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REFERENCENUMBERISO147192011EISO2011INTERNATIONALSTANDARDISO14719FIRSTEDITION20111201CHEMICALANALYSISOFREFRACTORYMATERIALGLASSANDGLAZESDETERMINATIONOFFE2ANDFE3BYTHESPECTRALPHOTOMETRICMETHODWITH1,10PHENANTHROLINEANALYSECHIMIQUEDEMATRIAUXRFRACTAIRES,DUVERREETDMAUXDOSAGEDEFE2ETFE3PARLAMTHODESPECTROPHOTOMTRIQUEENUTILISANTLA1,10PHNANTHROLINECOPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011ECOPYRIGHTPROTECTEDDOCUMENTISO2011ALLRIGHTSRESERVEDUNLESSOTHERWISESPECIFIED,NOPARTOFTHISPUBLICATIONMAYBEREPRODUCEDORUTILIZEDINANYFORMORBYANYMEANS,ELECTRONICORMECHANICAL,INCLUDINGPHOTOCOPYINGANDMICROFILM,WITHOUTPERMISSIONINWRITINGFROMEITHERISOATTHEADDRESSBELOWORISOSMEMBERBODYINTHECOUNTRYOFTHEREQUESTERISOCOPYRIGHTOFFICECASEPOSTALE56CH1211GENEVA20TEL41227490111FAX41227490947EMAILCOPYRIGHTISOORGWEBWWWISOORGPUBLISHEDINSWITZERLANDIIISO2011ALLRIGHTSRESERVEDCOPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011EISO2011ALLRIGHTSRESERVEDIIICONTENTSPAGEFOREWORDIV1SCOPE12NORMATIVEREFERENCES13TERMSANDDEFINITIONS14PRINCIPLEOFMETHODSAANDB25SAMPLEPREPARATION26INTERFERENCES27SAMPLEDISINTEGRATIONANDMEASUREMENT28CALCULATIONANDEXPRESSIONOFRESULTS99TESTREPORT10ANNEXAINFORMATIVEPRECISION11BIBLIOGRAPHY13COPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011EIVISO2011ALLRIGHTSRESERVEDFOREWORDISOTHEINTERNATIONALORGANIZATIONFORSTANDARDIZATIONISAWORLDWIDEFEDERATIONOFNATIONALSTANDARDSBODIESISOMEMBERBODIESTHEWORKOFPREPARINGINTERNATIONALSTANDARDSISNORMALLYCARRIEDOUTTHROUGHISOTECHNICALCOMMITTEESEACHMEMBERBODYINTERESTEDINASUBJECTFORWHICHATECHNICALCOMMITTEEHASBEENESTABLISHEDHASTHERIGHTTOBEREPRESENTEDONTHATCOMMITTEEINTERNATIONALORGANIZATIONS,GOVERNMENTALANDNONGOVERNMENTAL,INLIAISONWITHISO,ALSOTAKEPARTINTHEWORKISOCOLLABORATESCLOSELYWITHTHEINTERNATIONALELECTROTECHNICALCOMMISSIONIECONALLMATTERSOFELECTROTECHNICALSTANDARDIZATIONINTERNATIONALSTANDARDSAREDRAFTEDINACCORDANCEWITHTHERULESGIVENINTHEISO/IECDIRECTIVES,PART2THEMAINTASKOFTECHNICALCOMMITTEESISTOPREPAREINTERNATIONALSTANDARDSDRAFTINTERNATIONALSTANDARDSADOPTEDBYTHETECHNICALCOMMITTEESARECIRCULATEDTOTHEMEMBERBODIESFORVOTINGPUBLICATIONASANINTERNATIONALSTANDARDREQUIRESAPPROVALBYATLEAST75OFTHEMEMBERBODIESCASTINGAVOTEATTENTIONISDRAWNTOTHEPOSSIBILITYTHATSOMEOFTHEELEMENTSOFTHISDOCUMENTMAYBETHESUBJECTOFPATENTRIGHTSISOSHALLNOTBEHELDRESPONSIBLEFORIDENTIFYINGANYORALLSUCHPATENTRIGHTSISO14719WASPREPAREDBYTECHNICALCOMMITTEEISO/TC33,REFRACTORIESCOPