英文版GBT 15072.4-2008国标《贵金属合金化学分析方法 钯、银合金中钯量的测定 二甲基乙二醛肟重量法 》

PAGE\*MERGEFORMAT8ICS77.120.99H68NationalStandardofthePeople’sRepublicofChinaGB/T15072.4-2008ReplacesGB/T15072.4-1994TestmethodofpreciousmetalalloysDeterminationofpalladiumcontentforpalladiumandsilveralloysButanedionedioximegravimetry贵金属合金化学 分析 定性数据统计分析pdf销售业绩分析模板建筑结构震害分析销售进度分析表京东商城竞争战略分析 方法钯、银合金中钨钯量的测定二甲基乙二醛肟重量法(EnglishTranslation)Issuedate:2008-03-31Implementationdate:2008-09-01IssuedbyGeneralAdministrationofQualitySupervision,InspectionandQuarantineofthepeople'sRepublicofChinaStandardizationAdministrationofthepeople'sRepublicofChinaForewordSAC/TC243isinchargeofthisEnglishtranslation.IncaseofanydoubtaboutthecontentsofEnglishtranslation,theChineseoriginalshallbeconsideredauthoritative.ThisstandardisanintegratedrevisionofGB/T15072-1994(Chemicalanalysismethodsforpreciousmetalsandtheiralloys)(allparts),whichisdividedinto19parts:—GB/T15072.1-2008TestmethodsofpreciousmetalalloysDeterminationofgoldcontentforgold,platinumandpalladiumalloyspotentiometrictitrationwithferroussulfate.—GB/T15072.2-2008TestmethodsofpreciousmetalalloysDeterminationofsilvercontentforsilveralloyspotentiometrictitrationwithsodiumchloride.—GB/T15072.3-2008TestmethodsofpreciousmetalalloysDeterminationofplatinumcontentforgold,platinumandpalladiumalloysCurrenttitrationwithpotassiumpermanganate.—GB/T15072.4-2008TestmethodsofpreciousmetalalloysDeterminationofpalladiumcontentforpalladiumandsilveralloysbutanedionedioximegravimetry.—GB/T15072.5-2008TestmethodsofpreciousmetalalloysDeterminationofsilvercontentforgoldandpalladiumalloyspotentiometrictitrationwithpotassiumiodide.—GB/T15072.6-2008TestmethodsofpreciousmetalalloysDeterminationofiridiumcontentforplatinumandpalladiumalloyspotentiometrictitrationwithferroussulfate.—GB/T15072.7-2008TestmethodsofpreciousmetalalloysDeterminationofchromiumandironcontentsforgoldalloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.8-2008TestmethodsofpreciousmetalalloysDeterminationofcoppercontentforgold,palladiumandsilveralloysEDTAcomplexometricbacktitrationwiththioureaprecipitation.—GB/T15072.9-2008TestmethodsofpreciousmetalalloysDeterminationofindiumcontentforgoldalloysEDTAcomplexometricbacktitration.—GB/T15072.10-2008TestmethodsofpreciousmetalalloysDeterminationofnickelcontentforgoldalloysEDTAcomplexometricbacktitration.—GB/T15072.11-2008TestmethodsofpreciousmetalalloysDeterminationofgadoliniumandberylliumcontentsforgoldalloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.12-2008TestmethodsofpreciousmetalalloysDeterminationofvanadiumcontentforsilveralloysHydrogenperoxidespectrophotometry.—GB/T15072.13-2008TestmethodsofpreciousmetalalloysDeterminationoftin,ceriumandlanthanumcontentsinsilveralloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.14-2008TestmethodsofpreciousmetalalloysDeterminationofaluminiumandnickelcontentsforsilveralloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.15-2008TestmethodsofpreciousmetalalloysDeterminationofnickel,zincandmanganesecontentsforgold,silverandpalladiumalloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.16-2008TestmethodsofpreciousmetalalloysDeterminationofcopperandmanganesecontentsforgoldalloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.17-2008TestmethodsofpreciousmetalalloysDeterminationoftungstencontentforplatinumalloysTungstentrioxidegravimetry.