BS EN 12441-3-2002 Zinc and zinc alloys - Chemical analysis - Determination of lead cadmium and copper - Flame atomic absorption spectometric method《锌及锌合金 化学分析 铅、镉、铜的测定 火焰原子吸收光谱法》.pdf

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 It supersedes BS 3630-7:1967, BS 3630-8:1971, BS 3630-9:1969, BS 3630-13:1972 and BS 3630-14:1972 which are withdrawn.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