SIST EN 13628-2:2003
(Main)Packaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 2: Industrial methods
Packaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 2: Industrial methods
This part 2 should be read in conjunction with prEN (261190) part 1 and describes rapid methods as commonly used in quality control for example for monitoring the level of residual solvents used in the production of flexible packaging by static headspace chromatography. The procedure described in this part involves one single injection of the headspace which implies an incomplete extraction of the solvent. The values obtained may be lower than the absolute content which should be determined according to Part 1. During the analysis there may be interferences from possible products of thermal decomposition.
Verpackung - Flexible Packstoffe - Bestimmung der Restlösemittel durch statische Dampfraumanalyse mittels Gaschromatographie - Teil 2: Industrielle Verfahren
Dieser Teil der Europäischen Norm beschreibt Schnellverfahren, die üblicherweise in der Qualitätskontrolle angewendet werden, um Restgehalte von bei der Produktion von flexiblen Packmaterialien verwendeten Lösemitteln mittels gaschromatographischer Dampfraumanalyse zu überwachen. Das in diesem Teil beschriebene Verfahren beinhaltet eine Einfachinjektion des Dampfraumes, die eine unvollständige Extraktion des Lösemittels zur Folge hat. Die so erhaltenen Werte können geringer sein als der Absolutwert, der entsprechend Teil 1 bestimmt werden sollte. Reste von thermischen Zersetzungsprodukten werden von dieser Norm nicht erfasst.
Dieses Verfahren ist für flexible Packstoffe anwendbar, die aus ein- oder mehrschichtigen Kunststofffolien, Papier oder Karton, Metallfolien oder deren Verbundmaterialien bestehen.
Dieses Verfahren ist für Restlösemittelgehalte kleiner als 0,5 mg/m2 nicht anwendbar.
Emballage - Matériaux d'emballages souples - Détermination des solvants résiduels par chromatographie en phase gazeuse et espace de tete statique - Partie 2: Méthodes industrielles
La présente partie (partie 2), qu'il convient de consulter conjointement au prEN(261 WI 190) partie 1, décrit les méthodes rapides couramment utilisées pour le contrôle de la qualité, par exemple pour surveiller le niveau de solvants rési duels utilisés dans la fabrication d'emballages souples par chromatographie en phase gazeuse et espace de tete statique. Le mode opératoire décrit dans cette partie consiste en une injection unique de l'espace de tete impliquant une extraction incomplete du solvant. Les valeurs obtenues peuvent etre inférieures au contenu absolu qu'il convient de déterminer selon la partie 1.
Embalaža – Prožni embalažni materiali – Določevanje ostanka topil s statičnim vzorčevalnikom iz plinske faze (headspace) za plinsko kromatografijo – 2. del: Industrijska metoda
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Verpackung - Flexible Packstoffe - Bestimmung der Restlösemittel durch statische Dampfraumanalyse mittels Gaschromatographie - Teil 2: Industrielle VerfahrenEmballage - Matériaux d'emballages souples - Détermination des solvants résiduels par chromatographie en phase gazeuse et espace de tete statique - Partie 2: Méthodes industriellesPackaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 2: Industrial methods55.040SDNLUDQMHPackaging materials and accessoriesICS:Ta slovenski standard je istoveten z:EN 13628-2:2002SIST EN 13628-2:2003en01-julij-2003SIST EN 13628-2:2003SLOVENSKI
STANDARD
SIST EN 13628-2:2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13628-2October 2002ICS 55.040English versionPackaging - Flexible packaging material - Determination ofresidual solvents by static headspace gas chromatography -Part 2: Industrial methodsEmballage - Matériaux d'emballages souples -Détermination des solvants résiduels par chromatographieen phase gazeuse et espace de tête statique - Partie 2:Méthodes industriellesVerpackung - Flexible Packstoffe - Bestimmung derRestlösemittel durch statische Dampfraumanalyse mittelsGaschromatographie - Teil 2: Industrielle VerfahrenThis European Standard was approved by CEN on 26 August 2002.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13628-2:2002 ESIST EN 13628-2:2003
EN 13628-2:2002 (E)2ContentspageForeword.31Scope.42Normative references.43Principle.44Reagents.55Apparatus.56Sampling.87Test specimens.88Incubation of the test specimens.89Procedure.910Precision data.1211Test report.12SIST EN 13628-2:2003
EN 13628-2:2002 (E)3ForewordThis document EN 13628-2:2002 has been prepared by Technical Committee CEN/TC 261 "Packaging", thesecretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by April 2003, and conflicting national standards shall be withdrawn at the latest byApril 2003.This standard is part of a standard for determination of residual solvents by static headspace gas chromatography,which is published in two parts:- Part 1: Absolute methods- Part 2: Industrial methodsThis part of EN 13628 should be read in conjunction with EN 13628-1.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain,Sweden, Switzerland and the United Kingdom.SIST EN 13628-2:2003
