BS EN 13615-2001 Methods for the analysis of ingot tin - Determination of impurity element contents in tin grades 99 90 % and 99 85 % by atomic spectrometry《金属铸块锡的分析方法 原子吸收光谱测定法测定9.pdf

1、Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIBRITISH STANDARD BS EN 13615:2001 Methods for the analysis of ingot tin Determination of impurity element contents in tin grades 99,90 % and 99,85 % by atomic spectrometry The Europe

2、an Standard EN 13615:2001 has the status of a British Standard ICS 77.040.30; 77.150.60 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIBS EN 13615:2001 This British Standard, having been prepared under the direction of the Engine

3、ering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 23 July 2002 BSI 23 July 2002 ISBN 0 580 40129 4 National foreword This British Standard is the official English language version of EN 13615:2001. The UK participation in

4、its preparation was entrusted to Technical Committee NFE/27, Tin and tin alloys, which has the responsibility to: 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 public

5、ations referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the nece

6、ssary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the inte

7、rpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 15 and a back cover. The BSI co

8、pyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIEUROPEANSTANDARD NORMEEUROPENNE EUROPI

9、SCHENORM EN13615 December2001 ICS77.040.30;77.150.60 Englishversion MethodsfortheanalysisofingottinDeterminationofimpurity elementcontentsintingrades99,90%and99,85%byatomic spectrometry MthodespourlanalysedeslingotsdtainDtermination desteneursenimpuretsdansltaindequalit99,90%et 99,85%parspectromtrie

10、atomique VerfahrenfrdieAnalysevonZinninMasseln BestimmungdesGehaltesanVerunreinigungselementenin ZinnderReinheitsgrade99,90%und99,85%durch Atomspektrometrie ThisEuropeanStandardwasapprovedbyCENon5October2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsf

11、orgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioni

12、nanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembo

13、urg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMe

14、mbers. Ref.No.EN13615:2001E Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIEN13615:2001(E) 2 Contents page Foreword .3 1 Scope3 2 Normativereferences 3 3 Principle .3 4 Reagents 4 5 Apparatus.6 6 Sampling 6 7 Procedure.6 7.1 Prep

15、arationofthesolutionofthesampleundertest6 7.2 Preparationofcalibrationsolutions 6 7.3 Certifiedreferencematerials(CRM)7 7.4 Spectrometricmeasurements 7 8 Expressionofresults. .7 8.1 Determiningthemetalcontent . .7 8.2 Evaluationofprecision. 8 9 Testreport. .8 AnnexA (normative) Methodforcheckingatom

16、icabsorptionspectrometerperformance (basedonISO75301:1990) . 9 AnnexB (normative) Methodforcheckinginductivelycoupledplasmaatomicemission spectrometerperformance.12 Bibliography .14 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSI

17、EN13615:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC220“Tinandtinalloys”the secretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyJune2002,andconflictingnationa

18、lstandardsshallbe withdrawnatthelatestbyJune2002. TheannexesAandBarenormative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ir

19、eland,Italy,Luxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. 1Scope ThisEuropeanStandardspecifiesatomicspectroscopicmethods(AtomicAbsorptionSpectrometry (AAS)orinductivelycoupledplasmaAtomicEmissionSpectrometry(ICPAES)intendedforthe analysisofingottin.Itiswrittenf

20、orusebyexperiencedanalystsfamiliarwithatomicspectrometric techniques. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromother publications.Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthe publicationsarelistedhereafter.Fordatedreferen

21、ces,subsequentamendmentstoorrevisionsofany ofthesepublicationsapplytothisEuropeanStandardonlywhenincorporatedinitbyamendmentor revision.Forundatedreferencesthelatesteditionofthepublicationreferredtoapplies(including amendments). EN610, TinandtinalloysIngottin. 3Principle Thetestsampleisdissolvedinhy

22、drochloricacidplusnitricacidandtartaricorcitricacid,andthe concentrationoftheelementsoughtismeasuredusingatomicabsorptionspectrometryorinductively coupledplasmaatomicemissionspectrometry.Interferenceisminimisedbymatchingsampleand referencematerialsandbythechoiceofinstrumentparameters. Licensed Copy:

