1、BRITISH STANDARD BS EN 13628-2:2002 Packaging Flexible packaging material Determination of residual solvents by static headspace gas chromatography Part 2: Industrial methods The European Standard EN 13628-2:2002 has the status of a British Standard ICS 55.040 BS EN 13628-2:2002 This British Standar
2、d, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 21 October 2002 BSI 21 October 2002 ISBN 0 580 40626 1 National foreword This British Standard i
3、s the official English language version of EN 13628-2:2002. The UK participation in its preparation was entrusted by Technical Committee PKW/5, Primary and transport packaging, to Subcommittee PKW/5/26, Packaging made from flexible materials, which has the responsibility to: A list of organizations
4、represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondenc
5、e Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itsel
6、f confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and pr
7、omulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publ
8、ication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN136282 October2002 ICS55.040 Englishversion PackagingFlexiblepackagingmaterialDeterminationof residualsolventsbystaticheadspacegaschromatography Part2:Industrialmethods EmballageMatriauxdemballagessouples Dterminationdess
9、olvantsrsiduelsparchromatographie enphasegazeuseetespacedettestatiquePartie2: Mthodesindustrielles VerpackungFlexiblePackstoffeBestimmungder RestlsemitteldurchstatischeDampfraumanalysemittels GaschromatographieTeil2:IndustrielleVerfahren ThisEuropeanStandardwasapprovedbyCENon26August2002. CENmembers
10、areboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. T
11、hisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,C
12、zechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels
13、2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN136282:2002EEN136282:2002(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Principle4 4 Reagents.5 5 Apparatus .5 6 Sampling.8 7 Testspecimens 8 8 Incubationofthetestspecimens .8 9
14、Procedure .9 10 Precisiondata. 12 11 Testreport 12EN136282:2002(E) 3 Foreword ThisdocumentEN136282:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC261“Packaging“,the secretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byen
15、dorsement,atthelatestbyApril2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby April2003. Thisstandardispartofastandardfordeterminationofresidualsolventsbystaticheadspacegaschromatography, whichispublishedintwoparts: Part1:Absolutemethods Part2:Industrialmethods ThispartofEN13628shoul
16、dbereadinconjunctionwithEN136281. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norw
17、ay,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN136282:2002(E) 4 1Scope ThispartofthisEuropeanStandardspecifiesrapidmethodsascommonlyusedinqualitycontrolformonitoringthe levelofresidualsolventsusedintheproductionofflexiblepackagingbystaticheadspacechromatography.The proceduresdescribedint
18、hispartinvolveonesingleinjectionoftheheadspacewhichimpliesanincomplete extractionofthesolvent.Thevaluesobtainedmaybelowerthantheabsolutecontentwhichshouldbedetermined accordingtoPart1.Residuesfromthermaldecompositionproductsarenotwithinthescopeofthisstandard. Themethodisapplicabletoflexiblepackaging
19、materialsthatmayconsistofmonoormultilayerplasticfilms,paper orboard,foilorcombinationsthereof. Thismethoddoesnotapplytoresidualsolventswithamountslowerthan0,5mg/m. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereference
20、sarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(
