ISO 03613-2021.docx

INTERNATIONA1.STANDARDISO3613editionF(Wrth202105Meta1.1.icandotherinorganiccoatingsChromateconversioncoatingsonzinc,cadmium,a1.uminium-zinca1.1.oysandzinc-a1.uminiuma1.1.oysTestmethodsRevetementsmeta1.1.iquesetautresrefetementsinorganiques一Couchesdeconversionauchromatesurzinc,cadmiumeta1.1.iagesd1.a1.uminiumzincetdezmc-a1.uminiumMdthodesd'essaiIsoR强附卬02喇©ISO2021COPYRIGHTPROTECTEDDOCUMENT©ISO2021岫rkdea/山thUcdOthcnviscjft<c三orrtmcehDVBiwixuioiti08phnn11UatiocBhr<1.>hotoc<>p)Mng,ptbcatonpostingontheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanherequestedfromeitherISOattheaddressbe1.oworIS<smemberbodyinthecountryoftherequester.%,tft晒Iandonnet8CH-1214*crnicr,GenevaPhone：M1.22749O1.11Pub1.ishedinSwitzerhndContentsForewordivIntroductionv2 Scope13 Normativereferences14 Termsanddefinitions15 Reagents26 Apparatus3Testmethods46.1 1Cner*1.46.2 Testforthepresenceofaco1.our1.esschromatecoatingonzinc46.3 Testforthepresenceofaco1.our1.esschromatecoatingonzinc-a1.uminiumand!fractionofa1.umnuttiS311oys.56.5 Testforthepresenceofhexava1.entchromiuminbothco1.our1.essandco1.ouredGsqmatcG?HW睁56.5.1 Testmethodemp1.oyingtestso1.utionC1.56.5.2 Testmethodemp1.oyinga1.ternativetestso1.utionC2(destructive)56.5.3 E愉福给On研U1.tSSPeCtroPhotOmeter76.6 Determinationofhexava1.entchromiumcontentofco1.ouredchromatecoatings86.6.1 Preparationofca1.ibrationgraphH>-"""".-一M"“”"一,""-”-".-"”"”"-6.6.4 Expressionofresu1.ts86.7 Determinationoftota1.chromiumcontentofco1.ouredchromatecoatings96.7.2 Bhtptaititibnofca1.ibrationgraph96.7.3 Determination9卜XPreSSion(Jfrsu1.ts；6.8 的期盼bionAWrtt三tt出h8fipaOfbothco1.our1.essandco1.ouredchromate96.9 Testforadhesionbyabrasion97 6.10Qua1.ityeva1.uationtestofchromate1.ayersonzincandcadmiumsurfaces10Testreport108 Ib1.1.OgraPhy11ForewordISO(theInternationa1.OrganizationforStandardization)isawor1.dwidefederationofnationa1.standardsttiugh(ISOmrtmiw)bMd>niK盟RAucekdHpfff1.QbbGgbodyIcommitteehasbeenestab1.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.opthisdocumentandthoseintendedforitsfurthermaintenanceare蜩则搬of1.SOIEC(M1.糖八°忱刷感期taN螂$觊萨%COrdanCetheeditoria1.ru1.esoftheISO/IECDirectives.Part2(seewww.iso.org/direc1.ives).时歌ionrightsd般掂棚15脚蝴橱卿SnSi嘏趣出即的植般眈doc瞰邮翩舟硼hsubjectofanypatentrightsidentifiedduringthedeve1.opmerUW4io÷uwMM41.beintheIntroductionand/orontheISO1.istofpatentdec1.arationsreceived(seewww.iso.org/pa1.ents).Anytradeusedinthisconstitutenameendorsement,documentisinformationgivenfortheconvenienceofusersanddoesnotForanexp1.anationofthevo1.untarynatureofstandards,themeaningofISOspecifictermsand哪蝴蜘明瓶ationc。的福P奥爽融Mthe可般IIi潴称柝福ticn1盘件戏3以徽?盘?isoforeword.htn1.