1、InternationalStandardISO12219-11Firstedition2025-05Interiorairofroadvehicles一Part11:Thermaldesorptionanalysisoforganicemissionsforthecharacterizationonnon-metallicmaterialsforvehiclesAirInterieurdesvehiculesroutiersPartie11:AnalysepardesorptionthermiquedesemissionsorganiquespourlaCaracterisationdesm
2、ateriauxnonmetalliquesReferencenumberISO12219-ll:2025(en)COPYRIGHTPROTECTEDDOCUMENTISO2025Allrightsreserved.Unlessotherwisespecified,orrequiredinthecontextofitsimplementation,nopartofthispublicationmaybereproducedorutilizedotherwiseinanyformorbyanymeans,electronicormechanical,includingphotocopying,o
3、rpostingontheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbeloworISO,smemberbodyinthecountryoftherequester.ISOcopyrightofficeCP401Ch.deBlandonnet8CH-1214Vernier,GenevaPhone:+4122749Ol11Email:copyrightiso.orgWebsite:www.iso.orgPublishedinSwitzerl
4、andContentsPageForewordv1 Scope12 Normativereferences13 Termsanddefinitions14 Abbreviatedterms25 Samplingandstorage36 Apparatusandperformancecharacteristics36.1 Apparatus36.2 Performancecharacteristics37 Analysis47.1 Generalinformationonthermaldesorptionanalysis47.2 Cleaningofthedesorptiontubes57.3
5、Systemchecks57.3.1 General57.3.2 Checkstandardsolution67.4 Calibration77.4.1 General77.4.2 Calibrationsolutions77.4.3 Injectionofthecalibrationorcheckstandard77.4.4 TenaxTAdesorptiontube77.5 Sampleanalysisprocess77.5.1 Photographicdocumentationofthesamples77.5.2 Trimmingandweighingofthesamples77.5.3
6、 Calibrationrun,determinationofcalibrationfactors(responsefactor)87.6 Chromatographicevaluation87.6.1 General87.6.2 Integrationlimitsrelevantforquantification97.6.3 Peakintegration97.6.4 Evaluationforriderpeaksand“oil-hi11s”97.6.5 Calculationofemissions107.6.6 Qualitativeanalysis107.6.7 Reportingoft
7、heanalyticalresults118 Validationparameters128.1 Typicalmeasuredvaluevariationforrealsamples128.2 Quantificationlimitorlinearityoftoluene138.3 Variationandrecoveryoftoluene149 Knownproblemsandpossiblesourcesoferrors149.1 Samplepreparation149.2 Difficultsampleswithnon-uniformsurface149.3 Sampleswithh
8、igherwatercontent149.4 Lowerresultswhendesorptionstreamistoolow159.4.1 General159.4.2 Differencesbetweensampletubesmadeofmetalandglass159.5 Overorunderresultsduetodeviationsinthethermaldesorptiontemperature159.6 Dangerofconfusionduringtheidentificationofthesubstance169.7 Exceedingthedetectorlinearit
9、yinthecaseofhighemissionvalues17Annex A (informative)Materialspecifictestportions18Annex B (informative)Productionofpaintfilmsforthermaldesorption20AnnexC(informative)Examplesforsuitabletestequipment,testparametersandpossibleerrors22AnnexD(informative)Preparationofstandardsolutions32Bibliography33Fo
10、rewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherig
11、httoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmentabinliaisonwithIS0,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.Theproceduresusedtodevelopthisdocumentandthoseinten
12、dedforitsfurthermaintenancearedescribedintheISO/IECDirectives,Part1.Inparticular,thedifferentapprovalcriterianeededforthedifferenttypesofISOdocumentshouldbenoted.ThisdocumentwasdraftedinaccordancewiththeeditorialrulesoftheISO/IECDirectives,Part2(seewww.iso.org/directives).ISOdrawsattentiontothepossi
13、bilitythattheimplementationofthisdocumentmayinvolvetheuseof（八）patent(三).ISOtakesnopositionconcerningtheevidence,validityorapplicabilityofanyclaimedpatentrightsinrespectthereof.Asofthedateofpublicationofthisdocument,ISOhadnotreceivednoticeof（八）patent(三)whichmayberequiredtoimplementthisdocument.Howeve
