminationfortheAshofCoalWaterMixture.Thisstandardintegratesthe3standards-GB/T1574-1995
10、,GB/T4634-1996andGB/T18856.13-2002.ComparedwithGB/T1574-1995,GB/T4634-1996andGB/T18856.13-2002,themainchangesofthisstandardareasfollows: Thevolumeofstandardworkingsolutionoftitaniumdioxidewasmodified(6.3.3.1inGB/T1574-1995;6.3.3.1.1inthisedition); Amethodtoseparatelydeterminetitaniumdioxidewasadded(
11、see6.4); Wrongunitsweremodified(9.1.2.10and9.1.2.11inGB/T1574-1995;9.2.2.10and9.2.2.11inthisedition); Errorsinformulaweremodified(9.2.7inGB/T1574-1995;Formula26in9.2.4ofthisedition); Contentofnotewasadded(see11.2); AppendixAintheformerstandard(GB/T4634-1996)wasdeleted.ThisstandardwasproposedbytheChi
12、naNationalCoalAssociation.ThisstandardshallbeunderthejurisdictionofNationalTechnicalCommitteeonCoalofStandardizationAdministrationofChina.Draftingorganizationofthisstandard:theCoalAnalysisLaboratoryofCoalResearchInstitute.Chiefdraftingstaffsofthisstandard:ZhangKerui,XiaHuili,ChenSuize,DengXiumin,Zho
13、uGuoyue1WangZhiqian,andSuiYan.Thepreviouseditionsreplacedbythisstandardareasfollows: GB1574-1979,GB/T1574-1995; GB/T4634-1984,GB/T4634-1996; GB/T18856.13-2002.TestMethodforAnalysisofCoalAsh1 ScopeThisstandardspecifiesthereagentsandmaterials,instrumentsandequipment,analysisprocedure,resultcalculation
14、andmethodprecisionforthedeterminationofferrum,calcium,magnesium,potassium,sodium,manganese,phosphorus,silicon,aluminum,titaniumandsulphurincoalash.Thisstandardisapplicabletocoal,coke,coalwaterslurryandcoalgangue.2 NormativeReferencesThefollowingdocumentscontainprovisionswhich,throughreferenceinthist
15、ext,constituteprovisionsofthisstandard.Fordatedreferences,subsequentamendments(excludingcorrection)orrevisionsofthesepublicationsdonotapply.However,thepartieswhoenterintoagreementaccordingtothesespecificationsareencouragedtoresearchwhetherthelatesteditionsoftheselabelsareapplicable.Foranyundatedrefe
16、rences,thelatesteditionofthedocumentreferredtoapplies.GB/T483GeneralRulesforAnalyticalandTestingMethodsofCoal3 ReagentsWatermentionedinthisstandardisdeionizedwaterordistilledwaterwithequivalentpurity.4 InstrumentsandEquipment4.1 Mufflefurnace:withtemperatureregulatingdevice,thermocouple,andpyrometer
17、;itcanmaintainat(81510)andshallhavecorrespondingconstant-temperaturearea;upperpartofitsbackwallischimneywithdiameterof25mm-30mm,lowerparthasahole(forinsertionofthermocouple)whosepositionshallbesuchthattheheatcontact-pointofthethermocouplecanbe20mm-30mmawayfromthefurnacebottom;aventilationhole(diamet
18、e匚about20mm)shallbeonthefurnacedoor.4.2 High-temperaturemufflefurnace:withtemperaturecontroldevice;itcanmaintainat(100010)oC.6.3ContinuousDeterminationofFerricOxideandTitaniumDioxide(SpectrophotometricMethodwithFerrotitaniumReagent)6.3.1 MethodsummaryUndertheconditionofpH=4.74.9,ferricionreactswithf
19、errotitaniumreagenttogeneratepurplecomplex;usespectrophotometricmethodtodetermineferricoxide.Addadequateamountofascorbicacid,sothatpurpleofthesolutiondisappears;titanicionreactswithferrotitaniumreagenttogenerateyellowcomplex,usespectrophotometricmethodtodeterminetitaniumdioxide.6.3.2 Reagentsandmate
