1、BRITISH STANDARD BS EN 12963:2001 Adhesives Determination of free monomer content in adhesives based on synthetic polymers The European Standard EN 12963:2001 has the status of a British Standard ICS 83.180 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 12963:2001 This B
2、ritish Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 June 2001 BSI 06-2001 ISBN 0 580 37432 7 National foreword This British Standard is the official Eng
3、lish language version of EN 12963:2001. The UK participation in its preparation was entrusted to Technical Committee PRI/52, Adhesives, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Sta
4、ndards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Stand
5、ard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the res
6、ponsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN t
7、itle page, pages 2 to 7 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN12963 April2001 ICS83.180 Englishversion AdhesivesDeterm
8、inationoffreemonomercontentin adhesivesbasedonsyntheticpolymers AdhsifsDterminationdelateneurenmonomreslibres dansdesadhsifsbasedepolymressynthtiques KlebstoffeBestimmungdesfreienMonomeranteilsin KlebstoffenaufderBasissynthetischerPolymere ThisEuropeanStandardwasapprovedbyCENon1March2001. CENmembers
9、areboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. T
10、hisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,C
11、zechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CE
12、N Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN12963:2001EPage2 EN12963:2001 Contents Page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions . 4 4 Principle4 5 Safety4 6 Chemicals.4 7 Apparatus.5 8 Samplingandsamplepreparation. 5 9 Ch
13、romatographicconditions .5 10 Calibrationofthegaschromatograph . .6 11 Procedure .6 12 Expressionofresults 7 13 Testreport 7Page3 EN12963:2001 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC193“Adhesives“,thesecretariatof whichisheldbyAENOR. ThisEuropeanStandardshallbegiventhe
14、statusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2001,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2001. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementt
15、hisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom.Page4 EN12963:2001 1Scope ThisEuropeanStandardspecifiesasimpletestmethodforthegaschromatographicdetermina
16、tionoffree monomercontentinpolymericadhesivesafterspecifictreatment. Thistestmethodcanbeusedforthedeterminationofacrylic,styrene,vinylandotherunsaturatedmonomers. NOTEThismethodcouldalsobeusedforthedeterminationofothermonomers,ifapplicable. 2 Normativereferences ThisEuropeanStandardincorporatesbydat
17、edorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevi
18、sion.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN923 AdhesivesTermsanddefinitions EN1066 AdhesivesSampling EN1067 AdhesivesExaminationandpreparationofsamplesfortesting 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thetermsanddefinitions
19、giveninEN923apply. 4Principle 4.1 Waterborneadhesives Analiquotofanextractofthewaterborneadhesivetobeanalysedisinjectedintoagaschromatographequipped withacapillarycolumnandalineartemperatureprogrammer.ThemonomersaredetectedbyaFlameIonisation Detector(FID).Quantificationismadebypeakareameasurement. 4
20、.2 Solventborneorsolventlessadhesives Analiquotofthesolventborneorsolventlessadhesiveisdilutedwithasuitablesolvent.Thesolventshallbeable toconsiderablyreducetheviscosityoftheadhesivesolutionastoallowittobeinjectedintothegas chromatrograph.Thesolventshallnotinterferewiththemonomerstobedetected.Thedil
21、utedsolutionisanalysed astheextractasdescribedin4.1 5Safety Personsusingthisstandardshallbefamiliarwithnormallaboratorypractice. Thisstandarddoesnotpurporttoaddressallthesafetyproblems,ifany,associatedwithitsuse. Itistheresponsibilityoftheusertoestablishsafetyandhealthpracticesandtoensurecompliancew
22、ithany Europeanornationalregulatoryconditions. 6Chemicals Allthechemicalsusedforthetestshallbeofanalyticalgrade.Page5 EN12963:2001 7Apparatus Ordinarylaboratoryapparatusand, 7.1 Analyticalbalance ,accurateto0,1mg. 7.2 Ultrasonicbath. 7.3 Vials,ofa6mlcapacity. 7.4 Gaschromatograph ,havingaFIDdetector