愠isc加SH三WbW勘th1.aredar胡韵R+mitteefemm根WMd般rdiz杯腓的处8脚&他幽Kmmi瞬4oongs,TC262,Meta1.1.icandotnerinorganiccoatings,inc1.udingforcorrosionprotectionandcorrosiontestingofmeta1.sanda1.1.oys,inaccordancewiththeAgreementontechnica1.cooperationbetweenISOandCEN(ViennaAgreement).Thisfourtheditioncance1.sandrep1.acesthethirdedition(ISO3613:2010),whichhasbeentechnica1.1.yrevised.Themainchangescomparedwiththepreviouseditionareasfo1.1.ows:Tab1.e1hasbeenrevised;ana1.ysismethoddescribedin6.5wasa1.ignedwiththemethoddescribedinIEC62321-7-1；pWHfVWb(Wfttfif1.tionoftestso1.utionC2in432hasbeenrevisedandasecondstandard1.imitingtimehasbeenamendedin6.1;procedurefortestingwithtestso1.utionC2hasbeenrevisedin÷2;descriptionoftheca1.ibrationofspectrophotometerhasbeenadded.A三假d电塔郴fi1.三1.icsth1.scah8副RRwtm0三HHW4三nadona1.standardsbody.AIntroductionconversioncoatingsaswe1.1.asthetota1.chromiumcontentofchromateconversioncoatings."chromating”.ThedeprecatedZpassivation*isnotcorrect,asitdoesnotconformtotheISO2080designation,coatingsrep1.acinghexava1.entconversioncoatings.Passivationcontainingnowadaysoftenuseda1.1.owedCr(V1.)-free-A1.1.rightsreservedThisdocumentspecifiesmethodsforthequa1.itativedeterminationofthepresenceofchromateTheapp1.icationofverythin,co1.our1.ess,practica1.1.yinvisib1.echromateconversioncoatingsisfrequent1.yca1.1.ed“passivation：whi1.etheapp1.icationofthicker,co1.ouredchromateconversioncoatingsisca1.1.edandisthereforetermChromateconversioncoa1.ingsarebasedonaso1.utioncontainingCr(V),Boththeprocessso1.utionandtheContainchromatechromium.ThetermProductsisCr(V1.)arenotforwithinEUandprocessesusingCr(V1.)arestrict1.yregu1.ated.Meta1.1.icandotherinorganiccoatingsChromateconversioncoatingsonzinc,cadmium,a1.uminium-zinca1.1.oysandzinc-a1.uminiuma1.1.oysTestmethodsWARNINGThisdocumentca1.1.sfortheuseofsubstancesand/orproceduresthatcanbeinjurioustohea1.thifadequatesafetymeasuresarenottaken.Thisdomentdoesnotaddressanyhea1.thhazards,safetyorenvironmenta1.mattersassociatedwithitsuse.Itistheresponsibi1.ityoftheuserofthisdocumenttoestab1.ishappropriatehea1.th,safetyandenvironmenta1.1.yacceptab1.epracticesandtakesuitab1.eactionsforanynationa1.andinternationa1.regu1.ations.1Scope thepresenceofco1.our1.esschromateconversioncoatings,andzinc-a1.uminium(massfractionofa1.uminium:5%)a1.1.oys, themassperunitareaofbothco1.our1.essandco1.ouredcoatings, thequa1.ityofchromatecoatings. chromiumandco1.ouredproportionsandconversioncoatingscontaininge1.ectrochemica1.hexava1.entchromatepo1.ymersorwax.arefreefromanysupp1.ementarycoatings,suchasoi1.,waterorso1.vent-2Normativereferencesconstitutesrequirenents1.atesteditiondoment.referencedreferences,(inc1.udingamendments)app1.ies.app)ics.GravimetricmethodsIECTer111.Sanddefinitions(esf7nPart230:TestsTestDb:Dampheat,cyc1.ic(12h/12hcyc1.e)NCgrmwenddpfniricnwAre1.iwtpdinrhiwdccimonrThisdocumentspecifiesmethodsforthedeterminationof