1、BRITISH STANDARD BS EN 12441-3:2002 Zinc and zinc alloys Chemical analysis Part 3: Determination of lead, cadmium and copper Flame atomic absorption spectrometric method The European Standard EN 12441-3:2001 has the status of a British Standard ICS 77.120.60; 77.040.30 NO COPYING WITHOUT BSI PERMISS
2、ION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 12441-3:2002 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 January 2002 BSI 23 January 2002
3、ISBN 0 580 38163 3 National foreword This British Standard is the official English language version of EN 12441-3:2001. It supersedes BS 3630-7:1967, BS 3630-8:1971, BS 3630-9:1969, BS 3630-13:1972 and BS 3630-14:1972 which are withdrawn. The UK participation in its preparation was entrusted by Tech
4、nical Committee NFE/8, Zinc and zinc alloys, to Subcommittee NFE/8/4, Sampling and analysis of zinc and zinc alloys, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which imp
5、lement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not pur
6、port to include all the necessary provisions of a contract. Users of British Standards are responsible for their 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 Europea
7、n 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 UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages
8、 2 to 12, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN124413 October2001 ICS77.040.30;77.120.60 English
9、version ZincandzincalloysChemicalanalysisPart3:Determination oflead,cadmiumandcopperFlameatomicabsorption spectrometricmethod ZincetalliagesdezincAnalysechimiquePartie3: Dosagesduplomb,ducadmiumetducuivreMthodepar spectromtriedabsorptionatomiquedanslaflamme ZinkundZinklegierungenChemischeAnalyseTeil
10、3: BestimmungvonBlei,CadmiumundKupferFAAS Verfahren ThisEuropeanStandardwasapprovedbyCENon11August2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliograp
11、hicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheM
12、anagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZA
13、TION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN124413:2001EEN124413:2001(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4
14、3 Termsanddefinitions. .4 4 Principle4 5 Reagents.5 6 Apparatus .7 7 Sampling.7 8 Procedure .7 9 Calculationandexpressionofresults. 11 10 Testreport 11EN124413:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC209,“Zincandzincalloys“,the secretariatofwhichisheldbyAFNOR.
15、 ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyApril2002,andconflictingnationalstandardsshallbewithdrawnatthelatestby April2002. Withinitsprogramofwork,TechnicalCommitteeCEN/TC209entrustedCEN/TC209/WG6“Methodsofanalysis
16、 andtesting”withthepreparationofthefollowingdocument: prEN124413, ZincandzincalloysChemicalanalysisPart3:Determinationoflead,cadmiumandcopper Flameatomicabsorptionspectrometricmethod. Thisstandardispartofaseriesofelevenstandards.Theotherstandardsare: Part1:DeterminationofaluminiuminzincalloysTitrime
17、tricmethod Part2:DeterminationofmagnesiuminzincalloysFlameatomicabsorptionspectrometricmethod Part4:DeterminationofironinzincalloysSpectrophotometricmethod Part5:DeterminationofironinprimaryzincSpectrophotometricmethod Part6:DeterminationofaluminiumandironFlammeatomicabsorptionspectrometrymethod Par
18、t7:DeterminationoftinFlameatomicabsorptionspectrometricmethodafterextraction Part8:DeterminationoftininsecondaryzincFlameatomicabsorptionspectrometricmethod Part9:DeterminationofnickelinzincalloysFlameatomicabsorptionspectrometricmethod Part10:DeterminationofchromiumandtitaniuminzincalloysSpectropho