23、 Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIEN13615:2001(E) 4 4Reagents 4.1General Duringtheanalysis,unlessotherwisestated,useonlyreagentsofrecognisedanalyticalgradeand onlydistilledwaterorwaterofequivalentpurity. 4.2 Hydrochloricacid ,conc

24、entrated( 1,18g/ml). 4.3 Dilutehydrochloricacid (1+1) .Dilute100mlhydrochloricacid( 4.2)with100mlwater. WARNING Theacidshouldaddedtothewaterforsafetyreasons. 4.4 Dilutehydrochloricacid (1+19). Dilute10mlhydrochloricacid( 4.2)with190mlwater. 4.5 Nitricacid ,( 1,42g/ml). 4.6 Sulphuricacid ,( 1,84g/ml)

25、. 4.7 Tartaricacidorcitricacid . 4.8 Acidmixture .Add250mlhydrochloricacid( 4.2)to250mlwater.Cool.Add250mlnitricacid( 4.5) and50gtartaric(orcitric)acid( 4.7).Diluteto1lwithwater. 4.9 Dilutenitricacid(1+1) .Add100mlnitricacid( 4.5)to100mlwater. 4.10 Dilutenitricacid(1+4) .Add50mlnitricacid( 4.5)to200

26、mlwater. 4.11 Dilutenitricacid(1+9) .Add25mlnitricacid( 4.5)to225mlwater. 4.12 Dilutenitricacid(1%) .Dilute5mlnitricacid( 4.5)upto500ml. 4.13 Standardsolutionsofmetals.Freshlypurchasedstandardmetalsolutionsmaybeusedor standardmetalsolutionsshouldbemadeupasfollows( 4.13.1to 4.13.25). 4.13.1 Standarda

27、ntimonysolution(1 mlcontains1 mgSb) .Place0,10 gSbin5 mlsulphuric acid( 4.6)andheattocompletedissolution.Cool.Carefullyaddapproximately10mlwaterandcool again.Transfertoa100mlvolumetricflaskwithdilutehydrochloricacid(1+1)( 4.3). 4.13.2 Standardantimonysolution(1mlcontains0,2mgSb) .Transfer10,00mlofSb

28、solution 4.13.1 toa50mlvolumetricflaskandmakeuptovolumewithdilutehydrochloricacid(1+1)( 4.3). 4.13.3 Standardcoppersolution(1mlcontains1mgCu) .Dissolve0,10gCuin10mldilutenitric acid(1+4)( 4.9)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.4 Standardcoppersolution(1mlcontains0

29、,2mgCu) .Transfer10,00mlofCusolution 4.13.3 toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.5 Standardleadsolution(1mlcontains1mgPb) .Dissolve0,10gPbin10mldilutenitricacid (1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.6 Standardleadsolution(1mlcontai

30、ns0,1mgPb) .Transfer5,00mlofPbsolution 4.13.5toa 50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.7 Standardbismuthsolution(1mlcontains1mgBi) .Dissolve0,10gBiin10mldilutenitric acid(1+1)( 4.9)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. Licensed Copy: Wang Bin, ISO/Exch

31、ange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIEN13615:2001(E) 5 4.13.8 Standardbismuthsolution(1mlcontains0,1mgBi) .Transfer5,00mlofbismuthsolution 4.13.7 toa50mlvolumetricflaskandmakeuptovolumewithdilutehydrochloricacid(1+1)( 4.3). 4.13.9 Standardcadmiumsoluti

32、on(1mlcontains1mgCd) .Dissolve0,10gCdin10mldilutenitric acid(1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.10 Standardcadmiumsolution(1 mlcontains0,01 mgCd) .Transfer1,00 mlofcadmium solution4.13.9toa100mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.11 St

33、andardzincsolution(1mlcontains1mgZn).Dissolve0,10 gZnin10 mlnitricacid (1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.12 Standardzincsolution(1mlcontains0,01mgZn) .Transfer1,00mlofzincsolution 4.13.11 toa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.13

