1、Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSIDRAFT FOR DEVELOPMENT DD CEN/TS 14577:2003 Materials and articles in contact with foodstuffs Plastics Polymeric additives Test method for the determination of the mass fraction of a pol
2、ymeric additive that lies below 1 000 Daltons ICS 67.250, 83.040.30 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSIDD CEN/TS 14577:2003 This Draft for Development was published under the authority of the Standards Policy and Strateg
3、y Committee on 16 January 2004 BSI 16 January 2004 ISBN 0 580 43260 2 National foreword This Draft for Development is the official English language version of CEN/TS 14577:2003. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of pu
4、blications and is of a provisional nature because of the need to develop a reliable method of test for the determination of molecular weight fractions below 1 000 Daltons in polymeric additives. It should be applied on this provisional basis, so that information and experience of its practical appli
5、cation may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated 2 years after its publication by
6、the European organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period, the r
7、esponsible BSI Committee will decide whether to support the conversion into a European standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1, Migration from plastics, at British Standards House,
8、389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which i
9、mplement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. Summary of pages
10、 This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 14, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Lice
11、nsed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSITECHNICALSPECIFICATION SPCIFICATIONTECHNIQUE TECHNISCHESPEZIFIKATION CEN/TS14577 December2003 ICS67.250,83.040.30 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics Polymeri
12、cadditivesTestmethodforthedeterminationofthe massfractionofapolymericadditivethatliesbelow1000 Daltons WerkstoffeundGegenstndeinKontaktmit LebensmittelnKunststoffePolymereZusatzstoffe PrfverfahrenzurBestimmungdesMasseanteilseines polymerenZusatzstoffesunter1000Dalton ThisTechnicalSpecification(CEN/T
13、S)wasapprovedbyCENon17 th March2003forprovisionalapplication. TheperiodofvalidityofthisCEN/TSislimitedinitiallytothreeyears.AftertwoyearsthemembersofCENwillberequested tosubmittheir comments,particularlyonthequestionwhethertheCEN/TScanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannounce
14、theexistenceofthisCEN/TSinthesamewayasforanENandtomaketheCEN/TSavailable .It ispermissibletokeepconflictingnationalstandardsinforce(inparalleltotheCEN/TS)untilthefinaldecisionaboutthep ossible conversionoftheCEN/TSintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepub
15、lic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B105
16、0Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.CEN/TS14577:2003 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSICEN/TS14577:2003(E) 2 Contents page Foreword3 1 Scope 5 2
17、 Principle5 3 Reagents.5 4 Apparatus .6 5 Preparationofstandardsandsamples .8 6 SECanalysis .8 7 Expressionofresults . .10 8 Testreport . .11 AnnexA (informative) Couplingofliquidchromatographicpolymerseparationswithmass spectrometry 12 AnnexZA (informative) ClausesofthisTechnicalSpecificationaddres
18、singessentialrequirementsor otherprovisionsofEUDirectives. . 13 Bibliography 14 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSICEN/TS14577:2003(E) 3 Foreword Thisdocument(CEN/TS14577:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC194
19、,“Utensilsin contactwithfood“,thesecretariatofwhichisheldbyBSI. ThisdocumenthasbeenpreparedunderamandategiventoCENbytheEuropeanCommissionandtheEuropean FreeTradeAssociation. ForrelationshipwithEUDirective(s),seeinformativeannexZA,whichisanintegralpartofthisdocument. AnnexAisinformative. Accordingtot