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,INTERNATIONALSTANDARDISO147192011EISO2011ALLRIGHTSRESERVED1CHEMICALANALYSISOFREFRACTORYMATERIALGLASSANDGLAZESDETERMINATIONOFFE2ANDFE3BYTHESPECTRALPHOTOMETRICMETHODWITH1,10PHENANTHROLINE1SCOPETHISINTERNATIONALSTANDARDSPECIFIESASPECTRALPHOTOMETRICMETHODWITH1,10PHENANTHROLINEFORTHEQUANTITATIVEDETERMINATIONOFFE2ANDFE3INOXIDICRAWANDBASICMATERIALSFORCERAMICS,GLASSANDGLAZES,EGFELDSPAR,KAOLINITES,CLAY,LIMESTONE,QUARTZREFRACTORYMATERIALSTHISINTERNATIONALSTANDARDCOULDBEEXTENDEDTOOTHERALUMINOSILICATEMATERIALS,PROVIDINGTHATUNCERTAINTYDATAISPRODUCEDTOSUPPORTITHOWEVER,THEREMIGHTBEPROBLEMSINTHEDECOMPOSITIONOFHIGHPURITYALUMINAANDCHROMEORESAMPLESTHEMETHODISNOTSUITABLEFORREDUCEDMATERIALS,SUCHASSILICONCARBIDE,GRAPHITEMAGNESIA,ETC2NORMATIVEREFERENCESTHEFOLLOWINGREFERENCEDDOCUMENTSAREINDISPENSABLEFORTHEAPPLICATIONOFTHISDOCUMENTFORDATEDREFERENCES,ONLYTHEEDITIONCITEDAPPLIESFORUNDATEDREFERENCES,THELATESTEDITIONOFTHEREFERENCEDDOCUMENTINCLUDINGANYAMENDMENTSAPPLIESISO648,LABORATORYGLASSWARESINGLEVOLUMEPIPETTESISO1042,LABORATORYGLASSWAREONEMARKVOLUMETRICFLASKSISO3696,WATERFORANALYTICALLABORATORYUSESPECIFICATIONANDTESTMETHODSISO5022,SHAPEDREFRACTORYPRODUCTSSAMPLINGANDACCEPTANCETESTINGISO6286,MOLECULARABSORPTIONSPECTROMETRYVOCABULARYGENERALAPPARATUSISO86561,REFRACTORYPRODUCTSSAMPLINGOFRAWMATERIALSANDUNSHAPEDPRODUCTSPART1SAMPLINGSCHEMEISO10725,ACCEPTANCESAMPLINGPLANSANDPROCEDURESFORTHEINSPECTIONOFBULKMATERIALSISO116482,STATISTICALASPECTSOFSAMPLINGFROMBULKMATERIALSPART2SAMPLINGOFPARTICULATEMATERIALSISO12677,CHEMICALANALYSISOFREFRACTORYPRODUCTSBYXRAYFLUORESCENCEXRFFUSEDCASTBEADMETHODISO26845,CHEMICALANALYSISOFREFRACTORIESGENERALREQUIREMENTSFORWETCHEMICALANALYSIS,ATOMICABSORPTIONSPECTROMETRYAASANDINDUCTIVELYCOUPLEDPLASMAATOMICEMISSIONSPECTROMETRYICPAESMETHODS3TERMSANDDEFINITIONSFORTHEPURPOSESOFTHISDOCUMENT,THETERMSANDDEFINITIONSGIVENINISO26845APPLYCOPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011E2ISO2011ALLRIGHTSRESERVED4PRINCIPLEOFMETHODSAANDBSAMPLESAREDIGESTEDINAMIXTUREOFHYDROFLUORICACIDANDSULFURICACIDINTHEPRESENCEOFACOMPLEXINGAGENT,1,10PHENANTHROLINE,FE2IONSFORMAPINKCOMPLEXTHEPINKCOMPLEXISMEASUREDPHOTOMETRICALLYAT510NMINANAQUEOUSSOLUTIONQUANTITATIVERESULTSAREOBTAINEDBYCALIBRATIONWITHREFERENCESOLUTIONSTHESUMOFTHEDETERMINATIONOFBOTHIRONSPECIESCORRESPONDSTOTHETOTALIRONCONTENTTHISINTERNATIONALSTANDARDPROVIDESTWOSAMPLEDISSOLUTIONTECHNIQUESIINMETHODA,TENTIMESMORESAMPLE500