thepresenceOfhexava1.entchromiuminco1.our1.essandco1.ouredcoatingsonzincorcadmiumora1.uminiumzinc(massfractionofa1.uminium:55%fwithinarangeof54%to56%massfraction) thetota1.chromiumcontentperunitareaonzincandcadmium, thesatisfactoryadhesionofchromateconversioncoatings,andThesemethodsareapp1.icab1.etoco1.our1.essinvaryingchromateproducedbyeitherchemica1.ortriva1.entandprocesses,andbasedcoatingsthatThefo1.1.owingdocumentsarereferredtointhetextinsuchawaythatsomeora1.1.oftheircontentundatedreferences,theofthisoftheFordateddocumenton1.ytheanyeditioncitedForISO3892.Conversioncoatingsonmeta1.1.icmateria1.s-Determinationofcoatingmassperunitarea-ISO4520,Chromateconversioncoatingsone1.ectrop1.atedzincandcadmiumCOatingS360068-2-30rEnvironmenta1.ISOandIECmaintaintermino1.ogica1.databasesforUSRinSiandardizadonatthefo1.1.owingaddresses:ISOOn1.inebrowsingp1.atform:avai1.ab1.eath1.1.pswsvw.iso.orgobpUf1.tessonIyorheRunfaJ*ofspecd«rf«»t?dr»ri)1.1.0ica1.gradeanddisti1.1.edwaterorwaterofequiva1.entpurity,4.1 Testso1.utionA(see6.2).Disso1.veIgofdipheny1.carbazideinamixtureof20m1.ofacetone,60m1.ofg1.acia1.aceticacidand40m1.Gihchfiri1.hd也ig®1.oraimkbf(idni【nbcaker.h和irt1.U&mhofso】UdDn:(?附皿11帆谕出ftb故idc*JFnivJ8A4tGHWofhydrogenperoxide(30%vo1.umefraction)s1.ow1.ywithcontinuousstirring.1.eavetheso1.utionintheopenbeakerfor24hinafumecupboard,toa1.1.owexcessch1.orinetoescape,beforeuse.肖挑rtJA%te田也唱§3都丽丽t¼Ufoncent?咖MH1.ter1.o<¼rdeder.sixmonths.4.2 Testso1.utionB(see6.3).Disso1.ve50gof1.eadacetatetrihydrate(CH3COO)2Pb3HzOin11Ofdisti1.1.edwaterorwaterofeq1.uUoie11tputrtifi11surettadjrifcytHwso1.utionaridJqHpee<WthepHoftheAnywhiteprecipitateformedduringtheinitia1.preparationoftheso1.utionmaybedisso1.vedbysma1.1.8序onssti<B幅吊4g国MJ1.暨超烯Ftisappear.notreducedtoava1.uebe1.ow5,5.Discardthe4.3 Testso1.utionC(see6,5).4.3.1 Testso1.utionC1.Disso1.ve0,4gofdipheny1.carbazideinamixtureof20m1.ofacetoneand20m1.ofethano1.(96%).Afterdisso1.ution,ntide20th1.r)7J6prior(U1.hx)phosphoricacidso1.utionand20m1.ofdisti1.1.edwater.Preparethis4.3.2Testso1.utionC2.Add700m1.oforthophosphoricacidrofspecificgravity1,7,t。250m1.ofdisti1.1.edwaterorwaterofequiva1.entpurityandmakeupto1000m1.Disso1.ve0,5gof1,S-C1.ipheny1.carbazideofana1.ytica1.reagentgradein50m1.ofacetoneofana1.ytica1.reagentgrade.Di1.utes1.ow1.y,whi1.estirring,with50m1.ofdisti1.1.edwaterorwaterofequiva1.entpurity(蜂idfafftMsukso1.ution阴述小件atRWisGt4cj;祗出hqaeda由to网disco1.oured.Fromthisstockso1.ution,preparetwoCr(VI)standardso1.utions.1.,5dipheny1.carbazideto1,5-dipheny1.carbazone,whichformsared-vio1.etco1.ouredcomp1.exwiththedeve1.opedCr(III).Thesamp1.etobetestedshou1.dhaveasurfaceareaof(50±5)cm2.Forfastenersorsamp1.eswitha§福超姐WaCeOb前铜nusetot则曲g81r8C的州Hfe9加访1晚SSi隰!刷附祖河H则帆连1s(11faceareamaybeusedbyreducingthewaterextractionvo1.ume,whi1.emaintainingthesamesurfaceareatoextractionvo1.umeratio(1Cm2:1m1.).Aminimumsurfaceareaof25cm2isrecommended.Simi1.ar1.y,池瞬心邮加用*姆11碘us%a哪蝴做郦r*1.