20、heCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoannouncethisEuropeanSpecification:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway, Portugal,Slovakia,Spain,Sweden
21、,SwitzerlandandtheUnitedKingdom. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSICEN/TS14577:2003(E) 4 Introduction Someadditivesusedtomakeplasticsintendedtocomeintocontactwithfoodstuffsareknownaspolymeric additives1.Theyareaddedtopl
22、asticsinordertoachieveatechnicaleffectbuttheydonotinisolationhavethe physicalpropertiesrequiredofusableplasticsmaterialsandarticles.Inthisrespecttheydifferfromthehigh polymersthatareusedtomakeplastics.Thesepolymericadditivesdonotgenerallyhaveasinglemolecular weightbuttheyhaveamolecularweightdistribu
23、tionasaresultofsynthesis.Theymayalsoshowfurther complexitywithdifferentendgroupchemistry(becauseofdifferentinitiationandterminationprocesses),different repeatunits(becauseoftwoormoremonomersusedtomakerandomorblockcopolymers)anddifferentchain shapes(becauseoftheformationoflinear,branchedandcyclicstru
24、ctureswithinthechains). Theseadditivesmaymigrateintofoodstuffsplacedincontactwiththeplasticsandsotheirsafetymustbe evaluated.Onlythefractionoftheadditivewithmolecularmassbelow1000Daltons(D)isregardedasbeing toxicologicallyrelevantandsoadistinctionhasbeenmadebytheScientificCommitteeforFood(SCF)betwee
25、n polymericadditiveswithaweightaveragedmolecularmass(MW)below1000DandthosewithMWabove1000D 2.ForthosepolymericadditiveswithaMWabove1000D,onlyareducedsetofdatamayberequiredtoallow anevaluationoftheirsafety. TherequirementsoftheSCFandthepracticalimplicationshavebeendescribedanddiscussedinaCommission d
26、ocument3.Indecidingwhichtoxicologicalinformationisneeded,theSCFconsidersthedataavailableonthe monomersusedtomakethepolymericadditive,thesizeoftheadditivefractionwithMWbelow1000D,andthe formulationleveloftheadditiveusedintheplastic2.Itispossiblethatapolymericadditiveconsideredbythe SCFisgivenapproval
27、tobeusedinplasticsintendedforfoodcontact,butwithspecificationsincludingalimiton themassfractionoftheadditivebelowMW1000.Forthesereasons,forpetitionsandfortestingforcompliance,a methodoftestisrequiredtodeterminethemassfractionofapolymericadditivethatfallsbelowtheMW1000cut offsetbytheSCF. Licensed Cop
28、y: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSICEN/TS14577:2003(E) 5 1Scope ThisTechnicalSpecificationspecifiesatestmethodtodeterminethemassfractionofapolymericadditivethatfalls belowaMWof1000.Themethodisapplicabletopolymericadditives persei.e.
29、suppliedintheirusableform, beforeformulationintoaplastic.Themethodisalsoapplicabletopolymericadditivesextractedfromfinished plasticmaterialsandarticles,providedthatprecautionsaretakentoensuretheabsenceofanyinterferencefrom anyothercoextractivesderivedfromtheplastic. 2Principle Thepolymericadditiveis
30、fractionatedusingsizeexclusionchromatography(SEC)andthemassfractionbelowMW 1000Disdeterminedeithergravimetrically,offline,orbyusingchromatographicdetectorssuchasrefractive index,infrared,ultraviolet,orlightscatteringdetectors,online. Thechromatogramiscalibratedformolecularweighteitherbyusingcalibrat
31、ionstandards,wherethesesubstances areavailable,orbyusingmassselectivedetectorssuchasmassspectroscopy.Underidealconditionswhere thereisnointeractionwiththestationaryphase,intheSECseparationofoligoorpolymericmulticomponent systemsthecomponentsareseparatedwithrespecttotheirhydrodynamicvolumes.Consequen
32、tly,retentiontimes (elutionvolumes)indicatethemolecularsizeandcanbeconvertedintomolecularweightbyuseofcalibration standardsrunconcurrentlyorbyusingmolecularweightsensitivedetectors(onlineoroffline). Thepolymericadditivesubmittedtothetestshouldbethesameasthatusedtoformulatethefinishedplastic material
