1、BRITISH STANDARD BS EN 12441-5:2003 Zinc and zinc alloys Chemical analysis Part 5: Determination of iron in primary zinc Spectrophotometric method The European Standard EN 12441-5:2003 has the status of a British Standard ICS 77.040.30; 77.120.60 BS EN 12441-5:2003 This British Standard was publishe
2、d under the authority of the Standards Policy and Strategy Committee on 3 April 2003 BSI 3 April 2003 ISBN 0 580 41492 2 National foreword This British Standard is the official English language version of EN 12441-5:2003. It supersedes BS 3630-5:1963 which is withdrawn. The UK participation in its p
3、reparation was entrusted to Technical Committee NFE/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 publicatio
4、ns referred to in this document may be found in the 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 necessar
5、y provisions of a contract. Users are responsible 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 interpre
6、tation, 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 2 to 7 and a back cover. The BSI copyrig
7、ht date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN124415 March2003 ICS77.040.30;77.120.60 Englishversion ZincandzincalloysChemicalanalysisPart5:Determination ofiro
8、ninprimaryzincSpectrophotometricmethod ZincetalliagesdezincAnalysechimiquePartie5: DosageduferdanslezincprimaireMthode spectrophotomtrique ZinkundZinklegierungenChemischeAnalyseTeil5: BestimmungvonEiseninPrimrzink SpektrophotometrischesVerfahren ThisEuropeanStandardwasapprovedbyCENon21November2002.
9、CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCE
10、Nmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria
11、,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:r
12、uedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN124415:2003EEN124415:2003(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
13、 8 Procedure .5 9 Calculationandexpressionofresults. 7 10 Testreport 7EN124415:2003(E) 3 Foreword Thisdocument(EN124415:2003)hasbeenpreparedbyTechnicalCommitteeCEN /TC 209“Zincandzinc alloys“,thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypub
14、licationofanidenticaltextor byendorsement,atthelatestbySeptember2003,andconflictingnationalstandardsshallbewithdrawnatthe latestbySeptember2003. Withinitsprogrammeofwork,TechnicalCommitteeCEN/TC209entrustedCEN/TC209/WG6,“Methodsof analysisandtesting”withthepreparationofthefollowingdocument: EN124415
15、,ZincandzincalloysChemicalanalysisPart5:Determinationofironinprimaryzinc Spectrophotometricmethod . Thisstandardispartofseriesofelevenstandards.Theotherstandardsare: EN 124411, ZincandzincalloysChemicalanalysisPart1:Determinationofaluminiuminzincalloys Titrimetricmethod ; EN 124412, Zincandzincalloy
16、sChemicalanalysisPart2:Determinationofmagnesiuminzincalloys Flameatomicabsorptionspectrometricmethod ; EN 124413, ZincandzincalloysChemicalanalysisPart3:Determinationoflead,cadmiumandcopper Flameatomicabsorptionspectrometricmethod ; EN124414, ZincandzincalloysChemicalanalysisPart4:Determinationofiro
17、ninzincalloys Spectrophotometricmethod. . EN 124416, ZincandzincalloysChemicalanalysisPart6:DeterminationofaluminiumandironFlame atomicabsorptionspectrometricmethod ; prEN124417, ZincandzincalloysChemicalanalysisPart7:DeterminationoftinFlameatomic absorptionspectrometricmethodafterextraction ; prEN
