1、BRITISH STANDARD BS EN 12441-4:2003 Zinc and zinc alloys Chemical analysis Part 4: Determination of iron in zinc alloys Spectrophotometric method The European Standard EN 12441-4:2003 has the status of a British Standard ICS 77.040.30; 77.120.60 BS EN 12441-4:2003 This British Standard was published
2、 under the authority of the Standards Policy and Strategy Committee on 3 April 2003 BSI 3 April 2003 ISBN 0 580 41491 4 National foreword This British Standard is the official English language version of EN 12441-4:2003. The UK participation in its preparation was entrusted to Technical Committee NF
3、E/8, Zinc and zinc 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 publications referred to in this document may be found in th
4、e 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 necessary provisions of a contract. Users are responsible
5、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 interpretation, or proposals for change, and keep the UK i
6、nterests 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 7 and a back cover. The BSI copyright date displayed in this document indicates when
7、the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN124414 March2003 ICS77.040.30;77.120.60 Englishversion ZincandzincalloysChemicalanalysisPart4:Determination ofironinzincalloysSpectrophotometricmethod Zincetalliag
8、esdezincAnalysechimiquePartie4: DosageduferdanslesalliagesdezincMthode spectrophotomtrique ZinkundZinklegierungenChemischeAnalyseTeil4: BestimmungvonEiseninZinklegierungen SpektrophotometrischesVerfahren ThisEuropeanStandardwasapprovedbyCENon21November2002. CENmembersareboundtocomplywiththeCEN/CENEL
9、ECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthree
10、officialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,Fra
11、nce,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allri
12、ghtsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN124414:2003EEN124414:2003(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle4 5 Reagents.4 6 Apparatus .5 7 Sampling.5 8 Procedure .5 9 Calculationandexpression
13、ofresults. 7 10 Testreport 7EN124414:2003(E) 3 Foreword Thisdocument(EN124414:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC 209“Zincandzinc alloys“,thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,a
14、tthelatestbySeptember2003,andconflictingnationalstandardsshallbewithdrawnatthe latestbySeptember2003. Withinitsprogrammeofwork,TechnicalCommitteeCEN/TC209entrustedCEN/TC209/WG6“Methodsof analysisandtesting”withthepreparationofthefollowingdocument: EN124414, ZincandzincalloysChemicalanalysisPart4:Det
15、erminationofironinzincalloys Spectrophotometricmethod. Thisstandardispartofaseriesofelevenstandards.Theotherstandardsare: EN 124411, ZincandzincalloysChemicalanalysisPart1:Determinationofaluminiuminzincalloys Titrimetricmethod ; EN 124412, ZincandzincalloysChemicalanalysisPart2:Determinationofmagnes
16、iuminzincalloys Flameatomicabsorptionspectrometricmethod ; EN 124413, ZincandzincalloysChemicalanalysisPart3:Determinationoflead,cadmiumandcopper Flameatomicabsorptionspectrometricmethod ; EN 124415, ZincandzincalloysChemicalanalysisPart5:Determinationofironinprimaryzinc Spectrophotometricmethod ; E
17、N 124416, ZincandzincalloysChemicalanalysisPart6:DeterminationofaluminiumandironFlame atomicabsorptionspectrometricmethod ; prEN124417, ZincandzincalloysChemicalanalysisPart7:DeterminationoftinFlameatomic absorptionspectrometricmethodafterextraction ; prEN 124418, ZincandzincalloysChemicalanalysisPa
18、rt8:Determinationoftininsecondaryzinc Flameatomicabsorptionspectrometricmethod ; prEN 124419, ZincandzincalloysChemicalanalysisPart9:DeterminationofnickelinzincalloysFlame atomicabsorptionspectrometricmethod ; prEN 1244110, ZincandzincalloysChemicalanalysisPart10:Determinationofchromiumandtitaniumin
19、 zincalloysSpectrophotometricmethod ; prEN 1244111, ZincandzincalloysChemicalanalysisPart11:Determinationofsiliconinzincalloys Spectrophotometricmethod ; AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganisationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Aust
20、ria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN124414:2003(E) 4 1Scope ThisEuropeanStandardspecifiesaspectrophotometricmethodforthedeterminationofironi
21、nzincalloys.Itis applicabletotheproductsspecifiedinEN1774andEN12844. Itissuitableforthedeterminationofironcontents(massfractions)between0,01%and0,1%. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedatthe
22、appropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamend
23、ments). EN1774, ZincandzincalloysAlloysforfoundrypurposesIngotandliquid . EN12060:1997, ZincandzincalloysMethodofsamplingSpecifications . EN12844, ZincandzincalloysCastingsSpecifications . 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thetermsanddefinitionsgiveninEN12060:1997apply. 4Pri
24、nciple Formationofasulfosalicylicacidferriccomplexinanammoniacalmedium,afterseparationofthecopper. Spectrophotometricmeasurementoftheyellowcolourofthecomplexthusformed. 5Reagents 5.1 General Duringthetest,useonlyreagentsofknownanalyticalgradeanddistilledordemineralisedwater. 5.2 Puregranulatedcadmiu