20、rials6.3.2.1 Ascorbicacid.6.3.2.2 Ferrotitaniumreagentsolution:20gL.Weigh2gofferrotitaniumreagent(C6H48S2Na2);dissolveitintowater;diluteto100mLwithwater.6.3.2.3 Ammoniawater(GBT631):volumeratiois(1+6).6.3.2.4 Hydrochloricacid(GBT622)solution:volumeratiois(1+19).6.3.2.5 Sulfuricacidsolution:volumefra
21、ctionis50mLL.Measure5mLofsulfuricacid(GBT625);addwaterslowly;diluteto100mLwithwater.6.3.2.6 Buffersolution:pH=4.7.Weigh68gofsodiumacetatetrihydrate(CH3COONa3H2O)(GBT693)or41gofanhydrousSodiUmacetate(CHaCOONa)(GBT694);placeintoa400mLbeaker;addwatertodissolve;add29mLofglacialaceticacid(GBT676);dilutet
22、o1Lwithwater.6.3.2.7 Standardstocksolutionofferricoxide:1mgmL.Accuratelyweigh1.0000g(accurateto0.0002g)offerricoxideGRwhichhasbeendriedat105C110Cfor1h;placeitina400mLbeaker;add50mLofconcentratedhydrochloricacid(GBT622,GR);putonwatch-glass;heatituntiltheyaredissolved;cooldowntoroomtemperature;transfe
23、rintoa1Lvolumetricflask;dilutetothemarkwithwater;shakewell.6.3.2.8 Standardworkingsolutionofferricoxide:0.1mgmL.Accuratelypipet10mLofstandardstocksolutionofferricoxide;placeintoa100mLvolumetricflask;dilutetothemarkwiththehydrochloricacidsolution(6.3.2.4);shakewell.6.3.2.9 Standardstocksolutionoftita
24、niumdioxide:1mgmL.Accuratelyweigh0.5000g(accurateto0.0002g)oftitaniumdioxideGR;burnat10OOoCfor30min;putitina30mLporcelaincrucible;add8gofpotassium6.5DeterminationofAluminumOxide(ComplexometricTitrationwithVilliaumiteReplacingEDTA)6.5.1 MethodsummaryAddexcessiveEDTAsolutionintoweak-acidicsolution,soa
25、stoletittocomplexwithferrumion,aluminumionandtitaniumion,etc.;undertheconditionofpH=5.9,usexylenolorangeasindicator;usezincsalttodrop-addtheremainingEDTAsolution;thenaddvilliaumitetoreplacetheEDTAthatcomplexeswithaluminumandtitanium;usezincacetatestandardsolutiontotitrate;deducttheamountoftitanium,s
26、oastoobtaintheamountofaluminum.6.5.2 Reagents6.5.2.1 EDTAsolution:11gL.Weigh1.1gofEDTA(C10H14N28Na22H2O)(GBT1401);dissolveitintowater;anddiluteto100mLwithwater.6.5.2.2 Buffersolution:pH=5.9.Weigh200gofsodiumacetatetrihydrate(CH3COONa3H2O)(GBT693)or120.6gofanhydroussodiumacetate(CHaCOONa);dissolveiti
27、ntowater;add6.0mLofglacialaceticacid(GBT676);diluteto1000mLwithwater.6.5.2.3 Zincacetate:20gL.Weigh2gofzincacetateZn(CH3COO)22H2O(HG3-1098);dissolveitintowater;diluteto100mLwithwater.6.5.2.4 Potassiumfluoridesolution:100gL.Weigh10gofpotassiumfluoride(KF2H2O)(GB1271);dissolveitintowater;diluteto100mL
28、withwater;storeitintoapolyethylenebottle.6.5.2.5 Glacialaceticacid(GBT676)solution:volumeratiois(1+3).6.5.2.6 Ammoniawater(GBT631)solution:volumeratiois(1+1).6.5.2.7 Standardworkingsolutionofaluminumoxide:1mgmL.Placespectral-purealuminumsheetintoabeaker;use(1+9)hydrochloricacid(GBT622)solutiontosoak
29、anddissolveforfewminutes,sothatthesurfaceoxidationlayerisdissolved;usetiltingmethodtopouroutthehydrochloricacidsolution;usewatertocleanforseveraltimes;thenuseanhydrousethanol(GBT678)tocleanforseveraltimes;putitintoadryertodryfor4h.Anyoneofthefollowingmethodsmaybeselectedfortreatment.Method1(acid-dis