18、124418, ZincandzincalloysChemicalanalysisPart8:Determinationoftininsecondaryzinc Flameatomicabsorptionspectrometricmethod ; prEN 124419, ZincandzincalloysChemicalanalysisPart9:DeterminationofnickelinzincalloysFlame atomicabsorptionspectrometricmethod ; prEN 1244110, ZincandzincalloysChemicalanalysis
19、Part10:Determinationofchromiumandtitaniumin zincalloysSpectrophotometricmethod ; prEN 1244111, ZincandzincalloysChemicalanalysisPart11:Determinationofsiliconinzincalloys Spectrophotometricmethod ; AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesa
20、reboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN124415:2003(E) 4 1Scope ThisEuropeanStandardspecifiesaspectro
21、photometricmethodforthedeterminationofironinprimaryzinc.Itis applicabletotheproductsspecifiedinEN1179. Itissuitableforthedeterminationofironcontents(massfractions)between0,001%and0,1%. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.The
22、se normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicat
23、ionreferredtoapplies(includingamendments). EN1179, ZincandzincalloysPrimaryzinc. EN12060:1997, ZincandzincalloysMethodofsamplingSpecifications. 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thetermsanddefinitionsgiveninEN12060:1997apply. 4Principle Formationofasulfosalicylicacidferricco
24、mplexinanammoniacalmedium.Spectrophotometricmeasurementof theyellowcolourofthethusformedcomplex. 5Reagents 5.1General Duringthetest,useonlyreagentsofknownanalyticalgradeanddistilledordemineralisedwater. 5.2 Ammoniasolution, r =0,91g/ml. 5.3 Hydrochloricacid, r =1,19g/ml. 5.4 Hydrogenperoxide, 30%(ma
25、ssfraction). 5.5 Sulfosalicylicacid, 400g/lsolution. 5.6 Nickelchloridesolution Dissolve2gofnickelchloridehexahydrate(NiCl 2 .6H 2 O)in500mlofwater.Makeupto1landmix. 5.7 StandardironsolutionA Weigh0,250gofpureirontothenearest0,001g.Addbysmallfractionsapproximately10mlofhydrochloricacid (5.3).Oxidise
26、byaddingafewdropsofhydrogenperoxide(5.4).Decomposetheexcesshydrogenperoxideby boiling.Cooltoroomtemperature.Transferquantitativelytoa1lvolumetricflask.Dilutetothemarkwithwaterand mix.EN124415:2003(E) 5 1mlofthissolutioncontains0,250mgofiron. 5.8 StandardironsolutionB Transferexactly20mlofstandardiro
27、nsolutionA(5.7)toa100mlvolumetricflask.Dilutetothemarkwithwater andmix. 1mlofthissolutioncontains0,050mgofiron. 5.9 Nitricacid, r =1,4g/ml. 5.10 Aquaregia Mix3volumesofhydrochloricacid(5.3)with1volumeofnitricacid(5.9). 6Apparatus 6.1General Allglasswareusedforthepreparationofthesolutionsandfortheimp
28、lementationofthemethodshallbecleaned withboilingaquaregia(5.10)priortouse. 6.2Specific equipment Inadditiontostandardlaboratoryapparatus,aspectrophotometer,setatawavelengthof425nmandusing1cm opticalcellsshallbeused. NOTE Thedilutionandaliquotpartsdefinedinthisstandardonlyapplyif1cmcellsareused.Itisn
29、ecessarytoapplythe appropriatemodificationsinthecaseofcellswithotherdimensions. 7Sampling ThetestsampleshallbeselectedandpreparedinaccordancewiththeproceduregiveninEN12 060. 8Procedure 8.1 Testportion Weigh10gofthetestsampletothenearest0,01g. 8.2Blank test Simultaneouslywitheachdetermination,carryou
30、tablanktestusingthesamequantitiesofeachreagentand followingthesameprocedure. 8.3 Preparationofthetestsolution 8.3.1 Introducethetestportion(8.1)ina500mlbeakerfittedwithawatchglassanddissolvebycarefullyadding 50mlofhydrochloricacid(5.3).Oxidiseandcompletethedissolutionbyaddingafewdropsofhydrogenperox
