ISO 04491-1-2023.docx

INTERNATIONA1.STANDARDISO4491-1editionSecond2023-03Meta1.1.icpowdersDeterminationofoxygencontentbyreductionmethods一f飘篁a1.guide1.inesPoudresmeta1.1.iquesDosagedeVoxygeneparIesmethodesdereduction-Panie1:Directivesgenera1.esReferencenumberIS0449b1.:2023(E)©ISO2023COPYRIGHTPROTECTEDDOCUMENT©ISO2023IUirhM*hedbdi1.iUedotherwiseupdhi.or啪UIBndttaeDmk<nroni(ncm11ni10tf1.*Mqn1.C6pW11opypMRHt1.onmaytheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbe1.oworISO'smemberbodyinthecountryoftherequester.f),WV>fifiHipB1.andonnet8CH-1214Vernier,GenevaPhone：M1.22749O1.11觥ftte:丽丽BQrgPub1.ishedinSwitzer1.andContentsForewordivIntroductionv2 Scope13 Normativereferences14 Termsanddefinitions15 Samp1.ing1Meaningoftheresu1.tsaccordingtothemethodused25.1 Hydrogenasareducingagent26 5.2Carbonasareducingagent:reductionextractionmethod37 Summaryoftheimp1.ementationofmethodsforoxygendeterminationbyreduction3Practica1.app1.icationofthestandardmethods4ForewordISO(theInternationa1.OrganizationforStandardization)isawor1.dwidefederationofnationa1.standardsttiugh(ISOtnnhnfaaib11dg"hucekWwptagbody1.nmcrraMbtandriJ>teG4(nowhhUyca11tie<h11t2committeehasbeenestab1.ishedhastherighttoberepresentedonthatcommittee.Internationa1.organizations,governmenta1.andnon-governmenta1.,in1.iaisonwithISO,a1.sotakepartinthework.ISOco1.1.aboratesc1.ose1.ywiththee1.ectrotechnica1.standardization.Internationa1.E1.ectrotechnica1.Commission(IEC)ona1.1.mattersofTheproceduresusedtodeve1.opthisdocumentandthoseintendedforitsfurthermaintenanceareof1.SO1.EC(VifY1的Mtheeditoria1.ru1.esoftheISO/IECDirectives,Part2(secwww.iso.org/direc1.ives).时歌Onrightsd般掂棚1SW雌ns施娥卿瞄做喇颤比咻耨蝴瞬.subjectofanypatentrightsidentifiedduringthedeve1.opmen13th»doc向U1.beintheIntroductionand/orontheISO1.istofpatentdec1.arationsreceived(seewww.iso.org/patents).Anytradeusedinthisconstitutenameendorsement,documentisinformationgivenfortheconvenienceofusersanddoesnotForanexp1.anationofthevo1.untarynatureofstandards,themeaningofISOspecifictermsand族aR涸枭取OrRanfWMWass忠jSW窿inweW¾1.ft1.沁nBarP挑Jdead虐¾e盘w¼,w.iso.orgisotorewod.htm1.布备救胡(W底ffgred"feOdSTM懒Hea书的，做脩OTAfcpo1.W仰册W瓠28mmitteewiththeEuropean()mmitteeforStandardization(CEN)Technica1.CommitteeCEN/SSM11,Powdermeta1.1.urgy,inaccordancewiththeAgreementontechnica1.cooperationbetweenISOandCEN(ViennaAgreement).Thissecondeditioncance1.sandrep1.acesthefirstedition(ISO4491-1:1989),ofwhichitconstitutesaminorrevision.Themainchangesareasfo1.1.ows:thenormativereferencesinC1.ause2havebeenupdated;一and7havechangedp1.ace;editoria1.correctionsandupdatedISOformathavebeenapp1.ied.A1.istofa1.1.partsintheISO4491seriescanbefoundontheISOwebsite.AnyfeedbackorquestionsonthisdocumentShoUIdbdiW1.Wh。