1、BRITISH STANDARD BS EN 10276-2:2003 Chemical analysis of ferrous materials Determination of oxygen content in steel and iron Part 2: Infrared method after fusion under inert gas The European Standard EN 10276-2:2003 has the status of a British Standard ICS 77.040.30 BS EN 10276-2:2003 This British S
2、tandard, was published under the authority of the Standards Policy and Strategy Committee on 9 July 2003 BSI 9 July 2003 ISBN 0 580 42239 9 National foreword This British Standard is the official English language version of EN 10276-2:2003. The UK participation in its preparation was entrusted to Te
3、chnical Committee ISE/18, Sampling and analysis or iron and steel, 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 referre
4、d 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 necessary provisio
5、ns 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 interpretation, or
6、 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 13 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 EN102762 July2003 ICS77.040.30 Englishversion ChemicalanalysisofferrousmaterialsDeterminationofoxygen contentinsteelandironP
8、art2:Infraredmethodafterfusion underinertgas AnalysechimiquedesmatriauxferreuxDterminationde lateneurenoxygnedelacieretdelafontePartie2: Mthodeparabsorptiondanslinfrarougeaprsfusionsous gazinerte ChemischeAnalysevonEisenwerkstoffenBestimmung desSauerstoffgehaltsvonStahlundEisenTeil2: MessungderInfra
9、rotabsorptionnachAufschmelzenunter Inertgas ThisEuropeanStandardwasapprovedbyCENon7May2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferen
10、cesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCen
11、trehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEF
12、ORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN102762:2003EEN102762:2003(E) 2 Contents Foreword. 3 1 Scope . 4 2 Normativer
13、eferences . 4 3 Principle. 4 4 Reagentsandmaterials 4 5 Apparatus 6 6 Sampling 6 7 Procedure 7 7.1 General. 7 7.2 Generalinstructions . 7 7.3 Testportion . 7 7.4 Blanktest . 7 7.5 Calibration . 8 7.6 Preparationtest . 8 7.7 Determination 8 7.7.1 Method1 8 7.7.2 Method2 8 8 Expressionofresults . 9 8.
14、1 Methodofcalculation . 9 8.2 Precision 10 9 Testreport . 12 Bibliography . 13EN102762:2003(E) 3 Foreword ThisdocumentEN102762:2003hasbeenpreparedbyTechnicalCommitteeECISS/TC20“Methodsof chemicalanalysisofferrousproducts”,thesecretariatofwhichisheldbySIS. ThisEuropeanStandardshallbegiventhestatusofa
15、nationalstandard,eitherbypublicationofanidentical textorbyendorsement,atthelatestbyJanuary2004,andconflictingnationalstandardsshallbewithdrawnat thelatestbyJanuary2004. ThisdocumentincludesaBibliography. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing cou
16、ntriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands, Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN102762:2003(E) 4 1Scope ThisEuropeanStandardspecifiesa
17、ninfraredmethodafterfusionunderinertgasforthedeterminationof oxygeninsteelandiron. Themethodisapplicabletooxygencontentsbetween0,0005%(m/m)and0,01%(m/m). 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications. Thesenormativereferencesareciteda
18、ttheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplyto thisEuropeanStandardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthe latesteditionofthepublicationreferredtoapplies(includinga
19、mendments). EN102761 ChemicalanalysisofferrousmaterialsDeterminationofoxygen insteelandironPart1:Samplingandpreparationofsteel samplesforoxygendetermination. ENISO14284 SteelandironSamplingandpreparationofsamplesforthe determinationofchemicalcomposition(ISO14284:1996). 3Principle Fusionofatestportio
