1、BRITISH STANDARD BS EN 725-12:2001 Advanced technical ceramics Methods of test for ceramic powders Part 12: Chemical analysis of zirconia The European Standard EN 725-12:2001 has the status of a British Standard ICS 81.060.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS E
2、N 725-12:2001 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 June 2001 BSI 06-2001 ISBN 0 580 37668 0 National foreword This British Standard
3、 is the official English language version of EN 725-12:2001. The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secr
4、etary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standard
5、s Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to
6、understand the text; present to the responsible European committee any enquiries on the interpretation, 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
7、 cover, an inside front cover, the EN title page, pages 2 to 20, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHEN
8、ORM EN72512 April2001 ICS81.060.30 Englishversion AdvancedtechnicalceramicsMethodsoftestforceramic powdersPart12:Chemicalanalysisofzirconia CramiquestechniquesavancesMthodesdessaipour poudrescramiquesPartie12:Analysechimiquede zircone HochleistungskeramikPrfverfahrenfrkeramische PulverTeil12:Chemisc
9、heAnalysevonZirconiumoxid ThisEuropeanStandardwasapprovedbyCENon19February2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernin
10、gs uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesam
11、estatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMA
12、LISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN72512:2001EPage2 EN72512:2001 Contents Page Foreword 3 1Scope 4 2Normativereferences 4 3Concentrationranges 5 4Pr
13、inciple 5 5Reagents 5 6Apparatus 7 7Testsample 7 8Samplepreparation 8 9Calibration 10 10Adjustmentoftheapparatus 14 11Measurements 16 12Expressionofresults 17 13Accuracy 18 14Testreport 19 Bibliography 20Page3 EN72512:2001 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC184“Adv
14、ancedtechnical ceramics“,thesecretariatofwhichisheldbyBSI . ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyOctober2001,andconflictingnationalstandardsshall bewithdrawnatthelatestbyOctober2001. EN725Methodsoftestforcerami
15、cpowdersconsistsof12Parts: Part1: Determinationofimpuritiesinalumina Part2: Determinationofimpuritiesinbariumtitanate(ENV) Part3: Determinationoftheoxygencontentofnonoxidesbythermalextractionwithacarriergas Part4: DeterminationofoxygencontentinaluminiumnitridebyXRFanalysis(ENV) Part5: Determinationo
16、ftheparticlesizedistribution Part6: Determinationofthespecificsurfacearea Part7: Determinationoftheabsolutedensity Part8: Determinationoftappedbulkdensity Part9: Determinationofuntampedbulkdensity Part10: Determinationofcompactionproperties Part11: Determinationofdensificationonnaturalsintering(ENV)
17、 Part12: Chemicalanalysisofzirconia Thisstandardincludesabibliography. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,It
18、aly,Luxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom.Page4 EN72512:2001 1Scope ThispartofEN725specifiesmethodsforthedeterminationofthelevelsofsilicon,aluminium, titanium,iron,calcium,magnesium,potassium,sodium,yttrium,hafnium,ceriumandstrontiumusing flameatomicabso
19、rptionspectrometry(FAAS)andinductivelycoupledplasmaatomicemission spectrometry(ICPAES).Thesemethodsareapplicabletotheconcentrationrangesgiveninclause3, expressedasoxides. 2Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromother publications.Thesenormativeref
