1、ISOInternationalStandardISO19396-2Secondedition2025-06Paintsandvarnishes一DeterminationofpHvalue一Part2:pHsensorswithISFETtechnologyPeinturesetvernisDeterminationdeIavaleurdepHPartie2:SondesdepHdoteesdeIatechnologieISFETReferencenumberISO19396-2:2025(en)COPYRIGHTPROTECTEDDOCUMENTISO2025Allrightsreserv
2、ed.Unlessotherwisespecified,orrequiredinthecontextofitsimplementation,nopartofthispublicationmaybereproducedorutilizedotherwiseinanyformorbyanymeans,electronicormechanical,includingphotocopying,orpostingontheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOatth
3、eaddressbeloworISO,smemberbodyinthecountryoftherequester.ISOcopyrightofficeCP401Ch.deBlandonnet8CH-1214Vernier,GenevaPhone:+41227490111Email:copyrightiso.orgWebsite:www.iso.orgPublishedinSwitzerlandContentsPageForewordivIntroductionv1 Scope12 Normativereferences13 Termsanddefinitions14 Principle45 A
4、pparatusandmaterials45.1 pHmeasuringapparatus45.2 pHmeter45.3 ISFETsensor55.4 Buffersolutions66 Sampling67 Procedure77.1 Testconditions77.2 Calibration77.3 Numberofdeterminations77.4 MeasuringthepHvalue78 Evaluation79 Precision89.1 General89.2 Repeatabilitylimit,r89.3 Reproducibilitylimit,R810 Testr
5、eport8AnnexA(informative)Determinationofprecision9Bibliography11ForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterest
6、edinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnical
7、standardization.TheproceduresusedtodevelopthisdocumentandthoseintendedforitsfurthermaintenancearedescribedintheISO/IECDirectives,Part1.Inparticular,thedifferentapprovalcriterianeededforthedifferenttypesofISOdocumentshouldbenoted.ThisdocumentwasdraftedinaccordancewiththeeditorialrulesoftheISO/IECDire
8、ctives,Part2(seeWWW.iso.org/directives).ISOdrawsattentiontothepossibilitythattheimplementationofthisdocumentmayinvolvetheuseof（八）patent(三).ISOtakesnopositionconcerningtheevidence,validityorapplicabilityofanyclaimedpatentrightsinrespectthereof.Asofthedateofpublicationofthisdocument,ISOhadnotreceivedn
9、oticeof（八）patent(三)whichmayberequiredtoimplementthisdocument.HoweverlImplementersarecautionedthatthismaynotrepresentthelatestinformation,whichmaybeobtainedfromthepatentdatabaseavailableatWWW.iso.org/patents.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.Anytradenameusedinthisdocu
10、mentisinformationgivenfortheconvenienceofusersanddoesnotconstituteanendorsement.Foranexplanationofthevoluntarynatureofstandards,themeaningofISOspecifictermsandexpressionsrelatedtoconformityassessment,aswellasinformationaboutISOsadherencetotheWorldTradeOrganization(WTO)principlesintheTechnicalBarrier
11、stoTrade(TBT),seeWWW.iso.org/iso/foreword.htmLThisdocumentwaspreparedbyTechnicalCommitteeISO/TC35,Paintsandvarnishes,SubcommitteeSC9,Generaltestmethodsforpaintsandvarnishes,incollaborationwiththeEuropeanCommitteeforStandardization(CEN)TechnicalCommitteeCEN/TC139,Paintsandvarnishes,inaccordancewithth
12、eAgreementontechnicalcooperationbetweenISOandCEN(ViennaAgreement).Thissecondeditioncancelsandreplacesthefirstedition(ISO19396-2:2017),whichhasbeentechnicallyrevised.Themainchangesareasfollows: definitionsforntheoreticalslopeandstabilityofmeasuredvalue“havebeendeleted; theterm,ISFETelectrode11hasbeen
13、changedtor,ISFETsensorintheentiretextincludingthetitleofthedocument; thecalibrationf7.2hasbeenclarified; thenormativereferenceshavebeenupdated.AlistofallpartsintheISO19396seriescanbefoundontheISOwebsite.Anyfeedbackorquestionsonthisdocumentshouldbedirectedtotheusersnationalstandardsbody.Acompletelist