34、Standardironsolution(1mlcontains1mgFe) .Dissolve0,10gFewire(freefromrust)in 10mlofnitricacid(1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewith waterandmix. 4.13.14 Standardironsolution(1mlcontains0,02mgFe) .Transfer1,00mlofironsolution 4.13.13 toa50mlvolumetricflask.Makeuptovolumewith

35、waterandmix. 4.13.15 Standardarsenicsolution(1mlcontains1mgAs) .Dissolve0,1320gofAs 2 0 3 inalittle sodiumhydroxidesolution(1mol/l)andtransfertoa100mlvolumetricflask.Makeuptovolumewith waterandmix. 4.13.16 Standardarsenicsolution(1mlcontains0,1mgAs) .Transfer5,00mlarsenicsolution 4.13.15 toa50mlvolu

36、metricflask.Makeuptovolumewithwaterandmix. 4.13.17 Standardaluminiumsolution(1mlcontains1mgAl).Dissolve0,100gAlmetalin10ml nitricacid( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.18 Standardaluminiumsolution(1 mlcontains0,05 mgAl) .Transfer5,00 mlofaluminium solution4

37、.13.17toa100mlvolumetricflaskandmakeuptovolumewithdilutenitricacid(1%) (4.12). 4.13.19 Standardaluminiumsolution(1mlcontains0,005mgAl).Transfer5,00mlofaluminium solution4.13.18toa50mlvolumetricflaskandmakeuptovolumewithdilutenitricacid(1%)( 4.12). 4.13.20 Standardsilversolution(1mlcontains1mgAg).Dis

38、solve0,787gsilvernitratein50ml water.Transfertoa500mlvolumetricflaskandmakeuptovolumewithnitricacid(1%)( 4.12). 4.13.21 Standardsilversolution(1mlcontains0,1mgAg) .Transfer5,00mlofsilversolution( 4.13.20) toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.22 Standardnickelsolution(1mlconta

39、ins1,0mgNi) .Dissolve0,100gofnickelin10mlof nitricacid(1+4)(4.10)andtransfertoa100mlvolumetricflaskandmakeuptovolumewithwater andmix. 4.13.23 Standardnickelsolution(1mlcontains0,1mgNi) .Transfer5,00mlofnickelsolution 4.13.22 toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.24 Standardind

40、iumsolution(1mlcontains1,0mgIn) .Dissolve0,100gofindiumin10mlof nitricacid(1+4)( 4.10)andtransfertoa100mlvolumetricflaskandmakeuptovolumewithwater andmix. 4.13.25 Standardindiumsolution(1mlcontains0,1mgIn) .Transfer5,00mlofindiumsolution 4.13.24 toa50mlvolumetricflaskandmakeuptovolumewithdilutenitri

41、cacid(1%)( 4.12). Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 04 December 2002, Uncontrolled Copy, (c) BSIEN13615:2001(E) 6 4.14 Tin,min.purity99,99%. 5Apparatus 5.1 Ordinarylaboratoryapparatus .UsegradeAglassware. 5.2 Burette,ofcapacity5ml,graduatedin0,02ml. 5.3 Atomic

42、absorptionspectrometerorinductivelycoupledplasmaatomicemissionspectrometer , conformingtotheperformancerequirementsinnormativeannexesAandB. 5.4 Hollowcathodelampsorelectrodelessdischargetubesforantimony,bismuth,cadmium, copper,lead,silver,iron,zinc,arsenic,nickel,aluminium,indium,goldandcobalt . NOT

43、E Thepresenceofotherelementsmayalsoneedtobeascertained. 6Sampling ThesampleforanalysisshallbeobtainedasdescribedinEN610. 7Procedure 7.1 Preparationofthesolutionofthesampleundertest 7.1.1 Weigh1,0g0,1gofthesampleandtransfertoa250mlbeaker.Add20mloftheacid mixture( 4.8),heattocompletedissolutionandcool.Transfertoa100mlvolumetricflaskandmake uptothevolumewithdilutehydrochloricacid(1+19)( 4.4)andmix. 7.1.2 Prepareablanktestsolutionfollowingtheproceduredescribedin 7.1.1,butusing1,0gof highpuritytin( 4.14)insteadofthes