19、tometricmethod Part11:DeterminationofsiliconinzincalloysSpectrophotometricmethod AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,
20、Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom.EN124413:2001(E) 4 1Scope ThisEuropeanStandardspecifiesaflameatomicabsorptionspectrometrymethodforthedeterminationoflead, copperandcadmiuminzincandzincalloys.ItisapplicabletotheproductsspecifiedinEN988,
21、EN1179, EN1774,EN12844andprEN13283. Itissuitableforthedeterminationofleadcontents(massfractions)between0,0005%and2,5%,cadmium contents(massfractions)between0,0005%and0,3%,andcoppermassfractionsbetween0,0005%and4%. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provis
22、ionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencest
23、helatesteditionofthe publicationreferredtoapplies(includingamendments). EN988, ZincandzincalloysSpecificationsforrolledflatproductsforbuilding. EN1179, ZincandzincalloysPrimaryzinc. EN1774, ZincandzincalloysAlloysforfoundrypurposesIngotandliquid. EN12060 ,ZincandzincalloysMethodofsamplingSpecificati
24、ons. EN12844, ZincandzincalloysCastingsSpecifications. prEN13283, ZincandzincalloysSecondaryzinc. 3 Termsanddefinitions Forthepurposesofthisstandard,thetermsanddefinitionsgiveninEN12060andthefollowingapply. 3.1 flameatomicabsorptionspectrometry measurementoftheabsorptionofelectromagneticradiation,em
25、ittedbyanelementatadeterminedwavelength,by anabsorbentmedium(flame)formedofatomsofthesameelementthatareinthegroundstate.Eachelement absorbsradiationofspecificwavelengthsandtheintensityoftheabsorbedradiationisproportionaltothe concentrationofsaidelement 4Principle Asampleofthemetaloralloyisdissolvedi
26、namixtureofhydrochloricacidandnitricacidand,afteradequate dilutionandatomizationofthesolutionintoanairacetyleneflame,thecontentoftheparticularelementis determinedbyflameatomicabsorptionspectrometry. Sample(s)ofsecondaryzinccontainingtinaredissolvedinhydrochloricacid/hydrogenperoxide. NOTE Forleadcon
27、tents(massfractions)between0,0005%and0,005%,thedeterminationcouldbeprecededbyan enrichmentoftheleadbysimultaneousprecipitationwithcoppersulphideasatraceimpurityscavengerfromammoniacal solutioninthepresenceofammoniumfluoride,aspecifiedamountofthioacetamidebeingusedasprecipitatingagent.EN124413:2001(E
28、) 5 5Reagents 5.1General Duringthetest,useonlyreagentsofknownoranalyticalgradeanddistilledordemineralizedwater. 5.2 Hydrochloricacid, 1,19g/ml 5.3 Nitricacid, =1,4g/ml 5.4 Hydrochloricacidnitricacidmixture Mix180volumesofhydrochloricacid(5.2)with4volumesofnitricacid(5.3).Thismixtureshallbefreshlypre
29、pared justbeforeuse 5.5 Hydrochloricacid (1+6) Mix1volumeofhydrochloricacid(5.2)with6volumesofwater. 5.6 Zincpowder Zincpowderofparticlesizelessthan60 m,preparedfromzinchavingapurityofnotlessthan99,995%. 5.7 Zincchloridesolution, 200g/l Introduce200gofzinc(minimumpurity99,995%)intoa2lbeaker.Add100ml
30、ofwaterand700mlof hydrochloricacid(5.2)carefullyinsmallamountstocontroltherateofreaction.Afterdissolutionevaporatecarefully toasyrupyconsistency.Aftercooling,takeupwithabout800mlwaterandwarmgentlytodissolveanysalts.Add 20gofzincpowder(5.6)andshakefromtimetotimefornotlessthan30min.Transferintoa1lvolu
31、metricflask, dilutetothemarkwithwaterandmix.Allowtosettleandfilterthesolutionwithoutwashingtheresidue.Storeina polyethylenebottle. 1mlofthissolutioncontainsapproximately200mgofzinc. NOTE Ifzincwithapurityofnotlessthan99,9999%isused,thetreatmentwithzincpowdermaybeomitted. 5.8 Lead,cadmiumorcopper,1g/