usqfMnationa1.standardsbody.Acomp1.ete1.istingofthesebodiescanbefoundatwww.iso.org/inembers.htrn1.Introductionparticu1.armeta1.s.Amonga1.wayspresentimpuritieswhicha1.1.oypowder,presentininamountsgreaterthanthosemoistureCoatingspowderpreparationandspontaneous1.yformedstorage.oxidationofthemeta1.byairorproductionmateria1.and/orthefromtheCqUiPnWmPoWdCrS)JCfraCIOryCerarnicsimpuritiesoriginatingfrommasspractice,oxygencontentsinmeta1.1.icpowders1.iemost1.yintherangeofamassfractionof0,1%toaexamp1.e:b) reductionInethodsxontenhvhichre1.ated,presenttheIosstota1.1.ymasspartia1.1.y,samp1.ereducedbyreduction,orbyc) separationmethods,inwhich:eva1.uatedPhaseexamp1.ese1.ective1.ya1.uminiumpowder,a1.uminiumisdisso1.ved(assmedbromine-methano1.documentConsidersofmeta1.reductionmethods,asthesearecommon1.yusedin1.aboratoriesforInpowdermeta1.1.urgy,thepurityofthepowdersisanimportantparameterforthemanufactureofsinteredro1.eitisthevariousinanymeta1.ormaybeandpowder,oxygenp1.aysaencounteredincompactmeta1.s.Oxygenismost1.ycombinedintheformofoxideswhichappearinthefo1.1.owingways:Oxidefi1.mduringonpartic1.esurfaces,duringhand1.ingandbyOxideinc1.usions,beingeitheroxidesofthemainmeta1.remaining1.oca1.1.yunreducedduringthevtherawprocess(incaseofreduced(e.g.otheroxidefromme1.tingfurnaceinatomizationprocesses).Infractionof1%.Thedeterminationofoxygencontentcanbemadebymeansofmanyphysica1.orchemica1.methods,fora)specificmethods,suchasactivationana1.ysisormassspectrometry,inwhichthee1.ement0isdirect1.ydetermined;carbon.OxygeninisOxideseithertoare,oforofthethroughhydrogentotheamountofwaterorCO/COzproducedbythereaction;eithertheoxidephaseisse1.ective1.ydisso1.vedanddeterminedchemica1.1.y(forexamp1.eincopperpowder,wherecopperoxideisdisso1.vedbyhydroch1.oricacid);orthemeta1.(forisindisso1.ved,andtheinso1.ub1.eresidueinoxide)isreagent,1.eavinga1.uminiumoxide).Theana1.ysingagreatvarietyon1.ypowders.Meta1.1.icpowdersDeterminationofoxygencontentbyreductionmethodsfa里a1.guide1.ines1ScopeThisdocumentisthefirstpartofaseriesofstandardsdea1.ingwiththedeterminationofoxygencontentmetaUtfipwridmib)idifibNrrntthods.iHtepprifisith0>trit8idano)tained.thesemethodsandgivesThetestmethodsareapp1.icab1.egenera1.1.ytoa1.1.powdersofmeta1.s,a1.1.oys,carhidesandmixturesHowever,thereexistcertain1.imitationswhichdependuponthenatureoftheana1.ysedmeta1.These21.i,WWitive停超前(S(三e4.2Wst四，的Uw用白以S9his11H闻ent.Mf%傕才nrefrf1.*y<%1护aeediHbna1.1.Nt册PIie$.朝entundatedreferences,the1.atesteditionofthereferenceddocument(inc1.udinganyamendments)app1.ies.ISO3954,Powdersforpowdermeta1.1.urgica1.purposesSamp1.ingI8CM49械照g的配帼收Mh戚时面曲脸门ofoxygencontentbyreductionmethodsPart2:1.ossof网”现§DeterminationofoxygencontentbyreductionmethodsPart3:f÷W及水他4f佻i俯渊仰tf1.DeterminationofoxygencontentbyreductionmethodsPart4:Tota1.3TermsanddefinitionsNotermsanddefinitionsare1.istedinthisdocument.ISOandIECmaintaintermino1.ogydatabasesforuseinstandardizationatthefo1.1.owingaddresses:-ISOOn1.inebrowsingp1.atform:avai1.ab1.eathttps:/www.iso.org/obp4ECS俄澹杀：avai1.ab1.eathttpswww.e1.ectFopedia.orgForsamp1.ingofthepowder,theproceduresinISO3954sha1.1.beused.Thepowdersha1.1.betestedintheas-receivedcondition.frtuthUAtxU(etts(j11ashi1.iitgUiytorcaIdnq1.IatCS1.