23、andalineartemperatureprogrammer. 7.5 Capillarycolumn ,of30mlength,0,32mminternaldiameter,andsilicacoatedwithafilmof polyethyleneglycol20Mof1 mthickness.Othercolumnshavingequivalentorsuperiorperformancesmayalsobe used. 7.6 Integratororsuitablerecorder Therecordershallhaveafullscaledeflectionof10mV,af
24、ullscaleresponsetimeof2sorless,andamaximum noiselevelof 0,03%. 7.7 Microsyringe,ofa10 lto50 lcapacitygraduatedto1 l. 8 Samplingandsamplepreparation AsampleoftheadhesiveshallbetakeninaccordancewithEN1066andpreparedfortestinginaccordancewith EN1067. 9Chromatographic conditions Typicaloperatingconditio
25、ns(maybemodifiedaccordingtoseparationproblems,ifnotedinthetestreport). Carrier:Hydrogen Columnflow:1,5ml/min Splitflow:5ml/min Carrierpressure:20kPa Injectortemperature:350 C Detectortemperature:350 C Initialtemperature:50 C Initialtime:5min Rate:30 C/min Finaltemperature:190 C Totalanalysistime:16,
26、5minPage6 EN12963:2001 10 Calibrationofthegaschromatograph 10.1 Externalstandardmethod Determinetheresponseareasandtheretentiontimesofeachmonomerexpectedtobepresentintheadhesiveby injectingsamplesofastandardamountof4 lwithvariousconcentrationsofeachmonomer.Measurethepeak areasoftheindividualcomponen
27、tsandplottheareasversustheiramounts. 10.2 Internalstandardmethod Determinetheresponsefactorsandtheretentiontimesofeachcomponentexpectedtobepresentintheadhesive byinjectingasolutioncontainingmeasuredamountsofaninternalstandardandofthesinglecomponent. Thesolventshallbethesameastheoneusedforthesamplean
28、alysis(11). Calculatethepeakareasandcalculatetherelativeresponsefactor,RF,usingthefollowingequation: AsxWc RF= AcxWs where: As=peakareaoftheinternalstandard Ac=peakareaofthesinglecomponent Ws=weightoftheinternalstandard Wc=weightofthesinglecomponent 11Procedure 11.1General Iftheinternalstandardmetho
29、dischosen(10.2),preparetheinternalstandardsolutionmeasuringaproperamount ofinternalstandardanddissolvingitinthesolventtobeusedfortheextraction(11.2)orforthedilution(11.3and 11.4). Inthecase11.2theinternalstandardshouldbepreferablysolubleintheextractionsolventinordertoseparateit quantitativelyfromthe
30、waterphase. Inject4 lofsolventphase.Thevolumehastobepreciseiftheexternalstandardmethodisused. 11.2 Waterborneadhesives Forwaterborneadhesivesweightinavial(7.3)3gofadhesiveusingthebalance(7.1),addexactly5mlofhexane andplugthevial.Putthevialintheultrasonicbath(7.2)for10mintopromotetheextraction.Remove
31、thevialfrom thebath,allowtosettlefor15min.Thetwophaseswillseparateclearly. Othersolventscanbeusedinsteadofhexane.Theyshallbeabletoextractquantitativelythemonomersand clearlyseparatefromwater. 11.3 Solventborneadhesives Forsolventborneadhesivesweight1gofsolution.Ifnecessary,dilutewithsolventtoobtaina
32、ninjectablesolution. Fordiluting,oneofthesolventsalreadycontainedinthesolventborneadhesive,istobepreferred.Page7 EN12963:2001 Plugthevialandstirtohomogenise. 11.4Solventless adhesives Forsolventlessadhesivesmakeasolutioninasuitablesolventandproceedasdescribedin11.2.Thesolventshall notinterferewithth
33、emonomerstobeanalyzed. 12 Expressionofresults Determinetheconcentrationofeachcomponentasappropriate: a)iftheexternalstandardmethodisfollowed,calculatetheconcentrationofthecomponentdividingtheabsolute amountobtainedinthecalibrationcurve(in g)bytheweightofthesamples(ingrammes); b)iftheinternalstandard
34、methodisfollowed,calculatetheconcentrationusingtheecuationgivenbelow: AcxRFxCsxWs C= AsxWd Where C=concentrationofthesinglecomponentinmilligrammesperkilogram Ac=peakareaofthesamecomponent RF=relativeresponsefactorofthesamecomponent Cs=concentrationoftheinternalstandardintheinternalstandardsolutionin
35、milligrammesperkilogram Ws=weightoftheinternalstandardsolutioningrammes As=peakareaoftheinternalstandard Wd=weightoftheoriginalsampleingrammes 13 Testreport Thetestreportshallinclude: a)referencetothisEuropeanStandard; b)thetypeanddesignationoftheadhesivetested; c)theresultofthetestexpressedinaccord
36、ancewithclause12; d)anymodificationtotheproceduredescribedandanycircumstanceswhichmayhaveaffectedtheresult(sample preparation,extractionsolvent,calibration,etc.); e)thedateofthetest.BS EN 12963:2001 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent nat
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