30、solutionmethod):accuratelyweigh0.5293g(accurateto0.0002g)ofaluminumsheetaftertreatment;placeitina150mLbeaker;add50mL(1+1)ofhydrochloricacid(GBT622)solution;heatitonelectricfurnaceatlowtemperatureuntilitdissolves;transferthesolutionintoa1000rLvolumetricflask;dilutetothemarkwithwater;shakewell.Method2
31、(alkali-dissolutionmethod):accuratelyweigh0.5293g(accurateto0.0002g)ofaluminumsheetaftertreatment;placeitina150mLbeaker;add2gofpotassiumhydroxide(HGB3006)Addsodiumhydroxideintoashsampleformelting;placeitintoboilingwaterforleaching;acidifyitwithhydrochloricacid;evaporateittodryness;inthemediumofhydro
32、chloricacid,useanimalgluetocondensesilicicacid;precipitateandfilterit;burnandweighit.7.1.2 Reagentsandmaterials7.1.2.1 Sodiumhydroxide(GB6629):granular.7.1.2.2 Hydrochloricacid(GBT622).7.1.2.3 95%ethanol(GBT679)orabsoluteethanol(GBT678).7.1.2.4 Hydrochloricacidsolution:volumeratiois(1+1).7.1.2.5 Hyd
33、rochloricacidsolution:volumeratiois(1+3).7.1.2.6 Hydrochloricacidsolution:volumeratiois(1+50).7.1.2.7 Animalgluesolution:10gL.Weigh1gofanimalglue;placeinto100mLofwaterat7080.Itshallbepreparedimmediatelybeforeuse.7.1.3 Testprocedure7.1.3.1 Weigh0.480.52g(accurateto0.0002g)ofashsample;placeintoasilver
34、crucible;wetitwithafewdropsofethanol(7.1.2.3);add4gofsodiumhydroxide;putoncruciblecover;putitintomufflefurnace(4.1);risefurnacetemperatureslowlyfromroomtemperatureto650C700in11.5h;meltfor1520min.Takeitoutcooldownwithwater;wipeupouterwallofthecrucible;placeitintoa250mLbeaker;add1mLofethanol(7.1.2.3)a
35、ndadequateamountofboilingwater;immediatelyputonwatch-glass.Afterseverereactionstops,usehydrochloricacidsolution(7.1.2.4)andhotwatertoalternatelycleanthecrucibleanditscover;add20mLofhydrochloricacidsolution(7.1.2.2);shakewell.7.1.3.2 Placethebeakeronthehotplate;slowlyevaporateittodryness(withyellowsa
36、ltparticle);takeitdown.Aftercooling;add20mLofhydrochloricacidsolution(7.1.2.2);putonwatch-glass;heatittoabout80;add10mLofanimalgluesolutionat7080;stiritsharplyfor1min;keepitwarmfor10min;takeitout;cooldown;addabout50mLofhotwater;stiritsothatthesaltisfullydissolved;filteritwithquantitativefilterpaperi
37、ntoa250mLvolumetricflask;washthesedimentwithhydrochloricacid(7.1.2.5)for45times;wipeupthecupwallandglassrod(withrubberhead)withhothydrochloricacidsolution(7.1.2.6);washthesedimentfor35times;thenwashitwithhotwaterforabout10times.7.1.3.3 Transferthesedimentandfilterpaperintoaporcelaincruciblethathasbe
38、enconstantweight;incineratethefilterpaperatlowtemperature;thenburninhigh-temperaturemufflefurnace(4.2)of1000oC20for1h;takeitoutandcooltitratetheresultantofcalciumandmagnesium.1.1.1.1 Reagent7.4.2.1 Triethanolaminesolution:volumeratiois(1+4).7.4.2.2 Ammonia(GBT631)solution:volumeratiois(1+1).7.4.2.3
39、Sodiumdiethyldithiocarbamate(referredtoascupron)solution:50gL.Weigh2.5gofcupron(HG3-962);dissolveitinwater;addfivedropsofammoniasolution(7.4.2.2);dilutewithwaterto50mL;storeinabrownbottleafterbeingfilteredwithrapidfilterpaper.7.4.2.4 Sodiumpotassiumtartratetetrahydratesolution:100gL.Weigh10gofsodium
