EN 13615-2001 en Methods for the Analysis of Ingot Tin - Determination of Impurity Element Contents in Tin Grades 99 90% and 99 85% by Atomic Spectrometry (Incorporating Corrigendu.pdf

1、BRITISH STANDARD BS EN 13615:2001 Incorporating Corrigendum No. 1 Methods for the analysis of ingot tin Determination of impurity element contents in tin grades 9 9 , 9 0% a n d 9 9 , 8 5% b y atomic spectrometry The European Standard EN 13615:2001 has the status of a British Standard ICS 77.040.30;

2、 77.150.60 BS EN 13615:2001 This British Standard, having been prepared under the direction of the Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 23 July 2002 BSI 24 October 2003 ISBN 0 580 40129 4 National forewo

3、rd This British Standard is the official English language version of EN 13615:2001, including Corrigendum December 2002. The UK participation in its preparation was entrusted to Technical Committee NFE/27, Tin and tin alloys, which has the responsibility to: A list of organizations represented on th

4、is 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 Catalogue under the section entitled “International Standards Correspondence Index”, or by usin

5、g the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity fr

6、om legal obligations. 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 developments and promulgate them in the

7、 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 copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13789 Cor

8、rigendum No. 1 24 October 2003 Deletion of the last paragraph in 7.2EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13615 December2001 ICS77.040.30;77.150.60 Incorporating Corrigendum December 2002 Englishversion MethodsfortheanalysisofingottinDeterminationofimpurity elementcontentsintingrades99,90

9、%and99,85%byatomic spectrometry MthodespourlanalysedeslingotsdtainDtermination desteneursenimpuretsdansltaindequalit99,90%et 99,85%parspectromtrieatomique VerfahrenfrdieAnalysevonZinninMasseln BestimmungdesGehaltesanVerunreinigungselementenin ZinnderReinheitsgrade99,90%und99,85%durch Atomspektrometr

10、ie ThisEuropeanStandardwasapprovedbyCENon5October2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsm

11、aybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official ver

12、sions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMIT

13、EEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13615:2001EEN13615:2001(E) 2 Contents page Foreword .3 1 Scope3 2 Normativereferences 3 3 Principle .3 4 Reagents 4 5 Apparatus.6 6 Sampli

14、ng 6 7 Procedure.6 7.1 Preparationofthesolutionofthesampleundertest6 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 (norma

15、tive) Methodforcheckingatomicabsorptionspectrometerperformance (basedonISO75301:1990) . 9 AnnexB (normative) Methodforcheckinginductivelycoupledplasmaatomicemission spectrometerperformance.12 Bibliography .14EN13615:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC220“

16、Tinandtinalloys”the secretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyJune2002,andconflictingnationalstandardsshallbe withdrawnatthelatestbyJune2002. TheannexesAandBarenormative. Accordingtoth

17、eCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKing

18、dom. 1Scope ThisEuropeanStandardspecifiesatomicspectroscopicmethods(AtomicAbsorptionSpectrometry (AAS)orinductivelycoupledplasmaAtomicEmissionSpectrometry(ICPAES)intendedforthe analysisofingottin.Itiswrittenforusebyexperiencedanalystsfamiliarwithatomicspectrometric techniques. 2 Normativereferences

19、ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromother publications.Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthe publicationsarelistedhereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofany ofthesepublicationsapplytothisEuropeanStandardonl

20、ywhenincorporatedinitbyamendmentor revision.Forundatedreferencesthelatesteditionofthepublicationreferredtoapplies(including amendments). EN610, TinandtinalloysIngottin. 3Principle Thetestsampleisdissolvedinhydrochloricacidplusnitricacidandtartaricorcitricacid,andthe concentrationoftheelementsoughtis

21、measuredusingatomicabsorptionspectrometryorinductively coupledplasmaatomicemissionspectrometry.Interferenceisminimisedbymatchingsampleand referencematerialsandbythechoiceofinstrumentparameters.EN13615:2001(E) 4 4Reagents 4.1General Duringtheanalysis,unlessotherwisestated,useonlyreagentsofrecogniseda