MGISNECESSARYTHANFORMETHODB20MGTO30MGASACONSEQUENCE,THEAMOUNTOFREAGENTSNEEDEDAREREDUCEDFORMETHODBINBOTHMETHODS,AHFH2SO4DISSOLUTIONOFTHESAMPLEISCARRIEDOUTMETHODSAANDBIMPLEMENTDIFFERENTSTRATEGIESTOAVOIDOXIDATIONOFFE2TOFE3DURINGTHESAMPLEDISSOLUTIONANDMEASUREMENTWHILEINMETHODATHESAMPLESREACTINANAIRANDLIGHTTIGHTREACTIONVESSELWITHNITROGEN,INMETHODBTHESOLUTIONISSTABILIZEDWITHNITRILOTRIACETICACIDINSIMPLEPOLYSTYRENECUVETTESCOOLEDBYICEBOTHMETHODSAREAPPLICABLEFORTHEFULLRANGEOFMATERIALSCOVEREDBYTHESCOPEOFTHISINTERNATIONALSTANDARDFORSAMPLESWHICHAPPEARMOREHETEROGENEOUS,AHIGHERSAMPLEMASSFORTHEPREPARATIONMAYLEADTOMOREREPRODUCIBLERESULTSINTHISCASE,METHODASHALLBEAPPLIED5SAMPLEPREPARATIONTHESAMPLINGSHALLBEPERFORMEDINACCORDANCEWITHISO5022ORISO86561WITHREFERENCE,WHEREAPPROPRIATE,TOISO10725ANDISO116482THESAMPLESHALLBEGROUNDTOAPARTICLESIZELESSTHAN63MANDSTOREDAFTERWARDSINASTOPPEREDSAMPLEBOTTLEINADESICCATORTHESAMPLESSHALLBEDRIEDTOCONSTANTMASSAT110CBEFORETHEDETERMINATIONOFFE2/FE3WEIGHPRECISELYTHECORRECTSAMPLEAMOUNTFORTHEDISSOLUTIONNOTETHEDRYINGOFSAMPLESWILLNOTCHANGETHEFE2CONTENTINALMOSTALLREFRACTORYMATERIALSTHEMOISTURECONTENTMIGHTVARYWITHTIME6INTERFERENCESINTERFERENCESINTHEDETERMINATIONOFFE2/FE3CANBECAUSEDBYOTHERPOLYVALENTIONS,EGAS5/AS3,SB5/SB3,ETCTHEFORMATIONOFANINSOLUBLEPRECIPITATE,EGLEADANDBARIUMSULFATE,MAYALSOINTERFEREINTHEDETERMINATION7SAMPLEDISINTEGRATIONANDMEASUREMENT71METHODA711REAGENTSREAGENTSOFARECOGNIZEDANALYTICALGRADESHALLBEUSEDFORTHISANALYSIS7111WATER,ACCORDINGTOISO3696,ATLEASTOFGRADE27112SULFURICACID,H2SO4,1,84G/CM37113SULFURICACID11COPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011EISO2011ALLRIGHTSRESERVED37114HYDROFLUORICACID,HF,1,13G/CM37115HYDROFLUORICACID,WITHOUTREDUCINGAGENTSTRANSFER50MLOFHYDROFLUORICACID7114INTOAPLATINUMDISHADDONEDROPOF0,02MOL/LKMNO471115SOLUTIONHEATONASTEAMBATHUNTILTHEPERMANGANATEISREDUCEDCOOLFORUSEANDSTOREINAPOLYETHYLENEBOTTLE7116BORICACIDSOLUTIONADD90GOFBORICACIDH3BO3TO1800MLOFWATER7117HYDROXYLAMMONIUMCHLORIDE,NH2OHHCL100G/L71181,10PHENANTHROLINESOLUTION5G/L7119AMMONIUMACETATE,CH3COONH4APPROXIMATELY50BYMASSDISSOLVE50GOFAMMONIUMACETATEIN50MLOFWATER71110AMMONIUMIRONIISULFATEHEXAHYDRATE,FENH42SO426H2O711101IRONSTOCKSOLUTION1ML1MGFEWEIGH3,5108GOFAMMONIUMIRONIISULFATEHEXAHYDRATEFENH42SO426H2O71110ANDTRANSFERTOA500MLVOLUMETRICFLASKDISSOLVEINWATER,ADD8MLTO10MLOFHYDROCHLORICACID1,19G/CM3,DILUTETOVOLUMEANDMIX711102IRONSTANDARDSOLUTION1ML0,01MGFEDILUTE10MLOFTHEIRONSTOCKSOLUTIONTO1000