33、orarticle.Iftheadditiveisnotavailableassuch,thenitmaybeextractedfromthefinishedplasticand thensubmittedtothistestprocedureprovidedthatcareistakentoensurethatnosignificantinterferenceoccurs fromanyothercoextractivesfromtheplastic. NOTE Fortheseparationofpolarsubstancesinaqueoussystems,SECissometimesr
34、eferredtoasgelfiltration chromatography(GFC).Fortheseparationoforganicsubstancesinnonaqueoussystemsitissometimescalledgel permeationchromatography(GPC).ThetermandabbreviationSECisusedheretodescribeallthesetypesof chromatography. 3Reagents 3.1General Allreagentsshallbeofrecognisedanalyticalquality,un
35、lessotherwisespecified. 3.2 Molecularweightstandards 3.2.1General Avarietyofmolecularweightstandardsareavailablecommercially.Someareavailableinpureform,andothers asmixtureswithtwoormorespeciespresent.SincetheaimofMWcalibrationistosetthe1000Dcutoffpointin theSECchromatogram,itispreferablytohaveoneMWs
36、tandardcloseto1000Dwithtwootherseachside(i.e. aboveandbelow1000D)sothatthecutoffpointcanbedeterminedbyinterpolation. 3.2.2 Forpolarpolymericadditives Examplesofpolarpolymericadditivesincludepolyethyleneglycols(PEGs),lignosulfonates,polyacrylamidesand polyacrylates.PEGoligomersarecommonlyusedforSECca
37、librationinbothaqueousandpolarorganicsolvents. PEGcalibrantsareavailablecommerciallyfromthedimer(MW106)upwards.Polyethyleneoxide(PEO) standardsarealsoavailablecommercially. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 05 April 2004, Uncontrolled Copy, (c) BSICEN/TS14577:
38、2003(E) 6 3.2.3 Fornonpolarpolymericadditives Examplesofnonpolarpolymericadditivesarehydrocarbonoilsandwaxes,hydrogenatedhydrocarbonresins,and polyesterplasticisers.Polystyreneoligomersandindividualnalkanesarethemostwidelyusedstandardsfor calibratingSECinorganicsolvents.Polystyreneoligomersareavaila
39、blecommerciallyfromthedimer(MW162) upwards.Averylargenumberofnalkanesareavailableinpureform. 4Apparatus 4.1General Aninstrumentorpieceofapparatusismentionedonlyifitisspecial,ormadetoparticularspecifications.Usual laboratoryequipmentisassumedtobeavailable. 4.2 SECequipment Highperformanceliquidchroma
40、tograph,equippedwithadetectorsuitableforthepolymericadditiveundertest, andfittedwithafractioncollectorifitisintendedtocollectfractions.Theliquidchromatographshouldbecapable ofmaintainingaconstantflowrateofmobilephase. NOTE Underconditionsofconstantflow,theretentiontimeofacomponentisrelateddirectlyto
41、itselutionvolumewhich, ontheparticularSECcolumnemployed,isacharacteristicofitsmolecularsize. 4.3 SECcolumn Thecolumnhastopermittheseparationofthepolymericadditiveaccordingtoitsmolecularweightdistribution. ThecolumnshouldbecapableofseparatingtheadditiveespeciallyattheMW1000boundaryandtheporesize shou
42、ldbeselectedtogiveoptimumseparationinthisregion. NOTE1 Thechoiceoftheappropriatecolumntype(stationaryphase)dependsonthemolecularsizeandthechemical propertiesofthepolymericadditivestobecharacterised.MostSECcolumnswillfractionatewithinaparticularmolecularwei ght range,determinedbytheporesizeofthestati
43、onaryphase.Largemoleculesaretotallyexcludedfromthestationaryphaseand areelutedwiththevoidvolume.Smallmoleculesbelowthefractionationrangeareelutedatanelutionvolumeapproximately equaltothetotalbedvolume.Acolumnshouldbechosensothatthecriticalcutoffpointforthistest1000Doccursno tlater thanmidwaythrought
44、heseparationwindowbetweenthetotallyexcludedvolumeandthetotallyincludedvolume. NOTE2 Foronlinedetection,thecolumnshouldbeananalyticalcolumn,withtypicalinternaldiameterof3to7mm.The columnlengthrequireddependsontheefficiencyofthepackingmaterialemployed.Atypicalcolumnlengthwouldbe100to 300mm.Columnscanbelinkedinseriesifneededtoincreasetheseparation. NOTE3 Forofflinedetection,itisdesirabletousea