22、nalyticalgradeand onlydistilledwaterorwaterofequivalentpurity. 4.2 Hydrochloricacid ,concentrated( 1,18g/ml). 4.3 Dilutehydrochloricacid (1+1) .Dilute100mlhydrochloricacid( 4.2)with100mlwater. WARNING Theacidshouldaddedtothewaterforsafetyreasons. 4.4 Dilutehydrochloricacid (1+19). Dilute10mlhydrochl

23、oricacid( 4.2)with190mlwater. 4.5 Nitricacid ,( 1,42g/ml). 4.6 Sulphuricacid ,( 1,84g/ml). 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) .Add10

24、0mlnitricacid( 4.5)to100mlwater. 4.10 Dilutenitricacid(1+4) .Add50mlnitricacid( 4.5)to200mlwater. 4.11 Dilutenitricacid(1+9) .Add25mlnitricacid( 4.5)to225mlwater. 4.12 Dilutenitricacid(1%) .Dilute5mlnitricacid( 4.5)upto500ml. 4.13 Standardsolutionsofmetals.Freshlypurchasedstandardmetalsolutionsmaybe

25、usedor standardmetalsolutionsshouldbemadeupasfollows( 4.13.1to 4.13.25). 4.13.1 Standardantimonysolution(1 mlcontains1 mgSb) .Place0,10 gSbin5 mlsulphuric acid( 4.6)andheattocompletedissolution.Cool.Carefullyaddapproximately10mlwaterandcool again.Transfertoa100mlvolumetricflaskwithdilutehydrochloric

26、acid(1+1)( 4.3). 4.13.2 Standardantimonysolution(1mlcontains0,2mgSb) .Transfer10,00mlofSbsolution 4.13.1 toa50mlvolumetricflaskandmakeuptovolumewithdilutehydrochloricacid(1+1)( 4.3). 4.13.3 Standardcoppersolution(1mlcontains1mgCu) .Dissolve0,10gCuin10mldilutenitric acid(1+4)( 4.9)andtransfertoa100ml

27、volumetricflask.Makeuptovolumewithwaterandmix. 4.13.4 Standardcoppersolution(1mlcontains0,2mgCu) .Transfer10,00mlofCusolution 4.13.3 toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.5 Standardleadsolution(1mlcontains1mgPb) .Dissolve0,10gPbin10mldilutenitricacid (1+4)( 4.10)andtransfertoa

28、100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.6 Standardleadsolution(1mlcontains0,1mgPb) .Transfer5,00mlofPbsolution 4.13.5toa 50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.7 Standardbismuthsolution(1mlcontains1mgBi) .Dissolve0,10gBiin10mldilutenitric acid(1+1)( 4.9)andtransfe

29、rtoa100mlvolumetricflask.Makeuptovolumewithwaterandmix.EN13615:2001(E) 5 4.13.8 Standardbismuthsolution(1mlcontains0,1mgBi) .Transfer5,00mlofbismuthsolution 4.13.7 toa50mlvolumetricflaskandmakeuptovolumewithdilutehydrochloricacid(1+1)( 4.3). 4.13.9 Standardcadmiumsolution(1mlcontains1mgCd) .Dissolve

30、0,10gCdin10mldilutenitric acid(1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.10 Standardcadmiumsolution(1 mlcontains0,01 mgCd) .Transfer1,00 mlofcadmium solution4.13.9toa100mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.11 Standardzincsolution(1mlcontains

31、1mgZn).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 Standardironsolution(1mlcontai

32、ns1mgFe) .Dissolve0,10gFewire(freefromrust)in 10mlofnitricacid(1+4)( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewith waterandmix. 4.13.14 Standardironsolution(1mlcontains0,02mgFe) .Transfer1,00mlofironsolution 4.13.13 toa50mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.15 Standarda

33、rsenicsolution(1mlcontains1mgAs) .Dissolve0,1320gofAs 2 0 3 inalittle sodiumhydroxidesolution(1mol/l)andtransfertoa100mlvolumetricflask.Makeuptovolumewith waterandmix. 4.13.16 Standardarsenicsolution(1mlcontains0,1mgAs) .Transfer5,00mlarsenicsolution 4.13.15 toa50mlvolumetricflask.Makeuptovolumewith

34、waterandmix. 4.13.17 Standardaluminiumsolution(1mlcontains1mgAl).Dissolve0,100gAlmetalin10ml nitricacid( 4.10)andtransfertoa100mlvolumetricflask.Makeuptovolumewithwaterandmix. 4.13.18 Standardaluminiumsolution(1 mlcontains0,05 mgAl) .Transfer5,00 mlofaluminium solution4.13.17toa100mlvolumetricflaska