MLINAVOLUMETRICFLASKWITHDEIONIZEDWATER71111NITROGENGAS,WHITESPOTHIGHQUALITYTHEGASCYLINDERSHOULDBEPROVIDEDWITHATWOSTAGEREDUCINGVALVEANDAGASFLOWREGULATORFORAFLOWRATEOF28L/HTO280L/H71112HYDROCHLORICACID,HCL,1,19G/CM371113HYDROCHLORICACID1471114HYDROCHLORICACID11271115POTASSIUMPERMANGANATESOLUTION,KMNO4,0,02MOL/L3,16064G/L712APPARATUSFORSOLUTIONSTHATDONOTCONTAINHYDROFLUORICACID,ORDINARYLABORATORYAPPARATUSANDTHEUSUALLABORATORYGLASSWAREMADEFROMBOROSILICATEGLASSANDCOMPLYINGWITHTHEREQUIREMENTSOFRELEVANTINTERNATIONALSTANDARDSSHALLBEUSEDFORSOLUTIONSCONTAININGHYDROFLUORICACIDORANYACIDICFLUORIDE,PLASTICAPPARATUSSHALLBEUSEDGRADUATEDPLASTICGRADUATEDFLASKSSHALLBEUSEDFORSAMPLESTOCKSOLUTIONSANDCALIBRATIONSTANDARDS,ETCBEAKERS,STORINGBOTTLES,VOLUMETRICFLASKSANDPIPETTESSHALLBEPREPAREDBYFILLINGTHEMTO90OFTHEOVERFLOWCAPACITYWITHHYDROCHLORICACID71114OVERNIGHTAFTERTHESOAKING,THEYSHALLBEWASHEDTHOROUGHLYWITHWATERCOPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011E4ISO2011ALLRIGHTSRESERVED7121ANALYTICALBALANCE,CAPABLEOFREADINGTOTHENEAREST0,1MG7122VOLUMETRICFLASKS,COMPLYINGWITHTHEREQUIREMENTSOFCLASSAINISO10427123PIPETTES,OFSUITABLECAPACITIESCOMPLYINGWITHTHEREQUIREMENTSOFCLASSAINISO6487124MAGNETICSTIRRER7125MOLECULARABSORPTIONSPECTROMETER,CONFORMINGTOTHEREQUIREMENTSOFISO62867126OPTICALCELLS,ASRECOMMENDEDBYTHESPECTROMETERMANUFACTURER7127HOTPLATE7128REACTIONVESSELPLASTICORPOLYTETRAFLUOROETHYLENEPTFEBOTTLEORBEAKEROF250MLCAPACITYTHEVESSELWILLBEUSEDTOEXCLUDEAIROXYGENWHENREACTINGTHESAMPLEWITHTHEREAGENTSTHEVESSELCANBEFITTEDWITHARUBBERSTOPPER,ASSHOWNINFIGURE1,ORTHEVESSELCANBEABEAKERWITHTHELIPREMOVEDANDTHEBOTTOMOFANOTHERCONTAINERPLACEDONTOP,WITHTHEAPPROPRIATEOPENINGSFORINTRODUCTIONOFPURGEGAS,REAGENTS,ANDVENTTUBINGINORDERTOEXCLUDELIGHT,THEVESSELSHALLBECOVEREDWITHBLACKPAINTONTHESURFACETHEVESSELCOMPRISESTHECOMPONENTSDESCRIBEDIN71281TO7128571281PLASTICORTFEFLUOROCARBONBOTTLEORBEAKER,OF250MLCAPACITY71282PLASTICTUBE,USEDTOINTRODUCETHEPURGEGASINTOTHEVESSELITISADVISABLETOUSEACONNECTIONBETWEENTHEPLASTICT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GRADESHALLBEUSEDFORTHISANALYSIS7211WATER,ACCORDINGTOISO3696,OFATLEASTGRADE37212IRONPARENTSOLUTION,FE1000MG/LPARENTSOLUTIONOFTHECOMMERCIALLYAVAILABLEELEMENTWITH1000MG/LFE7213IRONREFERENCESOLUTION,FE100MG/L10MLOFTHEPARENTSOLUTION7212ISTRANSFERREDTOA100MLVOLUMETRICFLASKWHICHISFILLEDUPTOTHEMARKWITHWATER721172141,10PHENANTHROLINE,C12H8N1272151,10PHENANTHROLINESOLUTION,C12H8N1240G/L2GOF1,10