—GB/T15072.18-2008TestmethodsofpreciousmetalalloysDeterminationofzirconiumandgalliumcontentsforgoldalloysInductivelycoupledplasmaatomicemissionspectrometry.—GB/T15072.19-2008TestmethodsofpreciousmetalalloysDeterminationofvanadiumandmagnesiumcontentsforsilveralloysInductivelycoupledplasmaatomicemissionspectrometry.ThispartisthefourthofGB/T15072-2008.ThispartreplacesGB/T15072.4-1994(MethodsforChemicalAnalysisofPreciousMetalsandTheirAlloysPalladium,silveralloysDeterminationofpalladiumcontent).ThefollowingdeviationshavebeenmadewithrespecttotheGB/T15072.4-1994(thepreviousedition):—ThetitleofstandardischangedfromMethodsforChemicalAnalysisofPreciousMetalsandTheirAlloysPalladium,silveralloysDeterminationofpalladiumcontenttoTestmethodofpreciousmetalalloysDeterminationofpalladiumcontentforpalladiumandsilveralloysButanedionedioximegravimetry.—ThescopeofthestandardisextendedfromPdIr10,PdIr18,PdAgCuAuPtZn30-14-10-10-1,PdAgCu69-27,PdAgCu58-32,PdAgCu65-20,PdAgCu52-28,PdAgCu54-21,AgPd20,AgPd60ofthepreviouseditiontothisstandardisapplicabletothedeterminationofpalladiumcontentforalloysofPdIr,PdAgCu,PdAgCuAuPtZnandAgPd. The determination range of this standard(mass fraction)is4%to92%.—ThispartisdraftedinaccordancewiththerulesgivenintheGB/T20001.4-2001.ThispartwasproposedbyNonferrousMetalsIndustryAssociationofChina;ThispartwaspreparedbySAC/TC243ChineseNonferrousMetalStandardizationTechnicalCommittee.ThispartisexplainedbythenationalnonferrousmetalStandardizationTechnicalCommittee.Thepreviouseditionofthisstandardisasfollow:—GB/T15072.4-1994.TestmethodofpreciousmetalalloysDeterminationofpalladiumcontentforpalladiumandsilveralloysButanedionedioximegravimetryScopeThispartspecifiesamethodforthedeterminationofpalladiumcontentinpalladiumandsilveralloys.Thispartisapplicabletodeterminationofpalladiumcontentsbetween4%-92%inPdIr,PdAgCu,PdAgCuAuPtZnandAgPdalloys.NormativereferencesThefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthis,constituteprovisionsofthispart.Fordatedreferences,subsequentamendments(excludingcorrections),orrevisions,ofanyofthesepublicationsdonotapplytothispart.Howeverpartiestoagreementsbasedonthispartareencouragedtoinvestigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.YS/T371MethodsforchemicalanalysisofpreciousmetalsalloysGeneralrulesandregulations.MethodabstractThetestportionofPdIrandPdAgCuAuPtZnalloysshallbedissolvedwithmixtureacidofhydrochloricacidandnitricacid.PdAgCuandAgPdalloysshallbedissolvedwithnitricacid.Goldalloyshouldbereducedandseparatedbysodiumnitrite,andsilveralloyshouldbeseparatedbysilverchlorideprecipitation.Pdalloyshouldbeprecipitatedbybutanedionedioximein dilutehydrochloricacid.Themass fractionofpalladiumshouldbedeterminedbygravimetry.ReagentandmaterialUnlessotherwisenoted,reagentsandutensilareinaccordancewithYS/T371.4.1Sodiumchloride.4.2Hydrochloricacid(ρ1.19g/mL).4.3Nitricacid(ρ1.42g/L).4.4Aceticacid(ρ1.05g/L).4.5Ammoniumhydroxide(ρ0.90g/L).4.6Hydrochloricacid