21、includingamendments). ISO28591, SamplingproceduresforinspectionbyattributesPart1:Samplingschemesindexedbyacceptance qualitylimit(AQL)forlotbylotinspection . ISO28592, SamplingproceduresforinspectionbyattributesPart2:Samplingplansindexedbylimitingquality (LQ)forisolatedlotinspection . ISO57252, Accur
22、acy(truenessandprecision)ofmeasurementmethodsandresultsPart2:Basicmethodforthe determinationofrepeatabilityandreproducibilityofastandardmeasurementmethod. 3Principle Specimensoftheflexiblepackagingmaterialareplacedinahermeticallyclosedvialandheatedunderclosely controlledconditionsoftimeandtemperatur
23、etovaporizesolventsintotheheadspace.Theamountofsolvent releasedintotheheadspaceisdeterminedbytransferringanaliquotoftheheadspaceintoagaschromatograph foranalysis.Thetransfermaybeperformed: a)byspecificsemiautomaticorautomaticsystemswhichallowpressurizationoftheheatedvials; b)manuallyorautomaticallyb
24、yusingaheatedgastightsyringeoraloopwithoutpressurizationofthe heatedvials. Therelativeamountofresidualsolventisdeterminedbysingleheadspaceextractionusingexternalorinternal standards. NOTE Forreproducibilitythesameincubationconditionsshouldbeusedforeachsingleanalysis.Duringtheanalysis, therecouldbein
25、terferencesfrompossibleproductsofthermaldecomposition.Additionalpeaksduetotheseproductsshould notbeconsideredforevaluationofresidualsolvents.EN136282:2002(E) 5 4Reagents 4.1General Allreagentsshallbeofarecognizedanalyticalreagentgrade. NOTE Gradesstatedasbeingsuitableforchromatographycanbecommercial
26、lyavailableandarerecommendedforuse asreferenceforstandardcalibrationsolutions.Appropiatesafetyprecautionsshouldbeusedwhenhandlingtoxicand/or flammablesolvents. 4.2Referencesolvents, forthepreparationofstandardcalibrationsolutions. 4.3Dilutionsolvent, witharetentiontimedifferentfromthoseofresidualsol
27、ventsinthesample . NOTE Solventssuchashexane,cyclohexanaone,acidamidesandglyceroltriacetate(triacetin)areappropriate. 5Apparatus 5.1Glassvials, ofcapacity6ml,8ml,20ml,50mlor100mldependinguponthespecificrequirementsof accessoryequipment,forexample,theheadspacesampler,fittedwithaninertseptumsealandalu
28、miniumcrimp tops.Theseptumsealshallneitherabsorbnorreleasevolatilecomponents,shallbegastightduringincubation andshallpermitsamplesoftheheadspacegastobewithdrawnbysyringeforsubsequentanalysis. NOTE Elastomerslinedwithpolytetrafluoroethylene(PTFE)aresuitablematerialsforseptumseals. 5.2Crimpingtool, fo
29、rsealingthevialswiththealuminiumcrimptops. 5.3Sealremovingtool. 5.4Analyticalbalance, capableofweighingtothenearest0,1mg. 5.5Template, forcuttingsamples.Thedimensionsofthistemplateshallbematchedtothevialvolumeused. 5.6Scalpel,orsharpknife. 5.7Syringes (e.g.1l,10l) 5.8Gaschromatograph, havingaflameio
30、nizationdetectororequivalentforthesolventstobedetermined. 5.9Gaschromatographiccolumn, eitherpackedorcapillary,thatwillgivegoodresolutionofthesolventsto bedeterminedfromanyothercomponentsthatmightbeinjectedwiththespecimenoftheheadspace. Examplesforsuitablecolumnsandoperationconditionsare: a)Packedco
31、lumn length:3m; internaldiameter:3,2mm; columnfilling:80/120meshgraphitisedcarbon,deactivatedwithpolyethyleneglycol; carriergas:N 2 ,20ml/min; injectortemperature:220 C; temperatureprogramme:80 C;raisedto160 Cat6 C/min;raisedto225 C at1,5 C/min;heldfor16minEN136282:2002(E) 6 NOTE1 Acorrespondingchro
32、matogramobtainedforamixtureofsolventsisshowninFigure1. Key 1 4,23methanol 2 6,67ethanol 3 9,25acetone 4 17,06ethylacetate 5 19,1butanol 6 23,34trichloroethylene 7 28,4isobutylacetate 8 33,87methylisobutylketone 9 41,86toluene 10 64.06xylene A Retentiontime(min) B Peakheight Figure1Exampleofchromatog