飒scra%dju加强UrfaCe.Theresu1.tingabrasionsha1.1.a1.sobeana1.ysed.搁舐)曲翻M黜隔Or岫WrW丸hcq乱衡配b榔W席抑ping1.跖眼曲槐fk<三映照1.withforat1.east10mintodeoxygenateit.Thentota1.1.yimmersethesamp1.eintotheboi1.ingwaterandcoverthebeakeragainwithawatchg1.ass.Extractthesamp1.efor(10±0,5)minonceboi1.ingisresumed.If融噬州tU瓶喉雕器制陶稀幽砸赵福瞧聊潞为u腌s。IU槛眠超钳解晓临IOUr1.eSSandfreeofprecipitate.Adjustthevo1.umeto50m1.ifnecessary,fi1.tertheso1.utionthrougha0,45mmembranefi1.terintoadrybeaker.Makeuptheso1.utiontothemarkwithwater(seeC1.ause4)orreduce951.om1.fif<aruti。播牖就仙唠ath腋砒喇。聊J<R8F相加ker.血VOh联邮相册1.rbazideso1.ution(4.3.2)andmixwe1.1.A1.1.owtneso1.utiontostandtor10minfortheco1.ourreactiontobecomp1.eted.Theremainingportionoftheextractwi1.1.serveastheb1.ank.V1%8w>徜幅fWP%三tioncoatirfrptiOrfSJhWRW袖eb1.ance他W1.againsttheb1.ankwiththespectrophotometer(5.2).Makethreemeasurementsandtaketheaverageasthefina1.absorbanceofthesamp1.e.Insomecases,dependingonthetypeOfspectrophotometerused,thecorrectionfortheb1.ankhastobemademanua1.1.yintheco1.1.ecteddata.Measuretheabsorbanceofthecomparisonso1.utionfor0,10gcm2Cr(V1.)(4.3.2)threetimesasdescribedabove.Taketheaverageofthreemeasurementsasthefina1.absorbanceofthatcomparisonso1.ution.Measuretheabsorbanceofthecomparisonso1.utionfor0r13gc1112Cr(VI)(4.3.2)threetimesasdescribedabove.Taketheaverageofthreemeasurementsasthefina1.absorbanceofthatcomparisonso1.ution.1.1.4 Expressionofresu1.tsTheresu1.tsareexpressedasshowninTab1.e1.Tab1.e1Comparisonofso1.utionsObservationResu1.tingCr(Vi)concentrationincoatingDefinition2tttB问出nJJ三SamIntX>040gcmcm2andz<0.13gdetermination.fcx1.:Cie口thecomparisonso1.utionfor0.13g2>0,13gcmThesamp1.econtainsCr(VI).cm2Cr(VI)(4.3.2).扪欧册UrW%Mhethef删*Sonco1.our纵凯阿凡况褥4fi三藤勘A1.n网通棚曲鼓制KHnIenS展anthanc1.ear1.ydeterminedaspositiveforCr(VI)rmeasurementwiththespectrophotometerisnotnecessary.However,thereportsha1.1.statethattheresu1.tissignificant1.yabove0；13gcmzCr(V1.)basedonvisua1.8h黑冷ationpe*f1.ta座由岳蹲届fiUnta俄眠小山砥牺2Aco1.orimetricmeasurementsha1.1.1.1.5 Ca1.ibrationofspectrophotometerTheSpectiophotometersha1.1.beca1.ibratedusingab1.ankandthreestandardso1.utionsataminimum.Thestandardso1.utionconcentrationssha1.1.bracket0,10gm1.Cr(VI)and0,13gm1.Cr(V1.).Zerothespectrophotometerwiththe0,0gm1.b1.ankstandardandsavethisso1.utiontore-zerotheinstrumentbeforereadingsamp1.esandstandards.BtesdtncesWdgtoatM04ntUettr(Ve<MitoOwv贯andjMdasnintH由Htgaatiohytanda田剃OEngca1.ibrationcurve(1.inearfitwithzerointercept)sha1.1.haveaCone1.ationcoefficient0,995oranewcurvesha1.1.bebui1.t.Ca1.ibrationrvescanbeusedforuptoonemonthfrominitia1.generation.Co1.orimetricinstrumentsdesignedspecifica1.1.yforhexava1.entchromiumdetectionat540nmcanhaveapermanentca1.ibrationprovidedbythemanufacturerandnofurtherca1.ibrationisneeded.RefertoHgertHQR<ft1.SfftSUtonsa1.ysis.ensurethattheinstrumentisfunctioningproper1.yanditsworkingRegard1.essoftheinstrumenttype,aperformanceverificationusingthetwocomparisonso1.utions(seear“<WaM国卬耳尔福OUKiREtion1.8¾1W品CHy.measurementsandattheendofeachsamp1.esequencetoIDiiheiifraiia1.tiNdtbUtMifcffitbeotn5itMt<fdiwhnfft4f!piiitt<i(f1.)1.cgm1.)