14、r,implementersarecautionedthatthismaynotrepresentthelatestinformation,whichmaybeobtainedfromthepatentdatabaseavailableatwww.iso.org/patents.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.Anytradenameusedinthisdocumentisinformationgivenfortheconvenienceofusersanddoesnotconstitutea
15、nendorsement.Foranexplanationofthevoluntarynatureofstandards,themeaningofISOspecifictermsandexpressionsrelatedtoconformityassessment,aswellasinformationaboutISOsadherencetotheWorldTradeOrganization(WTo)principlesintheTechnicalBarrierstoTrade(TBT),seeWWW.isoQrgisoforeword.htmLThisdocumentwaspreparedb
16、yTechnicalCommitteeISO/TC146,Airquality,SubcommitteeSC6,Indoorair.AlistofallpartsintheISO12219seriescanbefoundontheISOwebsite.Anyfeedbackorquestionsonthisdocumentshouldbedirectedtotheusersnationalstandardsbody.Acompletelistingofthesebodiescanbefoundatwww.iso.org/membnrs.htmLInteriorairofroadvehicles
17、一Part11:Thermaldesorptionanalysisoforganicemissionsforthecharacterizationonnon-metallicmaterialsforvehicles1 ScopeThisdocumentdescribesananalyticalmethodtodeterminetheemissionsfromnon-metallicmaterialsusedformouldedpartsinmotorvehicles,suchastextiles,carpets,adhesives,sealingcompounds,forms,leather,
18、plasticparts,filmsandsheets,paintsormaterialcombinations.Thematerialsarecharacterizedintermsofthetypeandquantityoforganicsubstancesthatcanbeoutgassedfromthem.Forthispurpose,twoSemiquantitativesumvaluesaredetermined,whichallowanestimationoftheemissionsofvolatileorganiccompounds(VOCvalue)andtheproport
19、ionofcondensablesubstanceslowvolatile“foggingcompound(FOG)value.Furthermore,individualsubstancesoftheemissionaredetermined.Duringtheanalysis,thesamplesarethermallyextracted,theemissionsareseparatedbygaschromatographyanddetectedbymassspectrometry.Thetestmethodpresentedinthisdocumentprovidesvaluesthat
20、arevalidonlyforconditionsdescribedinthisdocument.Theresultswhichcanbeachievedusingthismethodarenotappropriateformakingfurtherestimationsofanykindofthehealtheffectsofemittedsubstancesnorshouldtheybeusedmightthatcanbefoundintheinteriorofacompletevehicleinstationarycondition,whiledrivingorinconditionss
21、imilartodriving.2 NormativereferencesThefollowingdocumentsarereferredtointhetextinsuchawaythatsomeoralloftheircontentconstitutesrequirementsofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionofthereferenceddocument(includinganyamendments)applies.ISO1600
22、0-6,Indoorair-Part6:Determinationoforganiccompounds(VVOC,VOC,SVOCJinindoorandtestchamberairbyactivesamplingonsorbenttubes,thermaldesorptionandgaschromatographyusingMSorMSFID3 TermsanddefinitionsForthepurposesofthisdocument,thefollowingtermsanddefinitionsapply.ISOandIECmaintainterminologydatabasesfor
23、useinstandardizationatthefollowingaddresses:一ISOOnlinebrowsingplatform:availableathttps:WWW.iso.org/obp一IECElectropedia:availableathttps:WWW.electropedia.org/3.1volatileorganiccompoundvalueVOCvaluetotalvolatileorganiccompoundvaluetotalofthereadilyvolatiletomediumvolatilesubstancesNote1toentry:TheVOC
24、valueiscalculatedasatolueneequivalent.Themethoddescribedinthisdocumentallowssubstancesintheboiling/elutionrangefromthebeginningofthechromatogramupton-Pentacosane(C25)tobedeterminedandanalysed.Note2toentry:ItisknownthattheretentionareabetweenClandC6cannotbecompletelyquantified.Note3toentry:Itcanbeass
25、umedthatthesesubstancescanbedetectedwhenanalysingtheairofthevehicleinterior.Fortheanalysis,thesample(3.4)isheatedat90for30min.TheVOCvalueisdeterminedbytwomeasurements.Thehighervalueofthemeasurementsisindicatedastheresult.3.2lowvolatile“foggingcompoundvalueFOGvaluetotalofsubstanceswithlowvolatilitywh