14、ingofthesebodiescanbefoundatWWW.iso.org/membnrs.htmLIntroductionThepHvalueofaqueousproductsisofdecisiveimportancefortheproductpropertiesanddurability.ISO19396-1specifiesamethodformeasuringthepHvalueusingpHsensorswithaglassmembrane.ThisdocumentcoversamethodformeasuringthepHvalueofdispersionsandcoatin
15、gmaterialsusingpHsensorswithion-sensitivefield-effecttransistor(ISFET)technology.PaintsandvarnishesDeterminationofpHvalue一Part2:pHsensorswithISFETtechnology1 ScopeThisdocumentspecifiesamethodformeasuringthepHvalueofdispersionsandcoatingmaterialsusingpHsensorswithion-sensitivefield-effecttransistor(I
16、SFET)technology.2 NormativereferencesThefollowingdocumentsarereferredtointhetextinsuchawaythatsomeoralloftheircontentconstitutesrequirementsofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionofthereferenceddocument(includinganyamendments)applies.ISO1513
17、PaintsandvarnishesExaminationandpreparationOftestsampIesISO4618,PaintsandvarnishesVocabularyISO15528,Paints,varnishesandrawmaterialsforpaintsandvarnishesSamplingISO80000-9,QuantitiesandunitsPart9:Physicalchemistryandmolecularphysics3 TermsanddefinitionsForthepurposesofthisdocument,thetermsanddefini
18、tionsgiveninISO4618,ISO80000-9andthefollowingapply.ISOandIECmaintainterminologydatabasesforuseinstandardizationatthefollowingaddresses: ISOOnlinebrowsingplatform:availableathttps:/www.iso.org/ObP IECElectropedia:availableathttps:WWW.electropedia.org/3.1PHmeasurefortheacidicorbasicreactionofanaqueous
19、solutionorpolymerdispersionNote1toentry:ForthenotationOfPH,thePandtheHareverticallyononeline.ThesameisvalidforpOH.Note2toentry:Theacidicreactionisdeterminedbytheactivityoftheexisting11hydrogenions”.Thebasicreactionisdeterminedbytheactivityoftheexistinghydroxideions.Thedirectrelationshipbetweentheact
20、ivitiesofthe“hydrogenionsandthehydroxideionsisdescribedbytheionicproductofthewater.SOURCE:ISO19396-1:2025,3.13.2pHvaluedecadallogarithmofthehydrogenionactivitymultipliedwith(-1)Qp=%+7h+wherea+istheactivityofthehydrogenion,inmol/kg;m0isthestandardmolality(1molkg);h+istheactivitycoefficientofthehydrog
21、enion;isthemolalityofthehydrogenion,inmolkg.Note1toentry:ForfurtherdetailsseeDIN19261.SOURCE:ISO19396-1:2025,3,23.3ISFETsensorion-sensitivefield-effecttransistorsensorcombinedpHsensorwithISFETtechnologypotentiometriccellprovidingavoltagewhichdependsonthepHvalue(3.2)ofthemeasuringmediumNote1toentry:T
22、hetwoelectrochemicalcellsaretheion-sensitivefield-effecttransistor(ISFET)(3.5)andthereferenceelectrode(3.4).1 referenceelectrode,consistingof2,3and42 referenceelement3 referenceelectrolyte4 diaphragm5 pHmeasuringsensor,consistingof6and76 ISFET(seeFigure4)7 openingtothemeasuringmediumgate8 temperatur
23、esensorUpHproportionalvoltageUDSvoltagereceiver/sender(drain/source)7dscurrentreceiver/sender(drain/source)Figure1DesignofanISFETsensor(schematicdiagram)3.4referenceelectrodeelectrodeprovidingaconstantpotentialWhichisindependentfromXhepHvalue(3.2)ofthemeasuringmediumNote1toentry:Atthetimeofpublicati
24、onofthisdocument,themostcommonlyusedtypeisthesilver/silverchloridereferenceelectrode,whosepotentialisstabilizedbyaconstantconcentrationofpotassiumchloride(KCl)inthereferenceelectrolyte.Thereferenceelectrolyteisincontactwiththemeasuringmediumviaadiaphragm.SOURCE:ISO19396-1:2025,3.4,modified-thelastse
25、ntenceinNote1toentryhasbeenadded.3.5ISFETion-sensitivefield-effecttransistormeasuringelectrodeelectrodeprovidingapHproportionalsignalwithasuitableelectroniccircuit3.6temperaturecompensationmathematicalcorrectionofthetemperatureinfluenceonthemeasuringsignalNote1toentry:Bythis,thetemperaturedependency