35、ndmakeuptovolumewithdilutenitricacid(1%) (4.12). 4.13.19 Standardaluminiumsolution(1mlcontains0,005mgAl).Transfer5,00mlofaluminium solution4.13.18toa50mlvolumetricflaskandmakeuptovolumewithdilutenitricacid(1%)( 4.12). 4.13.20 Standardsilversolution(1mlcontains1mgAg).Dissolve0,787gsilvernitratein50ml

36、 water.Transfertoa500mlvolumetricflaskandmakeuptovolumewithnitricacid(1%)( 4.12). 4.13.21 Standardsilversolution(1mlcontains0,1mgAg) .Transfer5,00mlofsilversolution( 4.13.20) toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.22 Standardnickelsolution(1mlcontains1,0mgNi) .Dissolve0,100gofn

37、ickelin10mlof nitricacid(1+4)(4.10)andtransfertoa100mlvolumetricflaskandmakeuptovolumewithwater andmix. 4.13.23 Standardnickelsolution(1mlcontains0,1mgNi) .Transfer5,00mlofnickelsolution 4.13.22 toa50mlvolumetricflaskandmakeuptovolumewithwaterandmix. 4.13.24 Standardindiumsolution(1mlcontains1,0mgIn

38、) .Dissolve0,100gofindiumin10mlof nitricacid(1+4)( 4.10)andtransfertoa100mlvolumetricflaskandmakeuptovolumewithwater andmix. 4.13.25 Standardindiumsolution(1mlcontains0,1mgIn) .Transfer5,00mlofindiumsolution 4.13.24 toa50mlvolumetricflaskandmakeuptovolumewithdilutenitricacid(1%)( 4.12).EN13615:2001(

39、E) 6 4.14 Tin,min.purity99,99%. 5Apparatus 5.1 Ordinarylaboratoryapparatus .UsegradeAglassware. 5.2 Burette,ofcapacity5ml,graduatedin0,02ml. 5.3 Atomicabsorptionspectrometerorinductivelycoupledplasmaatomicemissionspectrometer , conformingtotheperformancerequirementsinnormativeannexesAandB. 5.4 Hollo

40、wcathodelampsorelectrodelessdischargetubesforantimony,bismuth,cadmium, copper,lead,silver,iron,zinc,arsenic,nickel,aluminium,indium,goldandcobalt . NOTE Thepresenceofotherelementsmayalsoneedtobeascertained. 6Sampling ThesampleforanalysisshallbeobtainedasdescribedinEN610. 7Procedure 7.1 Preparationof

41、thesolutionofthesampleundertest 7.1.1 Weigh1,0g0,1gofthesampleandtransfertoa250mlbeaker.Add20mloftheacid mixture( 4.8),heattocompletedissolutionandcool.Transfertoa100mlvolumetricflaskandmake uptothevolumewithdilutehydrochloricacid(1+19)( 4.4)andmix. 7.1.2 Prepareablanktestsolutionfollowingtheprocedu

42、redescribedin 7.1.1,butusing1,0gof highpuritytin( 4.14)insteadofthesample. 7.2 Preparationofcalibrationsolutions Forthedeterminationoftheimpurities,weigh1,0g 0,1ghighpuritytin( 4.14)intoeachof7250ml beakers.Add20mloftheacidmixture( 4.8)andwarmtodissolve.Coolandtransfertoa100ml volumetricflaskandaddt

43、heamountsofthestandardmetalsolutionsshowninTable1. Finallymakeuptothemarkwithdilutehydrochloricacid( 4.4).EN13615:2001(E) 7 Table1Volumeofstandardmetalsolutionsused inthepreparationofthecalibrationsolutions FlaskNo. Standardmetalsolution ml Sb Cu Pb Bi Cd Zn 4.13.2 4.13.4 4.13.6 4.13.8 4.13.10 4.13.12 1 0,0 0,0 0,0 0,0 0,0 0,0 2 0,5 0,5 0,5 0,5 0,5 0,5 3 1,0 1,0 1,0 1,0 1,0 1,0 4 2,0 2,0 2,0 2,0 2,0 2,0