20、ninasingleusegraphitecrucibleunderheliumgasataminimumtemperatureof 2000C.Combinationoftheoxygenfromthesamplewithcarbonfromthecrucibletoformcarbonmonoxide. Eventuallytransformationofcarbonmonoxideintocarbondioxide. Measurementofinfraredabsorptionofthecarbonmonoxideordioxideanduseofacalibrationcurvepl
21、otted usingthemeasurementsobtainedwithpotassiumnitrate. 4 Reagentsandmaterials Duringtheanalysis,unlessotherwisestated,onlyreagentsofrecognisedanalyticalgradeshallbeused.The followingreagentsandmaterialsshallbeused: 4.1Helium, highpurity,totalimpuritycontent0,0005%(m/m). Anoxidationcatalystcopper(II
22、)oxideorplatinumtubeheatedtoatemperatureabove450Cshallbeused priortoapurifyingunit,whenthepresenceoforganiccontaminantsissuspectedinthehelium. 4.2Magnesiumperchlorate,Mg(ClO 4 ) 2 ,(commercialdesignation:anhydrone),particlesizefrom1,2 mmto2,0mm,or AnhydrousCalciumsulphate,(CaSO 4 ),(commercialdesign
23、ation:drierite),particle sizefrom0,6mmto0,85mm. 4.3Sodiumhydroxideongranulatedsupport,(NaOH), (commercialdesignation:ascarite),particle sizefrom0,7mmto1,2mm. 4.4Copperoxide,CuO 4.5Platinum,PtEN102762:2003(E) 5 4.6Tinornickelcapsules, Forexample 5mm,length13mm,weight160mg,withlowoxygencontent, lessth
24、an0,1 m g/mgofoxygen. Cutofftheupperpartofthetincapsuletoreducetheweightto50mgorthelengthto8mm. 4.7Water,highpurity, deionized,preparedjustbeforeuse. 4.8Potassiumnitrate, KNO3,highpurity,maximumtotalimpuritycontent0,0005%(m/m). Drybeforeuseat100Cto105Cfor2handallowtocoolinadessicator. 4.9Potassiumni
25、tratestocksolution, correspondingto4mg/mlofoxygen. Weigh,tothenearest0,1mg,8,416gofpotassiumnitrate(4.8). Placeina100mlbeakeranddissolveinabout50mlofwater(4.7). Transferquantitativelytoa1000mlvolumetricflask,dilutetothemarkwithwater(4.7),andmix. 1mlofthepotassiumnitratestocksolutioncontains4mgofoxyg
26、enaspotassiumnitrate. 4.10Potassiumnitratedilutedstocksolution, correspondingto0,4mg/mlofoxygen. Thissolutionshallbepreparedfreshlybeforeuse. Transfer10mlofthepotassiumnitratestocksolutionina100mlvolumetricflask,dilutetothemarkwith water(4.7),andmix. 1mlofthepotassiumnitratestocksolutioncontains0,4m
27、gofoxygenaspotassiumnitrate. 4.11Potassiumnitratestandardsolutions. Thesesolutionsshallbepreparedfreshlybeforeuse. TransferthevolumelistedinTable1ofthepotassiumnitratestocksolution(4.9)andofthepotassiumnitrate dilutedstocksolution(4.10)inaseriesofnine100mlvolumetricflasks,dilutetothemarkwithwater(4.
28、7), andmix. 100 m lofeachofthepotassiumnitratestandardsolutionscontainthemassofoxygen(aspotassiumnitrate) listedinthelastcolumnofTable1.EN102762:2003(E) 6 Table1Potassiumnitratestandardsolutions Potassiumnitrate standardsolution Volumeofpotassium nitratestocksolution (4.9)added (exceptforsolution4.1
29、1.2) Massofoxygenin 1mlofthe potassiumnitrate standardsolution Massofoxygenin 100 m lofthe potassiumnitrate standardsolution 4.11.1 0ml a 0mg 0 m g 4.11.2 3mlofpotassiumnitrate dilutedstocksolution (4.10) 0,012mg 1,2 m g 4.11.3 1,0ml 0,04mg 4 m g 4.11.4 2,0ml 0,08mg 8 m g 4.11.5 3,0ml 0,12mg 12 m g
30、4.11.6 5,0ml 0,20mg 20 m g 4.11.7 10,0ml 0,40mg 40 m g 4.11.8 20,0ml 0,80mg 80 m g 4.11.9 30,0ml 1,20mg 120 m g a zeromember:Thestandardsolution(4.11.1)isinfactthewater(4.7)usedforpreparingthe solutions. 4.12Graphitepowder, highpurity,withlowoxygencontent. 5Apparatus Theapparatusrequiredforfusionoft
31、hetestportionandmeasurementofthecarbonmonoxideordioxide extractedmaybeobtainedcommerciallyfromanumberofmanufacturers.Themanufacturersinstructionsfor theoperationoftheinstrumentshallbefollowed. 5.1Graphitecrucible, singleuse Highpuritycruciblessuitedtotheapparatusshallbeused. 5.2 Crucibletongs shallb