solution(1+1).4.7Hydrochloricacid solution(1+9).4.8Hydrochloricacid solution(2+98).4.9Mixed acid:3unitvolumehydrochloricacid(4.2)mixed with1unitvolumenitricacid(4.3),prepareitjustbeforeusing.4.10Mixed acid:30unitvolumehydrochloricacid(4.2)mixed with1unitvolumenitricacid(4.3),prepareitjustbeforeusing.4.11Ammoniumhydroxide(1+1).4.12Sodiumnitritesolution(100g/L).4.13Sodiumnitritesolution(10g/L).4.14Sodiumhydroxidesolution(100g/L).4.15Butanedionedioximeethanolsolution(10g/L).Thymolbluesolution(1g/L):weigh0.1gthymolblueina100mLbeaker,add2.2mLsodiumhydroxidesolution(4.13)anddiluteto100mLwithwater.SampleAlloysampleshouldbe rolledintothinsheetsofthicknessnotgreaterthan0.3mm,removeoilstainswithacetone,andcutintodebris,washedwithwater,driedandmixedwell.Analysisprocedure6.1TestportionWeighthetestportionaccordingtoTable1,accurateto0.00001g.Table1Mass fractionofpalladium/%Testportion/g>4.00to10.000.40>10.00to40.000.13>40.00to92.000.036.2DeterminationofthenumberTwoindependentdeterminationsshouldberequired,andaveragetheresults.6.3Determination6.3.1Dissolvingoftheportion6.3.1.1ThePdIralloyportionshouldbeplacedina400mLbeaker,thencoverthesurfacedishandadd10mLmixed acid(4.9)whichwasmixedbyhydrochloricacidandnitricacid,Heatingthesolutionatlowtemperatureuntiltestportioncompletelydissolved,thenremove,cool,washsurfacedishandbeakerwallwithwater.Afterthat,adding0.1gsodiumchlorideandevaporatethesolutiontoprecipitationofmoistsalt.Adding10mLhydrochloricacid(4.2)andevaporatethesolutiontoprecipitationofmoistsalt.Itshouldberepeated2times.6.3.1.2ThePdAgCuAuPtZnalloyportionshouldbeplacedina250mLbeaker,thencoverthesurfacedishandadd10mLhydrochloricacid(4.10).Heatingthesolutionatlowtemperatureuntiltestportioncompletelydissolved,thenremove,cool,washsurfacedishandcupwallwithwater.Afterthat,adding0.1gsodiumchlorideandevaporatethesolutiontoprecipitationofmoistsalt.Adding10mLhydrochloricacid(4.2)andevaporatethesolutiontoprecipitationofmoistsalt.Itshouldberepeated2times.6.3.1.3ThePdAgCuandAgPdalloysportionshouldbeplacedina250mLbeaker,thencoverthesurfacedishandadd10mLnitricacid(4.3).Heatingthesolutionatlowtemperatureuntiltestportioncompletelydissolved,thenremove,cool,washsurfacedishandcupwallwithwater.Afterthat,adding0.1gsodiumchlorideandevaporatethesolutiontoprecipitationofmoistsalt.Adding10mLhydrochloricacid(4.2)andevaporatethesolutiontoprecipitationofmoistsalt.Itshouldberepeated2times.6.3.2Separation6.3.2.1Adding10mLhydrochloricacid(4.2)and200mLwatertotheresidue(6.3.1.1),andadd15mLbutanedionedioximeethanolsolution(4.15)withagitate,stirringfor3minandstill