20、erencesarecitedattheappropriateplacesinthetextandthe publicationsarelistedhereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyof thesepublicationsapplytothisEuropeanStandardonlywhenincorporatedinitbyamendmentor revision.Forundatedreferencesthelatesteditionofthepublicationreferredtoapp
21、lies(including amendments). ISO3696 WaterforanalyticallaboratoryuseSpecificationandtestmethods ECSC/CI9 ChemicalanalysisofferrousmaterialsOperationalguidelinesforthe applicationofflameatomicabsorptionspectrometryinstandardmethods forthechemicalanalysisofironandsteelPage5 EN72512:2001 3Concentrationr
22、anges TheFAASandICPAESmethodsshallbeapplicabletotheconcentrationrangesforeachoxideas follows: Siliconoxide 10 g/gto5000 g/g; Aluminiumoxide 10 g/gto5000 g/g; Titaniumoxide 5 g/gto2000 g/g; Ironoxide 5 g/gto2000 g/g; Calciumoxide 5 g/gto5000 g/g; Magnesiumoxide 5 g/gto5000 g/g; Potassiumoxide 5 g/gto
23、2000 g/g; Sodiumoxide 5 g/gto2000 g/g; Yttriumoxide 5 g/gto5000 g/g; Hafniumoxide 100 g/gto5000 g/g; Ceriumoxide 5 g/gto5000 g/g; Strontiumoxide 10 g/gto5000 g/g. NOTEForconcentrationsabove5000 g/g,theXrayfluorescence(XRF)method,in prENISO12677:1998,shouldbeused. 4Principle Thetestsampleisdecomposed
24、byusingeitherafusionmethodoranacidmicrowavedissolution method.Thesolutionistransferredtoavolumetricflaskanddilutedtoaknownvolume.The determinationismadeusingFAASorICPAES 5Reagents 5.1General Reagentsofatleast99,99%purityorbetter,calibrationsolutionsofultrahighpurityanddistilled waterorwaterofpurity2
25、(accordingtoISO3696)orequivalent,shallbeused. 5.2Reagentsforfusion 5.2.1Lithiumtetraborate, Li 2 B 4 O 7 5.2.2Nitricacid,densityat20 o Capproximately1,33gml 1 , HNO 3Page6 EN72512:2001 5.3Reagentsforacidmicrowavedissolution 5.3.1Sulfuricacid(96%), H 2 SO 4 5.3.2Ammoniumfluoride, NH 4 F 5.3.3Hydroflu
26、oricacid(40%), HF 5.3.4Hydrochloricacid(30%), HCl 5.3.5Nitricacid(65%), HNO 3 5.4Reagentsforcalibration 5.4.1Purezirconiaofverylowandknownimpuritylevels 1 ) 5.4.2General Commercialsolutionsorsolutionsobtainedbydissolutionofpurechemicalproductataconcentration levelof0,1g/lofthefollowingshallbeused. 5
27、.4.2.1Silicon, Si 5.4.2.2Aluminium, Al 5.4.2.3Titanium, Ti 5.4.2.4Iron, Fe 5.4.2.5Calcium, Ca 5.4.2.6Magnesium, Mg 5.4.2.7Potassium, K 5.4.2.8Sodium, Na 5.4.2.9Yttrium, Y 5.4.2.10Hafnium, Hf 5.4.2.11Cerium, Ce 1 ) JohnsonMattheyspecpure,totalimpurities50 g/gfor30impurities,isanexampleofasuitableprod
28、uctavailablecommercially. ThisinformationisgivenfortheconvenienceofusersofthisstandardanddoesnotconstituteanendorsementbyCENofthisp roduct.Page7 EN72512:2001 5.4.2.12Strontium, Sr NOTECertificatesforanalysisshouldbeobtained. 6Apparatus 6.1Ordinarylaboratoryapparatusandapparatusforfusion. 6.1.1 Plati
29、numgoldalloycrucible andlid, withacapacityof35ml. 6.1.2 Mufflefurnace, suitableforoperationupto1200C 50C. 6.1.3 Magneticstirrer. 6.2ApparatusforacidmicrowavedissolutionandforFAASanalysis. 6.2.1 Microwaveunit, includingPTFElinedpressurevessels. 6.2.2 Flameatomicabsorptionspectrometer, conformingtoECS
30、C/CI9. 6.3ApparatusforICPAESanalysis 6.3.1 Inductivelycoupledplasmaspectrometer. 7Testsample Drythesampleat110C 10Cforatleast1h. Forthefusionmethod(see8.1): Weighapproximately0,08gofsampletothenearest0,0005g. Fortheaciddissolutionmethod(see8.2): Weighapproximately0,3gor0,125gofsampletothenearest0,00
31、05g.Page8 EN72512:2001 8Samplepreparation 8.1Fusion Weigh1goflithiumtetraborate(see5.2.1)intoaplatinumgoldalloycrucible(see6.1.1). Addapproximately0,08goftestsample(seeclause7)andmix. Placethecrucibleandcontentsintothemufflefurnace(see6.1.2)maintainedat1200C 50Cfor atleast30min. Afterthefirst15min,s
32、wirlthecontentsofthecrucibleforafewsecondsandreplaceinthefurnace. Attheendofthe30minremovethecruciblefromthefurnaceanddipitsbaseinwateratambient temperaturetoallowseasyremovalofthemeltfromthecrucible. Putthecrucibleandmeltintoa250mlbeakerwhichcontains50mlofwaterand10mlofnitricacid (see5.2.2). Placet