32、eusedforhandlingthecrucibles. 5.3Glasswoolfilters 5.4Micropipette, 100 m l,shallbeused,limitoferrorshallbelessthan1 m l. 6Sampling SamplingshallbecarriedoutinaccordancewithENISO14284andEN102761.EN102762:2003(E) 7 7Procedure 7.1General Theriskinvolvedwhenusinganapparatusforfusingthetestportionaremain
33、lyrisksofburns.Crucibletongs (5.2)andappropriatecontainersfortheusedcruciblesshallbeused. 7.2General instructions Itshallbecheckedthatglasswoolfilters(5.3)arecleanandtheyshallbechangedasoftenasnecessary. Iftheelectricitysupplyhasbeenswitchedoffforalongtime,theinstrumentshallbeallowedtostabilisefor t
34、hetimerecommendedbythemanufacturer. Afterchangingthefilters(5.3)and/orreagents(4.2,4.3and4.4),orwhentheapparatushasbeeninoperative foraperiod,theinstrumentshallbeallowedtostabilisebycarryingouttrialanalyses,theresultofwhichareto bedisregarded,thenproceedwithblankcalibrationandpreparationtestsasindic
35、atedin7.4,7.5and7.6 beforeanalysingthesample. Iftheinstrumentusedprovidesadirectreadinginpercentageofoxygen,theinstrumentreadingshallbe adjustedforeachcalibrationrangeasfollows: UsingaCRMwithahighoxygencontent,recordthecontentsmeasuredatdifferentlevelsoffurnaceheating power.Therequiredheatingpowerfo
36、rthedeterminationoftestsamplesisthatatwhichthereadinglevelsoff. Inordertodetermineahighalloytestsample,ahighalloyCRMshallbeusedtoknowtherequiredheating power. 7.3 Testportion Preparethetestportionofapproximately1ginaccordancewithEN102761. Weighthetestportiontothenearest1mg. 7.4Blank test Priortothed
37、etermination,thefollowingblanktestshallbecarriedoutinduplicate. Proceedasin7.7withouttestportion,enteringaweightof1g,andsettingtheblanksubtractionofthe instrumenttozero. Obtainthereadingoftheblanktest. Themeanvalueoftheblanktestshallbesufficientlylowwhencomparedtotheoxygencontenttobe determinedinthe
38、testportion. Formeanvaluesbelow8 m g/gofoxygen,neitherthemeanblankvaluenorthedifferencebetweenthetwo blankvaluesshouldexceed0,5 m g/gofoxygen.Formeanvaluesabove8 m g/gofoxygen,neitherthemean blankvaluenorthedifferencebetweenthetwoblankvaluesshouldexceed2 m g/gofoxygen. Iftheblankvaluesareabnormallyh
39、igh,thesourceofcontaminationshallbeinvestigatedandeliminated. Ifthemeanvalueoftheblankissatisfactory,itmaythenbeintroducedintheblanksubtractiondeviceofthe instrument.EN102762:2003(E) 8 7.5Calibration Priortothedetermination,thefollowingcalibrationshallbecarriedout. Prepareaccordingto4.11atleastfives
40、olutionschosenfromsolutions4.11.1to4.11.9indicatedinTable1, accordingtothelevelofoxygencontenttobedetermined. Usingthemicropipette(5.4),transfer100 m lofeachofthefreshlypreparedpotassiumnitratestandard solutions(4.11.1to4.11.9)toeachtinornickelcapsule(4.6)respectivelyanddryat90Cto95Cfor2h. NOTEThedr
41、yingofthecalibrationsolutionsinthetinornickelcapsulesshouldbedonestepwise,inordertoavoid splashingandlossofcalibrationmaterialduetooverrapidheatingbeforecompletevaporisationofthewater. Carefullypressthetinornickelcapsuleandproceedasin7.7,usingthetinornickelcapsuleasatestportion, enteringasampleweigh
42、tofonegram,andsettingthesamplefusiontemperatureto2000Ctolimittin vaporisation. Prepareacalibrationgraphbyplottingthereadingobtainedfromtheinstrumentagainstoxygencontent expressedinmicrogramsfromthelastcolumnofTable1. 7.6Preparation test Priortothedetermination,thefollowingpreparationtestinduplicates
43、hallbecarriedout. ChooseaCRMorroutinesample(tobepreparedjustbeforedetermination)withanoxygencontentcloseto thatexpectedinthesamplestobeanalysed. Proceedasin7.3forthepreparationofthispreliminarysample. Proceedasin7.7forthedeterminationonthepreliminarysample. Theresultsshallbewithinthelimitsofacontrolchartforthepreliminarysample. Ifnot,checkthepreparationconditionsandrepeatthesamplepreparationtest. 7.7Determination 7.7.1Method 1 Theelectrodeshallbecle