32、lsolutions Introduce0,500goflead,cadmiumorcopper(inallcaseswithapurityofnotlessthan99,9%)intoa100ml beakerfittedwithawatchglass,andaddabout10mlofwater.Dissolvebycarefullyadding5mlofnitricacid(5.3). Afterdissolution,heatthesolutionuntilnofurthernitrousgasisevolved.Coolandtransfertoa500mlvolumetric fl
33、ask,dilutetothemarkwithwaterandmix. 1mlofthissolutioncontains1mgoflead,cadmiumorcopper. 5.9 Standardsolutionsoflead,cadmiumorcopper Transfer25,00mlofeachofthesolutions,preparedasdescribedin5.8,intoaseriesof1000mlvolumetricflasks. Dilutetothemarkwithwaterandmix. 1mlofeachofthesesolutionscontains0,025
34、mgoflead,cadmiumorcopper. 5.10 Hydrochloricacid (1+1) Mix1volumeofhydrochloricacid(5.2)with1volumeofwater.EN124413:2001(E) 6 5.11 Ammoniasolution, =0,91g/ml 5.12 Perchloricacid ,60%(massfraction) 5.13Chloroform 5.14Hydrogenperoxide,30%(massfraction) 5.15Copper,5g/lsolution Dissolve1gofhighpuritycopp
35、ercontainingnotmorethan5 g/gofleadin15mlofhydrochloricacidsolution (1+1)(5.10).Addhydrogenperoxide(5.14)dropwiseandheatgentlyonahotplateuntildissolution.Evaporateto asyrupyconsistency.Takeupinwaterandtransferquantitativelytoa200mlvolumetricflask.Dilutetothemark withwaterandmix. 1mlofthissolutioncont
36、ains5mgofcopper. 5.16Thioacetamidesolution Freshsolution,preparedimmediatelybeforeusebydissolving300mgofthioacetamideinwaterandmadeupto 100ml. 5.17 Dithizonesolution Dissolve40mgofdithizonein1lofchloroform(5.13).Protectthissolutionfromlightandkeepitinabrownglass bottle. 5.18 Purifiedammoniumfluoride
37、solution Dissolve50gofammoniumfluoride,NH 4 F,inabout300mlofwaterinaplasticbeaker.AdjustthepHofthe solutionto7,50,1usingammoniasolution(5.11),andtransfertoa500mlshakingfunnel.Nowshake,while addingdithizonesolution(5.17)in15mlportions,discardingtheextracteachtimeuntilthefinalextractretainsthe puregre
38、encolourofthedithizonesolution.Removeresidualdithizonebyshakingseveraltimeswith15mlofpure chloroform(5.13).DrainthepurifiedammoniumfluoridesolutionintoaplasticbeakerandadjustitspHvalueto between9,8and10,0withammoniasolution(5.11).Transferthesolutiontoa500mlvolumetricflask,andmake uptothemarkwithwate
39、r.Mixandtransfertoaplasticbottleforstorage. 5.19Aquaregia Mix3volumesofhydrochloricacid(5.2)with1volumeofnitricacid(5.3). 5.20 Aluminium,50g/lsolution Introduce50gofaluminium,withaminimumpurityof99,995%andfreeoflead,cadmiumandcopperintoa1l beaker.Add200mlofwaterand200mlofhydrochloricacid(5.2).Afterd
40、issolutionevaporatecarefullytoasyrupy consistency.Aftercooling,takeupwithabout800mlofwaterandtransfertoa1lvolumetricflask.Add20gof aluminiumturningsandshakefromtimetotimefornotlessthan60minutes.Transfertoa1lvolumetricflask, dilutetothemarkwithwaterandmix.Allowtosettleandfilterthesolutionwithoutwashi
41、ngtheresidue.Storeina polyethylenebottle. 1mlofthissolutioncontainsapproximately50mgofaluminium.EN124413:2001(E) 7 6Apparatus 6.1General Allglasswareusedforthepreparationofthesolutionsandfortheimplementationofthemethodshallbecleaned withboilingaquaregia(5.19)priortouse. 6.2Specific equipment Inaddit
42、iontostandardlaboratoryapparatus,thefollowingshallbeused: a) atomicabsorptionspectrometer,equippedwithapremixburner,withfacilitiesforusingtheoxidizerfuel combinationofairacetylene; NOTE Theexcitationsourceshouldbeoperatedinaccordancewiththemanufacturersrecommendations.Theoptical pathlengthwithinthef
43、lameshouldbebetween5cmand10cm. b) pHmeter ; c) membranefiltrationapparatus ,withcellulosenitratemembranefilterhavingadiameterof50mmor30mm andaporesizeof0,45mor0,6m. 7Sampling ThetestsampleshallbeselectedandpreparedinaccordancewiththeproceduregiveninEN12060. 8Procedure 8.1 Testportion Weigh10gofthetestsampletothenearest0,01g. 8.2 Preparationofthetestsamplesolution 8.2.1 Introducethetestportion(8