由HtdrtdOasft>hrhSPdii)辑aiiriartdragcnrffthtubttsCFhmpforc,Thetestportionsha1.1.betakenimmediate1.ypriortotheana1.ysis.5 Meaningoftheresu1.tsaccordingtothemethodused5.1 Hydrogenasareducingagent5.1.1tthetesttemperaturesprescribedinthedetermination,on1.ythefo1.1.owingmeta1.shaveoxidestota1.1.yreducib1.ebyhydrogen：Fe,Ni,Co,Cu,g,Sn,Pb,W,Mo,ReA1.1.othercommonoxidesarenotreducib1.e,inparticu1.arA2O3,S1.2,ZrO2andotheroxidesofa1.ka1.i,R(Bf1.1.VHPMdBMb.rare-earthmeta1.s.Oxidesofchromium,manganese,titanium,andvanadiummay5.1.2However,otherreactionswithconstituentsofthepowdertakep1.aceduringthereductionprocess.a) WtupriwuroodJiMnniteyrtncfcrirtdjin>hesentpoUiHesarnpWeaB<idii*-sg<heatingvhichpossib1.ybyb) E1.ements,suchascarbon,nitrogen,su1.phur,phosphorus,freeorcombinedinthepowder,maybeyMd郦蝴陟网棚搬出陶端CCa1.Y期物CO砸酶IeOrbccausethcyrcactWHhc) Somemeta1.spresentinthepowder,suchas1.ead,tin,cadmium,zinc,maybepartia1.1.yorcomp1.ete1.yvo1.ati1.ized,dependingonthetestconditions.d) Carbonpresentinthepowdercana1.soreduceoxidesunderthespecifiedtestconditions,andpossib1.ya1.sooxidesthatnorma1.1.yarenotreducedorareon1.ypartia1.1.yreducedbyhydrogen,suchaschromium,manganeseandvanadiumoxides.e) A1.1.oypowderscontainingmeta1.1.ice1.ementswithhighaffinityforoxygen,suchaschromium,manganese,si1.icon,a1.uminiumandtitanium,maybeoxidizedduringthe1.estbyreactionwiththeatmosphereorwith1.essrefractoryoxides,entai1.inganapparentdecreaseofmeasuredoxygencontent.5.1.31.ossmethod4491-2,testportion.sbctttedtoaeddheattreatmenthdrogen.measured.Origirvanestimateoftheoxygencontentofameta1.powder,theoxideofwhichisreducib1.ebyhydrog-thntrtHitA%浊tte1.ya(hm11t11HiVdytfw呷teHjkredqJcwd>am*EtaRrfcmektqkiHbmdimfe.2pure1.yconventiona1.,anditsreproducibi1.ityrequiresascrupu1.ousrespectoftheoperatingprocedure.Thismethodiscommon1.yusedinroutinecontro1.ofpowdersofcertaindefinedmeta1.sinaccordancewithISO4491-2.5.1.4Themethodofdeterminationoxygenemanatingfromhydrogen-reducib1.eoxidesinaccordancewithISO4491-3,thequantityofwater(brinedbyhydrogenreductionoftheseoxidesismeasuredbytitration.Incomparisonwiththe1.ossinhydrogenmethod,thismethodismorespecificforthefo1.1.owingreasons:Theinterferenceofmoistureandadsorbedgasesispreventedbypre-treatmentat1.owtemperature.Withas1.ightmodificationoftheprocedure,itispossib1.etodeterminethewatercontentofthesamp1.e.Theinterferenceofmeta1.1.oidsandofvo1.ati1.emeta1.sisavoided.producingCarbonbemonoxideTherefore,Whicha1.ternativemeasuredareSpecifiediitration.Consequent1.y,acarboninterference.Thisexamp1.eisapp1.icab1.emasspacticewhen0,02samp1.edpow(ierpresentistoan-interference.Oxygenmethodcorrespondinghydrogen-reducib1.ereductionofSomcaccountcarbonhydrogen-reducib1.eoxides,irrespectiveofwhethertheactua1.reductionhastakenp1.acebymeansagreementandinterpretationhydrogen.resu1.tsuchshou1.dcase,madeWithconditionssha1.1.besubjecttoaspecia1.5.2 Carbonasareducingagent:reductionextractionmethodargon).tempcrature,onOOO0CmetaIana1.ysed,eitherOpcratingvacuumconditions11owchoseninertgasa1.1.