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