33、ramobtainedwithapackedcolumn or b)Capillarycolumn:(fusedsilica): length:30m; internaldiameter:0,32mm; stationaryphase:Poly(dimethylsiloxane)filmthickness3 m m; carriergas:He1,7ml/min; carriergassplitratio:1:20; injectortemperature:230 C; detector(flameionisation)temperature:280 C;EN136282:2002(E) 7
34、temperatureprogramme:50 Cheldfor5min;raisedto100 Cat5 C/min;raised to250 Cat10 C/min. NOTE2 AcorrespondingchromatogramisshowninFigure2. Key 1 Methanol 2 Ethanol 3 Isopropanol 4 Methylethylketone 5 Ethylacetate 6I s o b u t a n o l 7 Isopropylacetate 8 npropylacetate 9 Methylisobutylketone 10 Etoxypr
35、opanol 11 Toluene 12 nbutylacetate 13 Xylene 14 Butylcellosolve A Retentiontime(min) B Peakheight Figure2Exampleofchromatogramobtainedwithacapillarycolumn NOTE Otherapparatuswhichismorespecifictothealternativemethodsisidentifiedundertherelevantclauses.EN136282:2002(E) 8 6Sampling Samplingshallbeinac
36、cordancewithinternalqualitycontrolprocedures. SamplingshallfollowISO28591andISO28592. Samplesofpackagingmaterialsthataretobeanalyzedshallbehandledandstoredsoastopreventeitherlossof volatilesolventsorcontaminationbyabsorptionofvolatilesolventsthatmaybepresentinthesurrounding atmosphere.Samplingandana
37、lysisshallbedoneinaplacewheretheairissolventfreetoreducetheproblemof contaminationfromthesurroundingsduetothelowconcentrationofresidualsolventsinthesamples. NOTE Ifsamplesneedtobestoredtheyshouldbeintightlypackedrollformifpossible. Sheetsamplesmaybepreparedfromtherollbycuttingoutasquarewindow(severa
38、llayersofsheets)withaknife. Wheninformofsheetstheyshouldbestackedtightlytogethertoformacompact“block”andwrappedtightlyina barriermaterial,preferablyaluminiumfoilwithathicknessof30 m mto40 m m.Forstorageperiodsofmorethanone hourthewrappedsamplesshouldbestoredattemperaturesbelow5 Candinanatmospherefre
39、eofvolatile contaminants. 7 Testspecimens 7.1Specimenareainrelationtovialvolume Thespecimenareatobecutoutshalldependonthevialvolumeandthelevelofresidualsolventstobe determinedinthematerial.Usuallytheratiobetweenthespecimenarea(incm)andthevialvolume(inml)shall bebetweenthreeandfive.Thespecimensshallb
40、ecutoutusinganappropriatetemplate( 5.5). NOTE Asanexample,foravialwithavolumeof6mlto9mlaspecimenof30cm(2cm15cm)canbeusedor proportionaldimensionsforothervolumes. 7.2Testspecimens Fromarepresentativesample(seeclause 6)cutaspecimenusingatemplate( 5.5).Coilthespecimenrapidlyand immediatelyputitintothev
41、ial.Crimpthevialimmediatelytosealit. Thefollowingprecautionsshallbetaken: thedifferentstepsofthepreparationshallbedoneveryrapidlytoavoidevaporationofthesolvents; thespecimensshallalwaysbecutatadefinedplacee.g.onthesamedrawingprintedonthesameplace inthewidthandthetemplateforcuttingshallalwaysbeplaced
42、inthesamemanner. 8 Incubationofthetestspecimens Incubationtemperatureandtimeshallbechosentosuitthematerialsbeingtestedandthesolventslikelytobe present.Conditionsusedshallbeincludedinthetestreport. NOTE Incubationconditionsof110 Cfor20minarerecommended. Inordertocompareresidualsolventlevels,incubatio
43、nconditionsusedshallbethesame.Toensurerepeatability, thetemperatureshallbeaccurateto2 Candtimeshallbeaccurateto0,5min.EN136282:2002(E) 9 9Procedure 9.1General Quantitativeanalysisofresidualsolventsshallbecarriedoutusingoneofthetwomethodsofstaticheadspace chromatographydescribedinthisclause,asappropriate.Themethodsare: semiautomaticorautomaticinjection(see 9.2);and manualinjection(see 9.3). 9.2Semiautomaticorautomaticinjection 9.2.1General Thismethodshallbeusedwhereasemiautomaticorautomat
