EN 12441-6-2003 en Zinc and zinc alloys - Chemical analysis - Part 6 Determination of aluminium and iron-Flame atomic absorption spectrometric method《锌及锌合金 化学分析 第6部分 火焰原子吸收光谱法测定铝和铁.pdf

1、BRITISH STANDARD BS EN 12441-6:2003 Zinc and zinc alloys Chemical analysis Part 6: Determination of aluminium and iron Flame atomic absorption spectrometric method The European Standard EN 12441-6:2003 has the status of a British Standard ICS 77.040.30; 77.120.60 BS EN 12441-6:2003 This British Stan

2、dard was published under the authority of the Standards Policy and Strategy Committee on 1 April 2003 BSI 1 April 2003 ISBN 0 580 41493 0 National foreword This British Standard is the official English language version of EN 12441-6:2003. The UK participation in its preparation was entrusted to Tech

3、nical 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 publications referred to in this document

4、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 necessary provisions of a contract. User

5、s 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 interpretation, or proposals for change,

6、 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 10, an inside back cover and a back cover. The BSI copyright date d

7、isplayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN124416 March2003 ICS77.040.30;77.120.60 Englishversion ZincandzincalloysChemicalanalysisPart6:Determination ofaluminiumand

8、ironFlameatomicabsorptionspectrometric method ZincetalliagesdezincAnalysechimiquePartie6: DosagedelaluminiumetduferMthodeparspectromtrie dabsorptionatomiquedanslaflamme ZinkundZinklegierungenChemischeAnalyseTeil6: BestimmungvonAluminiumundEisenFAASVerfahren ThisEuropeanStandardwasapprovedbyCENon21No

9、vember2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCen

10、treortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbod

11、iesofAustria,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 Manage

12、mentCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN124416:2003EEN124416:2003(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle4 5 Reagents.5 6 Apparatus .6

13、7 Sampling.7 8 Procedure .7 9 Calculationandexpressionofresults. 9 10 Testreport 9 AnnexA (normative) Spectrallinesandoxidiserfuelcombinations .10EN124416:2003(E) 3 Foreword Thisdocument(EN124416:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC209“Zincandzincalloys, thesecretariatofwhichisheldbyAFNOR“

14、. ThisEuropeanStandard shallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbySeptember2003,andconflictingnationalstandardsshallbewithdrawnatthe latestbySeptember2003. Withinitsprogrammeofwork,TechnicalCommitteeCEN/TC209entrustedCEN/TC209/ WG6“Meth

15、odsof analysisandtesting ”withthepreparationthefollowingdocument: EN124416,ZincandzincalloysChemicalanalysisPart6:DeterminationofaluminiumandironFlameatomic absorptionspectrometricmethod. Thisstandardispartofaseriesofelevenstandards.Theotherstandardsare: EN 124411, ZincandzincalloysChemicalanalysisP

16、art1:Determinationofaluminiuminzincalloys Titrimetricmethod ; EN 124412, ZincandzincalloysChemicalanalysisPart2:Determinationofmagnesiuminzincalloys Flameatomicabsorptionspectrometricmethod ; EN 124413, ZincandzincalloysChemicalanalysisPart3:Determinationoflead,cadmiumandcopper Flameatomicabsorption

17、spectrometricmethod ; EN124414, ZincandzincalloysChemicalanalysisPart4:Determinationofironinzincalloys Spectrophotometricmethod. EN 124415, ZincandzincalloysChemicalanalysisPart5:Determinationofironinprimaryzinc Spectrophotometricmethod ; prEN124417, ZincandzincalloysChemicalanalysisPart7:Determinat

18、ionoftinFlameatomic absorptionspectrometricmethodafterextraction ; prEN 124418, ZincandzincalloysChemicalanalysisPart8:Determinationoftininsecondaryzinc Flameatomicabsorptionspectrometricmethod ; prEN 124419, ZincandzincalloysChemicalanalysisPart9:DeterminationofnickelinzincalloysFlame atomicabsorpt

19、ionspectrometricmethod ; prEN 1244110, ZincandzincalloysChemicalanalysisPart10:Determinationofchromiumandtitaniumin zincalloysSpectrophotometricmethod ; prEN 1244111, ZincandzincalloysChemicalanalysisPart11:Determinationofsiliconinzincalloys Spectrophotometricmethod ; AnnexAisnormative. Accordingtot