!byan>reti)cntsth1.6!u1.t%,theca1.ibrationsha1.1.bere-measured.NM住Me窗用ahftJa电面品4蝴粽f超R1.heS做88fVmX融1三2织肥>帮寄隔淅H的附蒯版a刊1.nceofthesamp1.esinthesequencesha1.1.bere-measured.6.6 DeterminationOfhexava1.entchromiumcontentofco1.ouredchromatecoatings6.6.1 Preparationofca1.ibrationgraph6.6.1.1Toaseriesoffive250m1.vo1.umetricf1.asks,addrespective1.y0m1.(i.e.thecompensationso1.ution),10m1.,20m1.,30m1.and40m1.ofstandardpotassiumdichromateso1.ution(4.9).Addtoeachf1.ask100m1.ofwaterand3m1.ofdi1.utesu1.furicacid(4.5).Toonef1.ask,add3m1.oftestso1.utionD(4.4)(4<*0)indf1.WieKaacByinarkniintheWvpeatdddiefcte争rocedwrmjtiddBfeintIitashRirofphosphatebufferso1.ution6.6.1.2absorptiometer(5.1)portionspectrophotometer(5.2anabsorptioneadreadingmeasuretheabsorbanceintestso1.utionD(4.4)astheco1.ourisnotstab1.e.Subtractthecompensationso1.ution(see6.6.1.1)fromeachreadingandp1.otthedifferencesagainstmicrogramsofchromiumper250m1.6.6.2 B1.anktestCarryoutab1.anktestinaccordancewith6.6.3andrecordtheresu1.t.fijm1.e)f1.Hheb1.atfkagcnts&9df0ters:S阿13阑dPMt1.itet1.tf6.6.pfttassiumdichromatc6.6.3 Determination6.6.3.1Cutatestpiecemeasuringabout50m11100mmfromthecoateditem.Bringto(heboi1.50m1.ofdisti1.1.edwaterinasuitab1.evesse1.andtota1.1.yimmersethetestspecimeninthis.1.eachforexact1.y5minwhi1.ethewatercontinuestoboi1.,removethespecimenandrinseoverthevesse1.Coo1.thevesse1.tmd250cnitcntsvo!umctricth11ipRuuxrthvetk1.-Btuiuti1.t1.utntx1.u-fki3kidw(th4.ft0a1.fim1.'fan!4hcdstiU8tiiuntentsadd3m1.oftestso1.utionD(4.4)andmix.Exact1.y2minaftertheadditionoftestso1.utionD,add25m1.ofphosphatebufferso1.ution(4.10),di1.utetothemarkandmix.6.6.3.2absorptiometer(5.1Jportionspectrophotometer5.2anabsorptionce1.1.readingmeasuretheabsorbanceintestso1.utionD(4.4)astheco1.ourisnotstab1.e.Subtracttheb1.anktestreading(see6.6.2)fromtheinstrumentreadingand,usingtheca1.ibrationgraph(see6.6.1),converttheresu1.tintomicrogramsper250m1.6.6.3.3Ifthereadingobtainedfa1.1.swithintheportionoftheca1.ibrationgraphbe1.ow10g,repeatthedeterminationusinga1.argertestpiece(1,5timesto2timesthedimensionsgivenin6.6.3.1).6.6.4 Expressionofresu1.tsDeterminethetota1.surfaceareaofcoatingonthetestspecimen,insquarecentimetres.DividetheBteeava1.entChromiumcontent,Obtaine<ibe1.11digdXPreJinidIiJgNidK(P6jhbjsurfaqBtimetntefcoating.6.7 Determinationoftota1.chromiumcontentofco1.ouredchromatecoatings6.7.1 Preparationofca1.ibrationgraph6.7.2 B1.anktest6.7.3 Determination6.7.3.1si