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