26、ofthepHvaluef3.2jofthemeasuringmediumcannotbecompensated.Therefore,thetemperatureisalwaysrecordedtogetherwiththepHvalue.SOURCE:ISO19396-1:2025,3,93.7practicalslopek,slopeofapHsensor(3.3),whichisobtainedbymeasuringthepHproportionalvoltagesofthepHsensorinatleasttworeferencebuffersolutions(3.9)-NU=pHNo
27、te1toentry:TheslopeobtainedduringcalibrationisacharacteristicforthequalityofthepHsensor.Note2toentry:Forfurtherdefinitionson“slopeandzeropointseeDIN19261.SOURCE:ISO19396-1:2025,3.103.8zeropointPhopHvalue(3.2)ofapHsensor(3.3),forwhichthepHproportionalvoltageofthepHsensorisU=0mVatagiventemperatureNote
28、1toentry:Thezeropointfortheion-sensitivefield-effecttransistor(ISFETjsensor(3.3)issetbycalibratingtheoffsetvoltageaccordingtotheinstructionsofthemanufacturer.SOURCE:ISO19396-1:2025,3.11,modifiedNote1toentryhasbeenreplaced,Note2toentryhasbeendeleted.3.9buffersolutionsolutionwithapHvalue(3.2)ofknownme
29、asurementuncertaintyNote1toentry:ThebuffersolutionisusedforcalibrationandadjustmentofpHmeters.BuffersolutionshaveapHvaluethatislargelynon-sensitivetodilutionandacidorbasicaddition.SOURCE:ISO19396-1:2025,3.124PrincipleThisdocumentcomprisesthedescriptionoftheISFETsensor,itscalibrationandcleaning,aswel
30、lastheprocedureofpHmeasurement.Thespecifiedmethodandmeasuringconditionsarebasedontheresultsofaninterlaboratorytest(seeAnnexA).5Apparatusandmaterials5.1pHmeasuringapparatusKey1234UseapHmeasuringapparatus(SeeFigure2)forpHmeasurementofpolymerdispersionsandcoatingmaterialsconsistingofapHmetersuitablefor
31、ISFETsensors,anISFETsensor,atleasttwobuffersolutions,containersforthebuffersolutionsandthemediumtobemeasured.TocleantheISFETsensor,aspraybottlewithdeionizedwaterorasuitablecleaningsolutionandasmallbrusharerecommended.Inaddition,itcanbehelpfultouseastand,astirringtool,athermostat,aswellasdatarecordin
32、gandanalysissystems.pHmetercleaningsolution(dependingontheproduct)measuringcontainersISFETsensorwithtemperaturesensorstandbuffersolutionsFigure2ExampleofapHmeasuringapparatus5.2 pHmeterThepHmetershallatleasthavethefollowingfunctions: pHvalue,withreadingaccuracyof0,01; pHproportionalvoltageoftheISFET
33、sensor,withaccuracyofatleast1mV; adjustmentoftheoffsetandindicationofzeropointoroffset; adjustmentofthepracticalslope; indicationofthemeasuringtemperature; temperaturecompensation:manuallyorautomaticallywithconnectedtemperaturesensor(externalorintegratedintheISFETsensor).5.3 ISFETsensorTheISFETandth
34、ereferenceelectrodearecombinedinoneunit(seeFigure3).Anintegratedtemperaturesensorisrecommended.Key1 connectingcable2 bendprotection3 sensorhead4 sensorshaft5 diaphragm6 ISFETFigure3ExampleofanISFETsensorKey1 referenceelectrode2 measuringmedium3 pH-sensitiveoxidefilm4 n-semiconductor5 contacttothemea
35、suringmedium(gate)6 p-semiconductor7 sender(sourceS8 receiver(drainD)9 regulatingcircuit(UDS=const,ds=const.UpHproportionalvoltageFigure4FunctionalprincipleoftheISFETtechnologyAsanexample,anISFETwithnpn-typedopingisillustratedinFigUre4.Insteadofacommonelectriccontactatthegate,thereisanion-sensitivef
36、ilm(usuallymetaloxides,suchasTgQ;Agq),whichisincontactwiththemeasuringmedium.TheactivityoftheH+ionsofthemeasuringmediumprovidesforapotentialonthesurfaceoftheion-sensitivefilm.Usingaregulatingcircuit,currentandvoltageattheISFETareconstantlymaintainedinordertoavoidthenonlinearcharacteristiccurveoftheI
