1、DRAFT FOR DEVELOPMENT DD ENV 14226:2002 Advanced technical ceramics Test methods for ceramic powders Determination of calcium, magnesium, iron and aluminium in silicon nitride by using flame atomic absorption spectroscopy (FAAS) or inductively coupled plasma atomic emission spectroscopy (ICP-AES) IC
2、S 81.060.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWDD ENV 14226:2002 This Draft for Development, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and
3、Strategy Committee on 20 May 2002 BSI 20 May 2002 ISBN 0 580 39644 4 National foreword This Draft for Development is the official English language version of ENV 14226:2002. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of public
4、ations and is of a provisional nature because it is considered that further experience is required in its application before it is converted into a European and hence British Standard. It should be applied on this provisional basis, so that information and experience of its practical application may
5、 be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion into a European Standard. A review of this publication will be initiated 2 years after its publication by the Euro
6、pean organization so that a decision can be taken on its status at the end of its three-year life. The commencement of the review period will be notified by an announcement in Update Standards. According to the replies received by the end of the review period, the responsible BSI Committee will deci
7、de whether to support the conversion into a European Standard, to extend the life of the prestandard or to withdraw it. Comments should be sent in writing to the Secretary of BSI Technical Committee RPI/13, Advanced technical ceramics, at 389 Chiswick High Road, London W4 4AL, giving the document re
8、ference and clause number and proposing, where possible, an appropriate revision of the text. 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 i
9、n 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 Standards Electronic Catalogue. Summary of pages This document comprises a front cover, an inside front cover, the ENV tit
10、le page, pages 2 to 11, 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 CommentsEUROPEANPRESTANDARD PRNORMEEUROPENNE EUROPISCHEVORNORM ENV14226 April2002 ICS81.060.30 Englishversion Adv
11、ancedtechnicalceramicsTestmethodsforceramic powdersDeterminationofcalcium,magnesium,ironand aluminiuminsiliconnitridebyusingflameatomicabsorption spectroscopy(FAAS)orinductivelycoupledplasmaatomic emissionspectroscopy(ICPAES) CramiquestechniquesavancesMthodesdessaipour poudrescramiquesDterminationdu
12、calcium, magnsium,fer,etaluminiumdanslenitrurepar spectromtriedabsorptionatomiquedanslaflamme (FAAS)ouparspectromtriedmissionatomiqueavec plasmacouplageinductif(ICPAES) HochleistungskeramikPrfverfahrenfrkeramische PulverBestimmungvonCalcium,Magnesium,Eisenund AluminiuminSiliciumnitridmittelsFlammen
13、Atomabsorptionsspektroskopie(FAAS)oder Atomemissionsspektroskopiemitinduktivgekoppeltem Plasma(ICPAES) ThisEuropeanPrestandard(ENV)wasapprovedbyCENon23December2001asaprospectivestandardforprovisionalapplication. TheperiodofvalidityofthisENVislimitedinitiallytothreeyears.AftertwoyearsthemembersofCENw
14、illberequestedto submittheir comments,particularlyonthequestionwhethertheENVcanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannouncetheexistenceofthisENVinthesamewayasforanENandtomaketheENVavailablepromp tly atnationallevelinanappropriateform.Itispermissibletokeepconflictingnationalstand
15、ardsinforce(inparalleltothe ENV)untilthefinal decisionaboutthepossibleconversionoftheENVintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Swi
16、tzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENV14226:2002EENV14226:2002(E) 2 F
17、oreword ThisdocumentENV14226:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC184“Advanced technicalceramics”,thesecretariatofwhichisheldbyBSI. ThisPrestandardincludesaBibliography. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoannounceth
18、isEuropeanPrestandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom.ENV14226:2002(E) 3 1Scope ThisEuropeanPrestandardspecifiesmethodsforthedeterminationofcalcium,mag
19、nesium,iron,and aluminium,usingflameatomicabsorptionspectroscopy(FAAS),orinductivelycoupledplasma atomicemissionspectroscopy(ICPAES). Themethodsareapplicabletotheconcentrationrangesgiveninclause3. 2Normativereferences ThisEuropeanPrestandardincorporates,bydatedorundatedreference,provisionsfromother
20、publications.Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthe publicationsarelistedhereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyof thesepublicationsapplytothisEuropeanPrestandardonlywhenincorporatedinitbyamendmentor revision.Forundatedreferencesthelatested
21、itionofthepublicationreferredtoapplies(including amendments). ISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods. 3Concentrationranges Themethodisapplicabletoconcentrationrangesforeachelementasfollows: Calcium 510 6 to50010 6 ( w/w); Magnesium 510 6 to20010 6 ( w/w); Iron 510 6 to25
22、010 6 ( w/w); Aluminium 510 6 to100010 6 ( w/w). 4Principle Thetestsampleisdecomposedusingeitheracidpressuredigestion,oracidpressuremicrowave digestion. TheresultingsolutionisdilutedtoadefinedvolumeandnebulizationintoaflameforFAAS,orintoa plasma,forICPAES(seeclause1). Foreachelement,comparisonismade
23、oftherecordedabsorbanceoremittedintensityforadetermined analyticalpeakwiththoseofarangeofsolutionsofknownconcentrations. 5Sampling BulksamplingisnotwithinthescopeofthisEuropeanPrestandardandthemethodstartswitha laboratorysizedsample.ENV14226:2002(E) 4 6Reagentsandmaterials 6.1General Allreagents,and
24、substances,shallbeofatleastanalyticalgrade.Distilledordeionisedwater, conformingtoISO3696,shallbeusedthroughoutthewholeprocedure. 6.2Reagentsforpreparation 6.2.1HydrofluoricacidHF 20 about1,16gml 1 . 6.2.2Nitricacid 20 about1,4gml 1 . 6.3.Reagentsforcalibration 6.3.1Allreagentsshallbeofultrahighpuri
25、ty. 6.3.2Silicon,commercialsolutionwithverylowandknownimpuritylevels,concentration10gl 1 . 6.3.3Calcium,commercialsolutionorsolutionobtainedbythedissolutionofapurechemicalproduct, concentration0,1gl 1 . 6.3.4Magnesium,commercialsolutionorsolutionobtainedbythedissolutionofapurechemical product,concen
26、tration0,1gl 1 . 6.3.5Iron,commercialsolutionorsolutionobtainedbythedissolutionofapurechemicalproduct, concentration0,1gl 1 . 6.3.6Aluminium,commercialsolutionorsolutionobtainedbythedissolutionofapurechemical product,concentration0,1gl 1 . 7Apparatus 7.1 SpectrometerusedforFAASandICPAESanalysisshoul
27、dcomplywiththerequirementslaid downinECSC/C9.TheICPAESshallbeequippedwithanebulizationsystemandtorchresistantto hydrofluoricacid. 7.2 Dryingoven ,capableofbeingcontrolledat(110 10) o C. 7.3 Desiccatorcontainingeffectivedesiccant. 7.4 Balance,toreadto0,1mg. 7.5 Samplejarorbag ,withaseal.ENV14226:2002
28、(E) 5 7.6 50mlvolumetricflasks ,resistanttohydrofluoricacid(e.g.polypropylene,PTFE). 7.7 Vessels,resistanttohydrofluoricacid,ofatleast30mlcapacity,andsuitableforoperationat (170 15) o Cfor15h,forusewith(7.8). 7.8 Acidpressuredigestionapparatus . 7.9 Vessels,resistanttohydrofluoricacid,forusewith(7.1
29、0). 7.10 Microwave digestionsystem . 8Samplepreparation Dryapproximately10gofthesampleat(110 10) o C,inthedryingoven(7.2)foratleast1h. Removeandcoolittoroomtemperatureinadesiccator(7.3).Whencoolstorethesampleinajaror bagthatisairtight(7.5). 9Procedure 9.1General 9.1.1 Dissolvethetestsamplebyacidpres
30、suredigestion(9.2)orbyacidpressuremicrowavedigestion (9.3) 9.1.2 Runablankinparallelwiththechosenprocedure,usingidenticalreagents,conditions,and dilutionsthroughout. 9.2Acidpressuredigestion Weigh(0,100 0,0005)goftestsample(8)intothePTFElinedvessel(7.6). Carefullyadd3mlofHF(6.2.1)and1mlofHNO 3 (6.2.