(forexamp1.e6 Summaryoftheimp1.ementationofmethodsforoxygendeterminationbyreductiona) carbon,forexamp1.e:whicharereducib1.ebyhydrogen("Hreducib1.e")andwhichpossib1.ycontainrepresentedbymcta1.ana1.ytica1.resu1.tshydrogen,thebehaviouroftheoxygenandcarboncontentisTab1.e1Representationofana1.ytica1.resu1.tswhenmeta1.sofoxidesarereducedbyhydrogenContentofoxygencontainedincarbonreducedoxidesOb) Anymeta1.(containingcarbonornot)However,interferenceofcarbonpresentinthesamp1.emayhavetobetakenintoaccountSomepartofthemeta1.oxides,whichotherwisemayhavebeenreducedbyhydrogen,arereducedbycarbon,1.owerresu1.twi1.1.obtained,dioxide,twonotmethodsbywaterMethod1:Oxygencontentcorrespondingtohydrogenrcducib1.coxides,withouttakingintoaccounta1.mostofcarbon(formethodhavinginfractionC<the%)orthecarbonisknowninbeUnrcactiveform.Thentheresu1.trepresentstheoxygencontentfromhydrogen-reducib1.eoxides.Method2:InthiscontenttheCOC2togasesre1.easedCarhOnoXide5,takingintooftheoxidesandcontainedintheHzcarriergastarequantitative1.yconvertedtomethaneandwateronanicke1.cata1.ystat380.Thetota1.waterdeterminedrepresentstheoxygencontentemanatingfromofcarbon.Withreferenceto5.1.2d),certainoxidescanbepartia1.1.yreducedbycarbon,i.e.oxideswhichotherwisewou1.dnotbereducedbyoftheInabethetestgreatcare.ThemethodinaccordancewithISO4491-4isbasedonthereductionofthesamp1.ebygraphiteatveryhighDepending(2theto3OOO),underoraareofpuresothattheoxidesreventhemostrefractoryones,arereducedtota1.1.y.Anyinterferenceiscomp1.ete1.yexc1.uded,andtheresu1.trepresentsaccurate1.ythetota1.oxygencontentofthesamp1.e.Twocasesareconsidered,Meta1.soxidesFe.Ni,Co,Cu,Ag,Sn,Pb,W,Mo.ReWhensuchatheisreducedbyaccordingtoTab1.e1.containedinhydrogenreducedoxidesOhfromremaining(unreduced)oxides0ContentofcarbonhavingreactedCoWhenreducedtota1.1.ybygraphite(reduction-extractionmethod),thetota1.oxygencontent.0t,ismeasured.7Practica1.app1.icationofthestandardmethodsTab1.e2givesasummaryoftheapp1.icab1.emethods,dependingonthetypeofpowderana1.ysedandMV¾ia)w1.ituxiRthu1.ui9gwinitfeuHM-natidw1.e0mhd.Itshou1.dbeemphasizedthatacombinationofonthe"hydrogen-reducib1.e"and-hydrogen-irreducib1.e"oxygen,i.e.thepresenceofrefractoryoxidesin"hydrt>gen-reducib!e"meta1.s;ontheinterna1.effectofcarbon,whenpresent,onthereductionofoxides.AnrR他物th硼蚓跌M%¼y冲y1.ossOm册蝌娜琼dtKy三JgWducibftgenptf1.ti8yway,thecontentofoxygennotreducedbyhydrogen(andbyinterna1.carbon)undertheconditionsofhydrogenreductioncanbedetermined.Tab1.e2ContentdetermineddependingonmethodusedPowderMethodHydrogen1.ossHydrogen-reducib1.eoxygenRcduction-CxtractionDirectmethodWithcorrectionforcarbonOninitia1.samp1.eOnsamp1.ereducedbyhydrogenNOTEInthistabic,interferencebymoisture,adsorbedgases,vo1.ati1.eandreoxidizab1.cmeta1.s,isassumedtobeabsent.ICS77.160