40、potassiumtartratetetrahydrate(GBT1288);dissolveitinwater;diluteto100mLwithwater.7.4.2.5 EDTAstandardsolution:asspecifiedin7.3.2.4.TiterT(MgO)ofthesolutiontomagnesiumoxideisconvertedaccordingtoFormula(18):T(MgO)=0.7187T(CaO)(18)Where,T(CaO)thetiterofEDTAstandardsolutiontocalciumoxide,inmg/mL;0.7187th
41、efactorbywhichcalciumoxideisconvertedtomagnesiumoxide.7.4.2.6 AcidchromeblueK-naphtholgreenBmixedindicates:Weigh0.50gofacidchromeblueK(HG10-1282)and1.25gofnaphtholgreenB;uniformlygrindthemwithpotassiumchloride(GBT646)thathasbeenpre-driedat110;putintoaflaskwithgroundmouth;storeinadryer.Orrespectively
42、preparethenintowatersolutions,namely,weigh0.04gofacidchromeblueKand0.08gofnaphtholgreenB;respectivelydissolvetheminto20mLofwater;priortouse,propermixtureratioshallbeconfirmedthroughexperiment.SinceacidchromeblueKsolutionisunstable,itshallbepreparedimmediatelybeforeuse.1.1.1.2 AnalysisprocedureAccura
43、telypipet10mLofsolutionCand10mLofsolutionD;respectivelypourtheminto250mLbeakers;dilutetoabout10OmLwithwater;add10mLoftriethanolaminesolution(ifthecontentoftitaniumdioxideisgreaterthan4.00%,5mLofsodiumpotassiumtartratetetrahydratesolutioncanbeaddedinadvance),10mLofammoniasolution,and1dropofsodiumpota
44、ssiumtartratetetrahydrate;uniformlymixeachreagentadded;addintheamountofEDTAstandardsolution(7.3.2.4)thatisslightlylessthanthatconsumedintheprocessofcalciumtitration;thenaddasmallamountofacidchromeblueK-naphtholgreenBmixedindicator,orseveraldropsofliquid1.1.1.3 Ammonia(GBT631)solution:volumeratiois(1
45、+1).1.1.1.4 Hydrochloricacid(GBT622)solution:volumeratiois(1+1).1.1.1.5 Bariumchloridesolution:100gL.Weigh10gofbariumchloride(GBT652);dissolveitinwater;diluteto100mLwithwater.1.1.1.6 Silvernitratesolution:10g/L.Weigh1gofsilvernitrate(GBT670);dissolveitinwater;diluteto100mLwithwater;addseveraldropsof
46、nitricacid(GBT626);storeinabrownbottle.1.1.1.7 Methylorangeindicator:2gL.Weigh0.2gofmethylorange;dissolveinwater;diluteto100mLwithwater.1.1.1.8 Filterpaper:medium-speedqualitativefilterpaper.1.1.1.9 Filterpaper:slow-speedqualitativefilterpaper.8.1.3Analysisprocedure8.1.3.1 Weigh0.2g0.5gofashsample(a
47、ccurateto0.0002g);placeitina250mLbeaker;add50mLofhydrochloricacidsolution(8.1.2.1);putwatch-glasson;heatupfor20min;thentakeitdown;addtwodropsofmethylorangeindicatorwhilethesolutionisstillwarm;neutralizethesolutionbyinjectingammoniawateruntilthesolutionjustchangescolor;thenaddexcessivethreetosixdrops
48、.Afterferrichydroxideprecipitates,filterthesolutionina300mLbeakerwithmedium-speedqualitativefilterpaper(8.1.2.7);usenearly-boiledhotwatertocleanandprecipitatefor10to12times;drop-addhydrochloricacidsolution(8.1.2.3)intothefilteredsolutionuntilthesolutionjustchangescolor;thenaddexcessive2mL;dilutethesolutiontoabout250mLwithwater.8.1.3.2 Heatthesolutiontoboil;drop-add10mLofbariumchloridesolutionwithcontinuousstirring;slightlyboilito