26、ichelutefromtheretentiontimeofn-tetradecane(inclusive)Note1toentry:Itiscalculatedashexadecaneequivalent.Substancesintheboilingrangeofn-alkanesC14toC32aredeterminedandanalysed.3.3retentionindexindexcalculatedwithaseriesofn-alkanesSOURCE:Reference63.4samplepartorpieceofaproductthatisrepresentativeofth
27、eproductionSOURCE:ISO12219-4:2013,3.153.5specimenarticlepreparedfromasample(3.4)SOURCE:ISO15906:2007,3.24 AbbreviatedtermsCIconfidenceintervalEIelectronimpactFIDflameionizationdetectorFOGlowvolatilefoggingcompoundsSemi-volatileorganiccompoundspronetocondensationonvehicleinteriorsurfacescausingToggin
28、g,ofthewindscreenandotherwindows/)GCgaschromatographMSDmass-selectivedetectorPESpolyesterfilmTDthermaldesorptionTICtotalionchromatogramTPOthermoplasticpolyolefinfoilVOCvolatileorganiccompound5 SamplingandstorageForsamplingandstorageofthesamples,theconditionsofISO12219-8:2018,Clauses8and10shouldbemet
29、6 Apparatusandperformancecharacteristics6.1 ApparatusThefollowinglaboratoryequipmentisneeded:一directlycoupledthermaldesorption/gaschromatographysystem;一GC(electroniccontrolofpneumaticsisrecommended;suitableinstrumentsarelistedinAnnexC):一afocusingdevicecomprisingacryofocusingorcold-trappingmechanism
30、whichcanbeheatedsufficientlyquicklytoreleasecompoundsofinterestandinjectthemintothecapillaryGCcolumnwithoutdispersion;MSD;emptydesorptiontubeswithinertsurface,internaldiameter4mmto5mm;一afusedsilicaGCcapillarycolumnof5%phenyl-methyl-siloxaneisselected;bondedcolumnsof30mto60m,internaldiameter0,25mmto
31、0,32mmandphasethickness0,25mto0,52mareexamplesofcolumnsproventobesuitableforVOCandFOGanalyses;一softwareforequipmentcontrol;一softwareforanalysisofchromatograms.6.2PerformancecharacteristicsThefollowingrecommendationsregardingtheperformanceshallbeconsidered:一Therecoveryratesofthesinglesubstances(calcu
32、latedastolueneequivalent)ofthecheckstandardsolutiondescribein731ShoUldbebetween60%and140%underVOCconditions,wherebytherecoveryofthetolueneshouldbeatleast80%andnomorethan120%.Itshouldbepossibletofallbelowthefollowingdetectionlimits(seeDIN32645,95%confidenceinterval):一IntheVOCruntoluene0,04g,andicosan
33、e(C20)0,06g.一IntheFOGrunn-alkaneC320,2g.一TenaxTAdesorptiontubes:Withregardtothedensityandamountonthepacking,refertotherecommendationoftheequipmentmanufacturers.Inparticular,careshouldbetakentoensurethattheTenaxTApackingfillsthetubesothatitcanbecoveredcompletelybytheheatedzoneoftheTDinstrumentstubehe
34、ater.ThetubesshouldbefilledwithasufficientamountofTenaxTAsothatnosubstancebreakthroughcanoccurduringsamplefeed.Furthermanufacturer-specificinformationisdescribedinformativelyintheClaUSeC.3.一Thisdocumentonlyusessorbenttubesforintroducingstandardstotheanalyticalsystem.Forthedeterminationofthedetection
35、limits,differentamountsofthetestsubstancesdissolvedinmethanol(forVOCrun)andn-pentane(forFOG)shouldbeinjectedintodesorptiontubes2)TenaxTAisthetradenameofaproductsuppliedbyBuchem.ThisinformationisgivenfortheconvenienceofusersofthisdocumentanddoesnotconstituteanendorsementbyISOoftheproductnamed.Equival
36、entproductsmaybeusediftheycanbeshowntoleadtothesameresults.ISO2025-Allrightsreserved3filledwithTenaxTAanddesorbedat280.ThesplitcharacteristicsandGCconditionsshouldconformtotheVOC/FOGmethodparameters.一Parametersforgaschromatographyforcalibrationandcontrolanalysis(examplesaregiveninTableC.l):一Fortolue
37、necalibrationandtheanalysisofthecontrolmix,thesameparametersshouldbesetasfortheVOCsamplerun(forretentiontimesofthecontrolmix,seeTableB.l).Theonlydifferenceisalaterstartofthedataloggingtomaskoutthemethanolpeak.HexadecanecalibrationiscarriedoutundertheGCconditionsoftheFOGanalysis.Theonlydifferenceisal