31、ide (5.4). Ifdissolutionisverydifficult,2mlofnickelchloridesolution(5.6)shouldbeaddedtoexpeditetheattack. 8.3.2 Decomposetheexcesshydrogenperoxidebyboiling.EN124415:2003(E) 6 8.3.3 Forironcontents(massfractions)equaltoorgreaterthan0,01%proceedasfollows(iflessthan0,01% see8.3.4): a) cooltoroomtempera
32、ture.Transferquantitativelytoa250mlvolumetricflask.Dilutetothemarkwithwater andmix; b) transfera25mlaliquottoa100mlvolumetricflask; c)add successively: 1) 25mlofwater; 2) 5mlofsulfosalicylicacid(5.5); 3) ammoniasolution(5.2)untilthesolutionbecomesyellow,then20mlinexcess; d) cooltoroomtemperature.Dil
33、utetothemarkwithwaterandmix. 8.3.4 Forironcontents(massfractions)lessthan0,01%proceedasfollows: a) evaporatethetestportionuntilasyrupyconsistencyisobtained; b) cooltoroomtemperature; c) takeupwithaminimumofwater(soasnottoexceed30ml)andtransferquantitativelytoa100mlvolumetric flask; d)add successivel
34、y: 1) 5mlofsulfosalicylicacidsolution(5.5); 2) ammoniasolution(5.2)untilthesolutionhasayellowcolour,then50mlinexcess; e) cooltoroomtemperature.Dilutetothemarkandmix.Measuretheabsorbanceofthesolutions(see8.5)after firstmeasuringthecalibrationgraphasin8.4. 8.4 Calibrationgraph NOTE Thefollowingisvalid
35、for1cmcellsandforironcontents(massfractions)of0mg,0,10mg,0,25mg,0,5mgand 1,00mgofironcorrespondingtomassfractionsinthetestportionof0%,0,01%,0,025%0,05%and0,1%whenusingthe procedurespecifiedin8.3.3and0%,0,001%0,0025%,0,005%and0,01%whenusingtheprocedurespecifiedin8.3.4.Itis necessarytoapplytheappropri
36、atemodificationsinthecaseofcellsofdifferentdimensions. 8.4.1 Introduceintoaseriesof100mlvolumetricflasks,0,00ml,2,00ml,5,00ml,10,00mland20,00mlof standardironsolutionB(5.8). 8.4.2 Addsuccessively: a) 5mlofsulfosalicylicacidsolution(5.5); b) ammoniasolution(5.2)untilthesolutionbecomesyellow,then20mli
37、nexcess. 8.4.3 Cooltoroomtemperature.Dilutetothemarkwithwaterandmix. 8.4.4 Measuretheabsorbanceofeachsolutionagainstthesolutionwith0,00mlstandardironsolutionB,in1cm cells,usingthespectrophotometer(6.2)atawavelengthof425nm. 8.4.5 Produceacalibrationgraphbyplottingtheironcontentversustheabsorbanceread
38、ingsobtainedforeach calibrationstandard.EN124415:2003(E) 7 8.5Spectrophotometric measurement Measuretheabsorbanceofthetestsolution(s)againsttheblanksolution(8.2)in1 cmcellsusingthe spectrophotometer(6.2)atawavelengthof425nm. 9 Calculationandexpressionofresults Determinefromthemeasuredabsorbanceofthe
39、testsolutiontheassociatedamountofironfromthecalibration graph(8.4).Ifanumberofdeterminationsarecarriedoutthenthemeanofallresultsshallbecalculatedbyadding theindividualresultstogetheranddividingbythenumberofindividualresults. ResultsshallbeexpressedasspecifiedinEN1179. 10 Testreport Thetestreportshal
40、lincludethefollowing: a) typeandidentificationofthesample; b) testmethodused,(i.e.referencetothisstandard); c) ironcontent,expressedaspercentagebymass,givingwherepossibletheresultsfortheindividualandthe meanvalues; d) anyunusualoccurrenceduringthedetermination; e) anystepsintheprocedurebeyondthosesp
41、ecifiedinthisstandard,andanycircumstancesthatmayhave affectedtheresults; f) dateoftesting; g) nameofthelaboratoryortestingorganisation; h) signatureofthelaboratorymanagerorotherresponsibleperson.BS EN 12441-5:2003 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the
42、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. Users of British Standards should make sure tha
43、t 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 Secretary 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 a