25、m ,freefromiron 5.3 Hydrochloricacid , r =1,19g/ml 5.4 Hydrochloricacid (1+1) Mix1volumeofhydrochloricacid(5.3)with1volumeofwater 5.5 Hydrogenperoxide ,30%(massfraction) 5.6 Sulfosalicylicacid ,800g/lsolution 5.7 Ammoniasolution , r =0,91g/mlEN124414:2003(E) 5 5.8 StandardironsolutionA Weigh0,250gof
26、pureirontothenearest0,001g.Addbysmallfractionsapproximately10mlofhydrochloricacid (5.3).Oxidisebyafewdropsofhydrogenperoxide(5.5).Decomposetheexcesshydrogenperoxidebyboiling. Cooltoroomtemperature.Transferquantitativelytoa1lvolumetricflask.Dilutetothemarkwithwaterandmix. 1mlofthissolutioncontains0,2
27、50mgofiron. 5.9 StandardironsolutionB Transferexactly20mlofstandardironsolutionA(5.8)toa100mlvolumetricflask.Dilutetothemarkwithwater andmix. 1mlofthissolutioncontains0,050mgofiron. 5.10 Nitricacid , r =1,4g/ml. 5.11 Aquaregia Mix3volumesofhydrochloricacid( 5.3) with1volumeofnitricacid(5.10). 6Appar
28、atus 6.1General Allglasswareusedforthepreparationofthesolutionsandfortheimplementationofthemethodshallbecleaned withboilingaquaregia(5.11)priortouse. 6.2Specific equipment Inadditiontostandardlaboratoryapparatus,aspectrophotometer,setatawavelengthof425nmandusing1cm opticalcells,shallbeused. NOTE The
29、dilutionandaliquotpartsdefinedinthisstandardonlyapplyif1cmcellsareused.Itisnecessarytoapplythe appropriatemodificationsinthecaseofcellswithotherdimensions. 7Sampling ThetestsampleshallbeselectedandpreparedinaccordancewiththeproceduregiveninEN12060. 8Procedure 8.1 Testportion Weigh10gofthetestsamplet
30、othenearest0,01g. 8.2Blank test Simultaneouslywitheachdetermination,carryoutablanktestusingthesamequantitiesofeachreagentand followingthesameprocedure.EN124414:2003(E) 6 8.3 Preparationofthetestsolution 8.3.1 Introducethetestportion(8.1)intoa500mlbeakerfittedwithawatchglassanddissolvebycarefullyaddi
31、ng 100mlofhydrochloricacid(1+1)(5.4).Oxidiseandcompletethedissolutionbyaddingafewdropsofhydrogen peroxide(5.5). 8.3.2 Decomposetheexcesshydrogenperoxidebyboiling. 8.3.3 Add2gofcadmium(5.2)andheatgentlyfor3min,shakingfrequentlyinordertoreducethecopper completely. 8.3.4 Cooltoroomtemperature.Filterand
32、washthrougharapidfilterpapercollectingthesolutionandwashings quantitativelyina250mlvolumetricflask.Dilutetothemarkwithwaterandmix. 8.3.5 Transfera25mlaliquottoa100mlvolumetricflask. Addsuccessively: a) 20mlofsulfosalicylicacidsolution(5.6); b) ammoniasolution(5.7)untilthesolutionhasayellowcolour,the
33、n20mlinexcess. 8.3.6 Cooltoroomtemperature.Dilutetothemarkwithwaterandmix. 8.4 Calibrationgraph NOTE Thefollowingisvalidfor1cmcellsandforironcontentsof0mg,0,10mg,0,25mg,0,50mgand1,00mg, correspondingtocontents(massfractions)inthetestportionof0%,0,010%,0,025%,0,050%and0,100%ofiron.Itis necessarytoapp
34、lyappropriatemodificationsinthecaseofcellsofdifferentdimensions. 8.4.1 Introduceintoaseriesof100mlvolumetricflasks,0,00ml;2,00ml;5,00ml;10,00mland20,00ml respectivelyofstandardironsolutionB(5.9).Dilutetoabout50ml. 8.4.2 Addsuccessively: a) 20mlofsulfosalicylicacidsolution(5.6); b) ammoniasolution(5.
35、7)untilthesolutionhasayellowcolour,then20mlinexcess. 8.4.3 Cooltoroomtemperature.Dilutetothemarkwithwaterandmix. 8.4.4 Measuretheabsorbanceofeachsolutionagainstthesolutionwith0,00mlstandardironsolutionBin1cm cells,usingthespectrophotometer(6.2)atawavelengthof425nm. 8.4.5 Produceacalibrationgraphbypl
36、ottingtheironcontentversustheabsorbancereadingsobtainedforeach calibrationstandard. 8.5Spectrophotometric measurement Measuretheabsorbanceofthetestsolution(s)againsttheblanksolution(8.2)in1 cmcellsusingthe spectrophotometer(6.2)atawavelengthof425nm.EN124414:2003(E) 7 9 Calculationandexpressionofresu
37、lts Determinefromthemeasuredabsorbanceofthetestsolutiontheassociatedamountofironfromthecalibration graph(8.4).Ifanumberofdeterminationsarecarriedoutthenthemeanofallresultsshallbecalculatedbyadding theindividualresultstogetheranddividingbythenumberofindividualresults. Theresultsshallbeexpressedasspec
38、ifiedinEN1774andEN12844. 10 Testreport Thetestreportshallincludethefollowing: a) typeandidentificationofsample; b) testmethod(i.e.referencetothisstandard); c) ironcontent,expressedaspercentagebymass,givingwherepossibletheresultsfortheindividualandthe meanvalues; d) anyunusualoccurrenceduringthedeter
39、mination; e) anystepsintheprocedurebeyondthosespecifiedinthisstandard,andanycircumstancesthatmayhave affectedtheresults; f) dateoftesting; g) nameofthelaboratoryortestingorganisation; h) signatureofthelaboratorymanagerorotherresponsibleperson.BS EN 12441-4:2003 BSI 389 Chiswick High Road London W4 4
40、AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision.
41、 Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Se
42、cretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: +44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of
43、standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel: +44 (0)20 8996 9001. Fax: +44 (0)20 8996 7001. Email: ordersbsi-. Standards are also available from the BSI website at http:/www.bsi-. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requested. Information on standards BSI provides a wide range of information on national, European and international standa