PHENANTHROLINE7214AREWEIGHEDINTOABEAKERANDDILUTEDWITHAPPROXIMATELY30MLOFWATER7211THESOLUTIONSHALLBETRANSFERREDINTOA50MLVOLUMETRICFLASKANDFILLEDUPTOTHEMARKWITHWATERTHESOLUTIONMAYBEUSEDFORABOUT4WEEKS7216SODIUMHYDROXIDE,NAOH7217SODIUMHYDROXIDESOLUTION,CNAOH5MOL/L200GOFSODIUMHYDROXIDE7216AREWEIGHEDINTOABEAKERANDDILUTEDWITHAPPROXIMATELY800MLOFWATER7211THESOLUTIONSHALLBETRANSFERREDINTOA1000MLPLASTICVOLUMETRICFLASKANDFILLEDUPTOTHEMARKWITHWATER7218NITRILOTRIACETICACID,NC6H9O637219NITRILOTRIACETICACIDSOLUTION,NC6H9O6340G/L2GOFNITRILOTRIACETICACID7218AREWEIGHEDINTOABEAKERANDDILUTEDWITH4MLOFSODIUMHYDROXIDESOLUTION7217ANDTHEN20MLOFWATER7211ISADDEDTHESOLUTIONSHALLBETRANSFERREDINTOA50MLVOLUMETRICFLASKANDFILLEDUPTOTHEMARKWITHWATERTHESOLUTIONSHALLBEMIXEDWELL72110BORICACID,H3BO372111BORICACIDSOLUTION,H3BO340G/L40GOFBORICACID72110AREWEIGHEDINTOA1LBEAKERANDDILUTEDWITHAPPROXIMATELY600MLOFWATER7211THESOLUTIONISWARMEDSLOWLYONAHEATINGPLATEUNTILALLTHECRYSTALSAREDISSOLVEDONCETHESOLUTIONHASCOOLEDBACKTOROOMTEMPERATURE,ITSHALLBETRANSFERREDINTOA1000MLVOLUMETRICFLASKANDFILLEDUPTOTHEMARKWITHWATERTHESOLUTIONMAYBEUSEDFORABOUT6MONTHS72112SULFURICACID,C1/2H2SO420MOL/L72113HYDROFLUORICACID,WHF401,13G/ML72114DECOMPOSITIONSOLUTION25MLOFSULFURICACID72112AND25MLOFHYDROFLUORICACID72113AREPOUREDCAREFULLYINTOAPLASTICBOTTLEITISCLOSEDTHOROUGHLYANDSHAKEN72115ASCORBICACID,C6H8O6COPYRIGHTINTERNATIONALORGANIZATIONFORSTANDARDIZATIONPROVIDEDBYIHSUNDERLICENSEWITHISONOTFORRESALENOREPRODUCTIONORNETWORKINGPERMITTEDWITHOUTLICENSEFROMIHS,ISO147192011E8ISO2011ALLRIGHTSRESERVED722APPARATUSAPPARATUSASDESCRIBEDIN712,TOGETHERWITHTHEFOLLOWINGELEMENTS7221POLYSTYRENETESTTUBES7222SPECTRALABSORPTIONSPECTROMETER7223POLYSTYRENECUVETTES,WITH10MMLAYERTHICKNESS,TOBESEALED723SAMPLEDISINTEGRATIONANDMEASUREMENT7231GENERALTHEDETERMINATIONISPERFORMEDINTWOSTEPSINTHEFIRSTSTEP,THEMASSCONTENTOFFE2ISDETERMINEDINTHESECONDSTEP,FE3ISREDUCEDTOFE2THEMASSCONTENTOFTHEFE2FORMEDISDETERMINEDLIKEWISETHEGLASSANDPOLYSTYRENECONTAINERS,ASWELLASTHEPIPETTES,SHALLBECLEANEDDIRECTLYBEFOREUSEWITHDILUTEDNITRICACIDAFTERWARDSTHEYSHALLBERINSEDTHOROUGHLYWITHWATER7232SAMPLEDECOMPOSITIONFORTHEDETERMINATIONOFIRONSPECIESPOLYSTYRENETESTTUBESSHOULDBEPROVIDEDINATESTTUBERACKFOREACHDETERMINATION,ONETESTTUBESHALLBETAKENTAKEANOTHERSIXTESTTUBESFORTHEPREPARATIONOFTHESTANDARDSOLUTIONSWEIGH20MGTO30MGOFTHESAMPLE,GROUNDACCORDINGTOCLAUSE5,INTOAPOLYSTYRENETESTTUBEMOIST
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