38、aterstartofthedataloggingtomaskoutthepentanepeak.一Comparedtothesampleruns,theGCrunscanbeshortenedbyabandoningtheoventemperatureprogramafterelutionofthecalibrationsubstances.7Analysis7.1 GeneralinformationonthermaldesorptionanalysisInaTDanalysis,smallamountsofthematerialareheatedinanemptythermaldesor
39、ptiontubeinadefinedprocess.ThevolatilesubstancesemittedduringthisprocessarecarriedbymeansofaGCcarriergastothefocusingtrapwithprogrammabletemperature.AschemeoftheprocessisgiveninFigure1.Followingtheheatingphase,thefocusingtrapisheatedupquicklyto280.Thefocusedsubstancesaredesorbedduringthisprocess.The
40、yaresplitduringtransfertothegas-chromatographicseparationcolumnandaredetectedbymassspectrometry.CalibrationwithreferencesubstancesallowsforaSemiquantitativeestimationtobecarriedout,expressedasgg.ToluenefortheVOCanalysisandn-hexadecanefortheFOGvalueareusedasquantitativereferencesubstances.Usingmasssp
41、ectraandretentionindices,thesubstancescanbeidentified.CarrierjasaVOC:30minat90oC.bFOG:60minat120.Figure1Principleofthermaldesorption7.2 CleaningofthedesorptiontubesAlldesorptiontubesusedshouldbecompletelyfreeofcontamination.Newtubesshouldalsobecleanedcarefullybeforeinitialusebymeansofanappropriateme
42、thod.Thefollowingprocedureisrecommendedforglasstubes.一Cleantheglasstubesbystoringtheminanalkalinecleaningsolutionforseveralhours,preferablyovernight.Then,rinsethoroughly,firstunderrunninghotwaterforatleastoneminuteandsubsequentlywithdeionizedwater.一Drythetubesinadryingovenforapproximately45minat105a
43、ndstoreinamannerthatisfreefromcontamination(e.g.wrappedairtightinaluminiumfoil)untilused.7.3 Systemchecks7.3.1 GeneralTheperformanceoftheequipmentsystemshouldbecheckedduringthesampleseriesbyanalysingaperformancecheckstandardsolution(see7.3.1).Thecheckstandardsolutionshouldcontainnon-polar,polaralkal
44、ineandacidiccomponentswhichwoulddemonstrateanoticeablepeaktailingintheeventofundesiredadsorptioneffects.Peaksinclosesuccessionsuchaso-xyleneandn-nonaneareusedforcheckingtheseparationperformanceofthechromatographycolumn.Underthechromatographicconditionschosen,thesetwosubstancepeaksshallbealmostbaseli
45、neseparated.Checkstandardsarealsousefultomonitorthedriftintheinstrumentresponseovertime.Allsubstancescontainedinthischeckstandardshouldbeuniquelyidentifiedduringthesearchinthemassspectraldatabase.Theperformanceofthemass-selectivedetectoristobeensuredbymassandsensitivitytuning,duringwhichthemanufactu
46、rersspecificationsshouldbeachieved.Inaddition,anair/watercheckshouldbeperformedtochecktheoverallsystemforleakages.TheTDGCsystemshouldalsobecheckedformemoryeffectsbyatleastcarryingoutablankrunwithanemptydesorptiontubebeforeeachsampleseries.Ifnegativeeffects(suchasstrongpeaktailing,interferingblankrun
47、peaksorsignificantlossofanalytes)occur,thesystemshouldbecleaned.Ifappropriate,theGCcolumn,glassline,transferlineorseals,forexample,shouldbereplaced.Thedocumentationoftheresultsofthecontrolrunsforeachsampleserieswithintheframeworkofqualitycontrolisrecommended(controlchart).Thefollowingparametersareex
48、amplesofexpedientcontrolvariables:一peakareacharacteristicsofthecheckstandardsubstances;calculationofconcentrationsofcheckstandardsubstancesastolueneequivalents;一retentiontimes.7.3.2 CheckstandardsolutionThesubstanceslistedinTabISLdissolvedinmethanolhaveprovedsuitableforcheckingthesystem(listedinelutionsequenceunderVOCcondition).Table1Checkstandard