31、2). Installthecapandclosethepressurevesselaccordingtothemanufacturersinstructions. Placethepressurevesselintotheheatingblockanddigestfor15hat(170 15) o C. Allowtocool. Aftercooling,openthepressurevesselaccordingtothemanufacturersinstructions. Checkthatthetestportionhasbeencompletelydigested. Ifnot,r
32、epeatthedigestion.ENV14226:2002(E) 6 Transferthedissolvedsampletoa50mlvolumetricflask(7.6)andrinsethepressurevessel,andlid withdistilledordeionisedwater. Makeuptothemarkwithdistilledordeionisedwaterandmixwell. 9.3Acidpressuremicrowavedigestion Examplesofprocedures: 9.3.1Weigh0,1g 0,0005goftestsample
33、(8)intothevessel(7.9). Add5mlofHF(6.2.1)and1mlofHNO 3 (6.2.2)andsealaccordingtothemanufacturersinstructions. Putthecappedvesselintothemicrowave. Applythefollowingstages: Stage1:Powerlevel60%for2min; Stage2:Powerlevel30%for15min; Stage3:Powerlevel0%for5min; Stage4:Powerlevel20%for20min. Allowthevesse
34、ltocoolinthemicrowaveforabout20min. Repeattheheatingcycleoncemore. Inspecttoseeifthetestsamplehascompletelydigested. Whencool,openthevesselaccordingtothemanufacturersinstructions. Transferthedissolvedsampleintoa50mlpolypropylenevolumetricflask(7.6),andrinsethepressure vessel,andlidwithdistilledordei
35、onisedwater. Mix,andmakeuptothemarkwithdistilledordeionisedwater. 9.3.2 Weigh0,1g 0,0005goftestsample(8)intothepressurevessel(7.7) Add,carefully,10mlofHF(6.2.1)and2mlofHNO3(6.2.2),andsealthevesselaccordingtothe manufacturersinstructions. Placethecappedvesselintothemicrowave. Applythefollowingstages:
36、ENV14226:2002(E) 7 Stage1:Temperature50 o Cfor2min; Stage2:Temperature150 o Cfor6min; Stage3:Temperature260 o Cfor18min; Stage4:Temperature0 o Cfor10min. Coolandopenthevesselaccordingtothemanufacturersinstructions. Inspectthesolution. Ifthesamplehasnotcompletelydissolvedrepeatstages1to4again. Transf
37、erthesolutionintoa50mlvolumetricflask(7.6),washingthepressurevesselandlidwith distilledordeionisedwater. Mixandmakeuptothemarkwithdistilledordeionisedwater. 10Calibrationsolutions Acalibrationgraphisobtainedusingcalibrationsolutionspreparedtospantherangeofconcentrations ofelementstobedeterminedinthe
38、testsolution.Thecalibrationsolutionsarepreparedusingthesame acidsthatwereusedtodigestthetestsampletoensureaccuratematrixmatching. Thefollowingprocedureisgivenasanexample: PreparethecalibrationsolutionsbyaddingthevolumesofsolutionsindicatedinTable1toaseriesof 50mlvolumetricflasks(7.6).Whenadditionsar
39、ecomplete,mixandmakethevolumeofeachflask uptothemarkwithdistilledwaterordeionisedwater.ENV14226:2002(E) 8 Table1Preparationofcalibrationsolutions S0 S1 S2 S3 S4 HF(6.2.1),ml 3,00 3,00 3,00 3,00 3,00 HNO 3 (6.2.2),ml 1,00 1,00 1,00 1,00 1,00 Si(6.3.2),ml 6,00 6,00 6,00 6,00 6,00 Ca(6.3.3),ml 0 0,05 0
40、,10 0,30 0,60 Concentration,10 6 ( w/v) 0 0,10 0,20 0,60 1,20 Mg(6.3.4) 0 0,025 0,05 0,15 0,30 Concentration,10 6 ( w/v) 0 0,05 0,10 0,30 0,60 Fe(6.3.5),ml 0 0,025 0,05 0,15 0,30 Concentration,10 6 ( w/v) 0 0,05 0,10 0,30 0,60 Al(6.3.6) 0 0,10 0,25 0,50 1,00 Concentration,10 6 ( w/v) 0 0,20 0,50 1,0
41、0 2,00 UsingetherFAASorICPAES,makemeasurementsofthecalibrationsolutionsforeachofthe elementsandprepareacalibrationcurveofabsorbanceorintensityagainstconcentrationforeach element. 11FAASAnalysis 11.1General Fitthecorrectburnerandlighttheflameinaccordancewiththemanufacturersinstructionsforigniting and
42、extinguishingthenitrousoxide/acetyleneflametoavoidexplosion.Ifnecessary,weartintedsafety glasseswhenevertheflameisburning. Setthewavelengthfortheelementtobeanalysed. NOTEThewavelengthsinTable2canbeusedfortheanalysis.Accordingtoanalyticalprocedureandelement concentration,otherwavelengthsmaybeused. Af
43、terpreheatingtheburnerfor10min,adjustthefuelandtheburnertoobtainmaximumabsorbance whileaspiratingthehighestcalibrationsolution. Aspiratewaterandthecalibrationsolutionstoestablishthattheabsorbancereadingisnotdriftingand settheinitialreadingforS0tozeroabsorbance. Aspiratewaterandascendingcalibrationso
44、lutionstoobtaindatatoconstructacalibrationgraph. Aspiratewaterandthentheblanksolutiontoobtainanabsorbanceavalue. Aspiratewaterandthentestsampletoobtainanabsorbancevalue. Calculatetheconcentrationofelementinthetestsample(clause12).ENV14226:2002(E) 9 11.2Inductivelycoupledplasmaspectrometer Followthemanufacturersinstructionsforignitingtheplasma.Ifnec
