EN 12441-4-2003 en Zinc and zinc alloys - Chemical analysis - Part 4 Determination of iron in zinc alloys - Spectrophotometric method《锌及锌合金 化学分析 第4部分 锌合金中铁含量的测定 分光光度法》.pdf

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

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