BS EN 12963-2001 Adhesives - Determination of free monomer content in adhesives based on synthetic polymers《胶粘剂 基于合成聚合物的胶粘剂中单体含量测定》.pdf

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

37、ional body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess

38、the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of

39、 which can be found on the inside front cover. Tel: 020 8996 9000. Fax: 020 8996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign s

40、tandards publications should be addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001. Standards are also available from the BSI website at http:/www.bsi-. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been pu

41、blished as British Standards, unless otherwise requested. Information on standards BSI provides a wide range of information on national, European and international standards through its Library and its Technical Help to Exporters Service. Various BSI electronic information services are also availabl

42、e which give details on all its products and services. Contact the Information Centre. Tel: 020 8996 7111. Fax: 020 8996 7048. Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and oth

43、er benefits contact Membership Administration. Tel: 020 8996 7002. Fax: 020 8996 7001. Further information about BSI is available on the BSI website at http:/www.bsi-. Copyright Copyright subsists in all BSI publications. BSI also holds the copyright, in the UK, of the publications of the internatio

44、nal standardization bodies. Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, photocopying, recording or otherwise without prior written permission from BSI. This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations. If these details are to be used for any other purpose than implementation then the prior writt