standingfor1h.6.3.2.2Adding4mLhydrochloricacidsolution(4.5)and100mLwatertotheresidue(6.3.1.2),Itshallbeheatedtoboiluntilsilverchlorideprecipitatedandagglomerated,placingthesolutionfor4hinthedark.Filteringwithmediumspeedfilterpaper,washingthebeakerandprecipitate6timeseachwithhydrochloricacidsolution(4.8),washingthebeakerandprecipitate2timeseachwithwater,discardingtheprecipitate.Adding2dropsofthymolbluesolution(4.16)tothefiltrate,thesolutionshallbeadjustedfromredtoorange(pH2)withsodiumhydroxidesolution(4.14),heatingtoboil,adding10mLsodiumnitritesolution(4.12)withagitate,thenboilthesolutionfor30minuntilgoldwasabletoprecipitatedandagglomerated.Filteringwithdensefilterpaperwhileitwashot,thebeakerandprecipitateshallbewashed5timeseachwithhotsodiumnitritesolution(4.13).Adding5mLhydrochloricacidsolution(4.6)intothebeakerandfilterpaper,thebeakerandprecipitateshallbewashed10timeseachwithhotwater,discardingtheprecipitate.Heatingthefiltrateandboilitfor1h.Thesolutionshallbeevaporatedtoprecipitationofmoistsalt.Adding10mLhydrochloricacid(4.2)andevaporatethesolutiontoprecipitationofmoistsalt.Itshallberepeated3times.Adding10mLhydrochloricacid(4.2)and200mLwater,thenadd10mLbutanedionedioximeethanolsolutionwithagitate,stirringfor3minandstill standingfor1h.6.3.2.3ThePdAgCuresidue(6.3.1.3)shallbeseparatedfromsilverinaccordancewiththeoperation(6.3.2.2),adding8mLhydrochloricacid(4.2)tothefiltrate,andwaterwasaddedtothetotalvolumeof200mL.Addbutanedionedioximeethanolsolution(4.15)withagitate,stirringfor3minandstill standingfor1h.6.3.2.4Adding100mLwatertotheAgPdresidue(6.3.1.3),adding10mLammoniasolution(4.11)withagitate.Untilyellowcolorofthesolutiondisappears(ifthepinkprecipitationisproduced,itshouldbeheatedslightlytodissolvedtheprecipitation),andthendroppingaceticacid(4.4)toadjustthesolutiontopH6.Adding5mLhydrochloricacidsolution(4.7),stirringfor3min,remove,andstill standingfor4hinthedark.Filteringwithmediumspeedfilterpaper,Thebeakerandprecipitateshallbewashed6timeseachwithhydrochloricacidsolution(4.8),Afterthat,washingthebeakerandprecipitate2timeseachwithwater,discardingtheprecipitate.Adding5mLhydrochloricacid(4.2)withagitate,andheatedtoboilfor5min,removeandcool.Addingwateruntilthetotalvolumeis200mL,addingbutanedionedioximeethanolsolutionwithagitate,stirringfor3minandstill standingfor1h.6.3.3 HYPERLINK"javascript:;"FiltrationTheprecipitationofbutanedionedioximepalladium(6.3.2.1,6.3.2.2,6.3.2.3,6.3.2.4)shallbevacuumfiltratedinaNo.4glasssandfiltercruciblewhichweredriedat110℃toconstantweight.Thebeakerandprecipitateshallbewashed10timeseachwithhydrochloricacid solution(4.8).Scrubbingtheedgeofthebeakerwithaglassrodwithrubberhead,thenwashthebeakerandprecipitate5timesinhotwateratabout85℃.6.3.4ConstantweightThecrucible(6.3.3)shallbedriedat110℃for1h.Removingandplaceinthedryerfor30min.Thenweighthedryermanytimesuntilconstantweight.7CalculationofanalysisresultsThemassfractionofpalladiumωPdshouldbecalculatedaccordingtoformula(1),andthevalueisexpressedas%:ωPd=（m1-m2）×0.3161m0×100----------------------(1)Intheformula:m1isthemassofbutanedionedioximepalladiumandcrucibleingrams(g).m2isthemassofthecrucibleingrams(g).m0isthemassofportioningrams(g).0.3161istheconversionofbutanedionedioximepalladiumtopalladium.Theresultsshouldbeexpressedtotwodecimalplaces.8Tolerance1Differencesbetweenlaboratoryanalysisresultsallowableshouldbenotmorethanlistedintable2.Table2.%MassfractionofpalladiumTolerance1>4.00~10.000.10>10.00~40.000.20>40.00~92.000.30