20、heCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,Swi

21、tzerlandandtheUnitedKingdom.EN124416:2003(E) 4 1Scope ThisEuropeanStandardspecifiesaflameatomicabsorptionspectrometrymethodinzincandzincalloysforthe determinationofaluminiumandiron.ItisapplicabletotheproductsspecifiedinEN988,EN1179,EN1774, EN12844andEN13283. Itissuitableforthedeterminationofironcont

22、ents(massfractions)between0,001%and0,5%andaluminium contents(massfractions)between0,0005%and0,5%. NOTE EN124411specifiesamethodforthedeterminationofaluminiumcontents(massfractions)between3%and 30%. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpub

23、lications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditiono

24、fthe publicationreferredtoapplies(includingamendments). EN988, ZincandzincalloysSpecificationsforrolledflatproductsforbuilding. EN1179, ZincandzincalloysPrimaryzinc. EN1774, ZincandzincalloysAlloysforfoundrypurposesIngotandliquid. EN12060:1997, ZincandzincalloysMethodofsamplingSpecifications. EN1284

25、4, ZincandzincalloysCastingsSpecifications. EN13283, ZincandzincalloysSecondaryzinc. 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thetermsanddefinitions giveninEN12060:1 997andthefollowing apply. flameatomicabsorptionspectrometry measurementoftheabsorptionofelectromagneticradiation,emi

26、ttedbyanelementatadeterminedwavelength,by anabsorbentmediumflameformedofatomsofthesameelementinthegroundstate.Eachelementabsorbs radiationofspecificwavelengthsandtheintensityoftheradiationabsorbedisproportionaltotheconcentrationof saidelement 4Principle Asampleofthemetaloralloyisdissolvedinhydrochlo

27、ricacidand,afteradequatedissolutionandatomisationof thesolutioninanairacetylene(ornitrousoxideacetylene)flame,thecontentoftheparticularcomponentis determinedbyatomicabsorptionspectrometry. ThewavelengthsofthespectrallinesareshowninannexA.EN124416:2003(E) 5 5Reagents 5.1General Duringthetestuseonlyre

28、agentsofknownanalyticalgradeanddistilledordemineralisedwater. 5.2Hydrochloricacid, r =1,19g/ml 5.3Nitricacid, r =1,4g/ml 5.4Hydrochloricacid (1+1) Mix1volumeofhydrochloricacid(5.2)with1volumeofwater. 5.5Hydrogenperoxide ,30%(massfraction) 5.6Iron ,1g/lsolution Introduce1,000gofpureiron(purity99,95%)

29、intoa250mlbeakerfittedwithawatchglassanddissolveby carefullyadding50mlofhydrochloricacid(1+1)(5.4).Aftereffervescencehasstopped,add1mlofhydrogen peroxide(5.5)andboiltocompletedissolution.Cooltoroomtemperatureandtransfertoa1lvolumetricflask.Add 50mlofhydrochloricacid(5.2),dilutetothemarkwithwaterandm

30、ix.Storeinapolyethylenebottle. 1mlofthissolutioncontains1mgofiron. 5.7Standardiron,solutionA Transfer10mlofironsolution(5.6)intoa500mlvolumetricflask.Add5mlofhydrochloricacid(5.2),dilutetothe markwithwaterandmix. 1mlofthissolutioncontains0,02mgofiron. Thissolutionshallbefreshlypreparedjustbeforeuse.

31、 5.8Standardiron,solutionB Transfer10mlofironsolution(5.6)intoa200mlvolumetricflask.Add2mlofhydrochloricacid(5.2),dilutetothe markwithwaterandmix. 1mlofthissolutioncontains0,05mgofiron. Thissolutionshallbefreshlypreparedjustbeforeuse. 5.9Aluminium, 1g/lsolution Introduce1,000gofaluminium(purity99,95

32、%min)intoa250mlbeakerfittedwithawatchglassanddissolveby carefullyadding50mlofhydrochloricacid(1+1)(5.4).Aftereffervescencehasstopped,add1mlofhydrogen peroxide(5.5)andboiltocompletedissolution.Coolandtransfertoa1lvolumetricflask.Add50mlofhydrochloric acid(5.2),dilutetothemarkwithwaterandmix.Storeinap