37、SFET.BetweentheISFETandthereferenceelectrode,voltageformswhichisproportionaltothepHvoltageU.5.4BuffersolutionsBuffersolutionswithspecificationsonprecision,durabilityandtemperaturedependencyshallbeused.NOTEBuffersolutionscanchangeduringstorageinclosedandespeciallyinopencontainers.6 SamplingTakearepre
38、sentativesampleoftheproducttobetestedasspecifiedinISO15528.ExamineandpreparethesamplesofcoatingmaterialsasspecifiedinISO1513.Sampling,transportofsamplesandsamplepreparationhaveinfluenceonthepHvalue.7 Procedure7.1 TestconditionsInordertoreducethermalandelectricalhysteresiseffects,ensurethatthetempera
39、turesofthetestsamples,sensor,demineralizedordistilledrinsingwaterandbuffersolutionsareasclosetooneanotheraspossible.Thetemperaturesofthetestsamplesandbuffersolutionsshallnotdifferbymorethan1.Thetemperatureforthedeterminationshallbe(232)(272)incountrieswithtropicalorhotclimates.ThepHvariationoverther
40、angeof20to30isnegligiblecomparedtothesystemmeasurementuncertainty.Inaddition,thetemperaturecompensatorintheinstrumentshouldbesetattheactualtemperature.Thesampletobemeasuredshallbehomogenous.7.2 CalibrationCarryoutatleastatwo-pointcalibration.ThepHvaluesofthebuffersolutionsshouldcloselybracketthemeas
41、uringrangeofthesamples.ThedifferencebetweenthevaluesofthetwobuffersolutionsshallbepH2.Refertothemanufacturers*specificationsoncalibration.NOTEThepHvalueofbasicbuffersolutionschangesrelativelyfast,byabsorbingCO介Omtheairandtherebythemeasurementuncertaintyincreases.AdjustthepHmeterwiththedataoftheISFET
42、sensor(slopeandzeropointoroffset)obtainedduringcalibration.Discardtheusedbuffersolutionsafteruse.7.3 NumberofdeterminationsCarryoutthedeterminationinduplicate.IfthesecondmeasurementdoesnotdeviatebymorethanpH=0,2fromthefirstmeasurement,thedeterminationiscompleted.Ifthetwomeasurementsdeviatebymorethan
43、pH=0,2fromeachother,twonewmeasurementsshallbecarriedout.7.4 MeasuringthepHvalueBeforeusingtheISFETsensor,rinseitwithwater(preferablydeionizedwater).Putthesampleinasuitable,cleananddrycontainer,andimmersetheISFETsensor.Thediaphragmshallbecoveredcompletely.ModeratelymovetheISFETsensorinthesampletobeme
44、asuredpriortomeasuring,soitisuniformlywashedroundwiththesamplematerial.StopmovingtheISFETsensor,waitfor2minanddocumenttheresult.CleantheISFETsensorandcarryoutthesecondmeasurementsubsequently.Aftercompletingthemeasurements,cleantheISFETsensorandstoreitinaccordancewiththemanufacturersspecifications.8
45、EvaluationExpressthemeanvaluefromtheduplicates,roundedtoonedecimalplace,asresult.9 Precision9.1 GeneralFordetailsonthedeterminationofprecision,seeAOneXA.9.2 Repeatabilitylimit,rTherepeatabilitylimit,r,isthevaluebelowwhichtheabsolutedifferencebetweentwotestresults(eachthemeanofthreevaliddetermination
46、s)canbeexpectedtoliewhenthismethodisusedunderrepeatabilityconditions.Inthiscase,thetestresultsareobtainedonidenticalmaterialbyoneoperatorinonelaboratorywithinashortintervaloftimeusingthestandardizedtestmethod.Therepeatabilitylimit,r,accordingtothisdocument,is0,2withagivenprobabilityof95%.9.3 Reprodu
47、cibilitylimit,RThereproducibilitylimit,R,isthevaluebelowwhichtheabsolutedifferencebetweentwosingletestresults(eachthemeanofthreevaliddeterminations)canbeexpectedtoliewhenthismethodisusedunderreproducibilityconditions.Inthiscase,thetestresultshavebeenobtainedonidenticalmaterialbyoperatorsonsucceedingdaysduringshiftoperationusingthestandardizedtestmethod.ThereproducibilityIimitlR,accordingtothisdocument,is0,4withagivenprobabilityof95%.10 TestreportThetestreportshallcontainatleastthefollowinginformation:a) alldetailsnecessarytoidentifytheproductundertest(manufa
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