EN 13628-2:2002 (E)41 ScopeThis part of this European Standard specifies rapid methods as commonly used in quality control for monitoring thelevel of residual solvents used in the production of flexible packaging by static headspace chromatography. Theprocedures described in this part involve one single injection of the headspace which implies an incompleteextraction of the solvent. The values obtained may be lower than the absolute content which should be determinedaccording to Part 1. Residues from thermal decomposition products are not within the scope of this standard.The method is applicable to flexible packaging materials that may consist of mono- or multilayer plastic films, paperor board, foil or combinations thereof.This method does not apply to residual solvents with amounts lower than 0,5 mg/m².2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).ISO 2859-1, Sampling procedures for inspection by attributes - Part 1: Sampling schemes indexed by acceptancequality limit (AQL) for lot-by-lot inspection.ISO 2859-2, Sampling procedures for inspection by attributes - Part 2: Sampling plans indexed by limiting quality(LQ) for isolated lot inspection.ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for thedetermination of repeatability and reproducibility of a standard measurement method.3 PrincipleSpecimens of the flexible packaging material are placed in a hermetically closed vial and heated under closelycontrolled conditions of time and temperature to vaporize solvents into the headspace. The amount of solventreleased into the headspace is determined by transferring an aliquot of the headspace into a gas chromatographfor analysis. The transfer may be performed:a) by specific semi-automatic or automatic systems which allow pressurization of the heated vials;b) manually or automatically by using a heated gastight syringe or a loop without pressurization of theheated vials.The relative amount of residual solvent is determined by single headspace extraction using external or internalstandards.NOTEFor reproducibility the same incubation conditions should be used for each single analysis. During the analysis,there could be interferences from possible products of thermal decomposition. Additional peaks due to these products shouldnot be considered for evaluation of residual solvents.SIST EN 13628-2:2003
EN 13628-2:2002 (E)54 Reagents4.1 GeneralAll reagents shall be of a recognized analytical reagent grade.NOTEGrades stated as being suitable for chromatography can be commercially available and are recommended for useas reference for standard calibration solutions. Appropiate safety precautions should be used when handling toxic and/orflammable solvents.4.2 Reference solvents, for the preparation of standard calibration solutions.4.3 Dilution solvent, with a retention time different from those of residual solvents in the sample.NOTESolvents such as hexane, cyclohexanaone, acid amides and glycerol triacetate (triacetin) are appropriate.5 Apparatus5.1 Glass vials, of capacity 6 ml, 8 ml, 20 ml, 50 ml or 100 ml depending upon the specific requirements ofaccessory equipment, for example, the headspace sampler, fitted with an inert septum seal and aluminium crimptops. The septum seal shall neither absorb nor release volatile components, shall be gas tight during incubationand shall permit samples of the headspace gas to be withdrawn by syringe for subsequent analysis.NOTEElastomers lined with polytetrafluoroethylene (PTFE) are suitable materials for septum seals.5.2 Crimping tool, for sealing the vials with the aluminium crimp tops.5.3 Seal removing tool.5.4 Analytical balance, capable of weighing to the nearest 0,1 mg.5.5 Template, for cutting samples. The dimensions of this template shall be matched to the vial volume used.5.6 Scalpel, or sharp knife.5.7 Syringes (e.g. 1 µl, 10 µl)5.8 Gas chromatograph, having a flame ionization detector or equivalent for the solvents to be determined.5.9 Gas chromatographic column, either packed or capillary, that will give good resolution of the solvents tobe determined from any other components that might be injected with the specimen of the headspace.Examples for suitable columns and operation conditions are:a) Packed columnlength: 3 m;internal diameter: 3,2 mm;column filling: 80/120 mesh graphitised carbon, deactivated with polyethyleneglycol;carrier gas: N2, 20 ml/min; injector temperature: 220 °C;temperature programme: 80 °C; raised to 160 °C at 6 °C/min; raised to 225 °Cat 1,5 °C/min; hel
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