33、olyethylenebottle. 1mlofthissolutioncontains1mgofaluminium. 5.10 Standardaluminium,solutionA Transfer10mlofaluminiumsolution(5.9)intoa100mlvolumetricflask.Add5mlofhydrochloricacid(5.2),dilute tothemarkwithwaterandmix.EN124416:2003(E) 6 1mlofthissolutioncontains0,1mgofaluminium. Thissolutionshallbefr

34、eshlypreparedjustbeforeuse. 5.11 standardaluminium,solutionB Transfer20mlofaluminiumsolution(5.9)intoa100mlvolumetricflask.Add5mlofhydrochloricacid(5.2),dilute tothemarkwithwaterandmix. 1mlofthissolutioncontains0,2mgofaluminium. Thissolutionshallbefreshlypreparedjustbeforeuse. 5.12Zinc,200g/lsolutio

35、n Introduce200gofzinc(purity99,995%,absentofironandaluminium)intoa2lbeaker.Add100mlofwaterand 700mlofhydrochloricacid(5.2)carefullyinsmallamountstocontroltherateofreaction.Add1mlofhydrogen peroxide(5.5)andevaporatecarefullyuntilasyrupyconsistencyisobtained.Aftercooling,dilutetoabout800ml withwateran

36、dwarmgentlytodissolveanysalts.Transferintoa1lvolumetricflask,dilutetothemarkwithwater andmix.Storeinapolyethylenebottle. 1mlofthissolutioncontains0,2gofzinc. 5.13 Sodiumchloride ,100g/lsolution 5.14Aquaregia Mix3volumesofhydrochloricacid(5.2)and1volumeofnitricacid(5.3). 5.15 Hydrochloricacid (1+19)

37、Mix1volumeofhydrochloricacid(5.2)with19volumesofwater. 5.16 Ammoniasolution , r =0,91g/ml 5.17 Lanthanumsolution Introduce5goflanthanumoxide(La 2 O 3 )ina200mlbeaker.Add5mlofwaterandcarefullydissolvewith20mlof hydrochloricacid(5.2).Afterdissolution,cooltoroomtemperatureandtransfertoa1lvolumetricflas

38、k.Dilutetothe markwithwaterandmix. 5.18Phenolphthaleine,ethanolicsolution. Dissolve1gofphenophtaleinein100mlofethanol. 6Apparatus 6.1General Allglasswareusedforthepreparationofthesolutionsandfortheimplementationofthemethodshallbecleaned withboilingaquaregia(5.14)priortouse.EN124416:2003(E) 7 6.2Spec

39、ificequipment Inadditiontostandardlaboratoryapparatus,thefollowingshallbeused: a) atomicabsorptionspectrometer, equippedwithapremixburner,withfacilitiesforusingtheoxidiserfuel combinationsofairacetyleneornitrousoxideacetylene. NOTE Excitationsourcesshouldbeoperatedinaccordancewiththemanufacturersrec

40、ommendations.Theopticalpath lengthwithintheflameshouldbebetween5cmand10cm. SpectrallinesandoxidiserfuelcombinationsarelistedinannexA. b) membranefiltrationapparatus ,withcellulosenitratemembranefilterhavingadiameterof50mmor30mm andaporesizeof0,45 m mor0,6 m m. 7Sampling Thetestsampleshallbeselecteda

41、ndpreparedinaccordancewiththeproceduregiveninEN12060. 8Procedure 8.1Testportion Weigh10gofthetestsampletothenearest0,001g. 8.2Preparationofthetestsolution 8.2.1 Introducethetestportion(8.1)intoa400mlbeakerfittedwithawatchglassanddissolvebycarefully adding50mlofhydrochloricacid(5.2).Oxidiseandcomplet

42、ethedissolutionbyaddingafewdropsofhydrogen peroxide(5.5). 8.2.2 Decomposetheexcesshydrogenperoxidebyboiling. 8.2.3 Cooltoroomtemperatureandtransfertoa100mlvolumetricflask.Intheparticularcaseofaluminiumin therangeofcontents(massfractions)between0,005%to0,025%,add5mlofsodiumchloridesolution(5.13) befo

43、redilutiontothemark(seeTable1).Dilutetothemarkwithwaterandmix. 8.2.4 UsingTable1asaguide,transferappropriatevolumesofsamplesolution(8.2.3)sodiumchloridesolution (5.13),andhydrochloricacid(5.2)toa100mlvolumetricflask.Dilutetothemarkwithwaterandmix. Table1Testsolutions Element Concentrationrange %(massfractions) Samples