33、hebeaker,coveredwithawatchglass,onamagneticstirrer(see6.1.3)andmaintainthe agitationuntilcompletedissolution. Removethebeakerfromthestirrer.Removethecrucibleandrinsewithdistilledwaterandtransferthe solutionintoa100mlvolumetricflask.Mixandmakeuptothemarkwithdistilledwater. NOTE1Automaticfusionapparat
34、usshouldbeusedwithcaretoensurecompletefusion thesample,followedbyasuitabledissolutionprocedure. NOTE2Topreventthemeltsticking,theuseofanewcrucibleisrecommended. 8.2Acidmicrowavedissolution 8.2.1 Example1 Weighapproximately0,3gofthetestsample(seeclause7)intothepressurevesselandadd3mlof sulphuricacid(
35、see5.3.1)and270mgofammoniumfluoride(see5.3.2). Closethevesselwiththevalveandhandtighten.Placethevesselintothemicrowaveunit.Setthe microwaveprogrammeandstart.Page9 EN72512:2001 NOTETypicalprogrammeformicrowavetimeandpowersettings: Time(min) Power(%) 26 0 15 30 50 20 20 Attheendoftheprogrammeallowtoco
36、ol,removethevesselandopencarefully. Transferthesolutionintoa100mlvolumetricflask.Rinsethevesselwithdistilledwaterandtransfer totheflask.Mixandmakeuptothemarkwithdistilledwater. 8.2.2Example2 Weighapproximately0,125goftestsample(seeclause7)intothepressurevesselandadd7mlof hydrofluoricacid(see5.3.3)an
37、d7mlofhydrochloricacid(see5.3.4)and1mlofnitricacid (see5.3.5). Closethevesselwiththevalveandtightenbyhand. Placethevesselintothemicrowaveunit.Settheprogrammefor5minat250C,followedby10min at260C,andstart. Attheendoftheprogramme,allowtocool,removethevesselandopencarefully. Transferthesolutionintoa100m
38、lpolypropylenevolumetricflask. Rinseoutthevesselwithdistilledwaterandtransfertotheflask.Add5,5mlofhydrochloricacid (see5.3.4). Mixandmakeuptothemarkwithdistilledwater. 8.3Blanktest Witheachanalysis,carryoutablankinparallelwiththetestsampleusingidenticalreagents, conditions,andanalyticalproceduresina
39、ccordancewiththechosendissolutionmethod(see8.1or 8.2).ThisblanksolutionshallbenamedS 0 .Page10 EN72512:2001 9Calibration 9.1General Theoptimumcalibrationgraphisobtainedusingcalibrationsolutionswithconcentrationsthatare compatiblebothwithFAASorICPAESanalyticalmethods,andwiththeimpurityconcentrationsi
40、n thesample. WARNINGTakecaretostoresolutionsinnonglassvessels. Exampleproceduresaregivenin9.2.1 and 9.2.2 9.2Calibrationsolutions 9.2.1Fusionmethod Weighfiveportionsof0,08gpurezirconia(see5.4.1)anddissolveaccordingtothemethodofsample preparationgivenin8.1.Transferthesolutionintoa100mlgraduatedflask,
41、withaminimumof washing.Addthequantitiesofstandardsolutions5.4.2.1to5.4.2.12giveninTable1andmakeupto themarkwithdistilledwater.Page11 EN72512:2001 Table1Volumeofstandardsolutions(l)tobeaddedtothecalibrationsolutionsafterfusion Calibration Standardsolutions (l) solution S 0 S 1 S 2 S 3 S 4 Si 0 50 100
42、 150 200 Al 0 50 100 150 200 Ti 0 100 150 200 250 Fe 0 50 125 200 300 Ca 0 50 125 200 300 Mg 0 100 150 200 250 K 0 50 150 250 350 Na 0 50 125 200 300 Y 0 50 150 250 350 Hf 0 50 150 250 350 Ce 0 50 150 250 350 Sr 0 50 150 250 350Page12 EN72512:2001 9.2.2Acidmicrowavemethod Weighfiveportionsof0,3gpure
43、zirconia(see5.4.1)anddissolveaccordingtothemethodofsample preparationgivenin8.2. Addthequantitiesofstandardsolutions5.4.2.1to5.4.2.12giveninTable2andmakeuptothemark withdistilledwater. NOTEForacidmicrowavedissolution,Example2in8.2.2,thevolumesinTable2should beadjustedforthesamplemass. Table2Volumeofstandardsolutions(l)tobeaddedtothecalibrationsolutions aftermicrowavedissolution Calibration Standardsolutions (l) solution S 0 S 1 S 2 S 3 S 4 Si 0 150 300 500 750 Al 0 20
