Packaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 1: Absolute methods

This part 1 describes methods for the quantitative determination of residual solvents in flexible packaging by static headspace chromatography. The chemical identities of the residual solvents to be determined by this must be known before commencing the analysis. During the analysis there may be interferences from possible products of thermal decomposition. Residues from thermal decomposition products are not within the scope of this standard. Additional peaks due to these products shall not be considered for evaluation of residual solvents.

Verpackung - Flexible Packstoffe - Bestimmung der Restlösemittel durch statische Dampfraumanalyse mittels Gaschromatographie - Teil 1: Absolute Verfahren

Dieser Teil 1 beschreibt Methoden zur quantitativen Bestimmung von Restlöse- mitteln in flexiblen Verpackungen durch statische Dampfraumanalyse mittels Gaschromatographie. Die chemische Identität der Restlösemittel, die mit dieser Methode bestimmt werden sollen, muß bekannt sein, bevor die Analyse durchgeführt wird. Während der Analyse können im Chromatogramm Überlagerungen durch thermische Abbauprodukte auftreten, deren Bestimmung nichtim Anwendungßweck dieser Norm liegt.

Emballage - Matériaux d'emballages souples - Détermination des solvants résiduels par chromatographie en phase gazeuse et espace de tete statique - Partie 1: Méthodes absolues

La présente partie de la présente Norme Européenne spécifie des méthodes de détermination quantitative des solvants résiduels présents dans les emballages souples, par chromatographie en phase gazeuse et espace de tete statique, l'identité chimique des solvants résiduels a déterminer étant connue avant le début de l'analyse. Les résidus issus des produits de décomposition thermique n'entrent pas dans le domaine d'application de la présente norme.
La méthode s'applique aux matériaux d'emballages souples pouvant etre constitués de films plastiques mono- ou multicouches, de papier ou de carton, de feuilles d'aluminium ou d'une combinaison de ces matériaux.
La présente méthode ne s'applique pas aux solvants résiduels dont les quantités sont inférieures a 0,5 mg/m2.

Embalaža – Prožni embalažni materiali – Določevanje ostanka topil s statičnim vzorčevalnikom iz plinske faze (headspace) za plinsko kromatografijo – 1. del: Absolutna metoda

General Information

Status
Published
Publication Date
30-Jun-2003
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jul-2003
Due Date
01-Jul-2003
Completion Date
01-Jul-2003

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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 1: Absolute VerfahrenEmballage - Matériaux d'emballages souples - Détermination des solvants résiduels par chromatographie en phase gazeuse et espace de tete statique - Partie 1: Méthodes absoluesPackaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 1: Absolute methods55.040SDNLUDQMHPackaging materials and accessoriesICS:Ta slovenski standard je istoveten z:EN 13628-1:2002SIST EN 13628-1:2003en01-julij-2003SIST EN 13628-1:2003SLOVENSKI

STANDARD
SIST EN 13628-1:2003

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13628-1October 2002ICS 55.040English versionPackaging - Flexible packaging material - Determination ofresidual solvents by static headspace gas chromatography -Part 1: Absolute methodsEmballage - Matériaux d'emballages souples -Détermination des solvants résiduels par chromatographieen phase gazeuse et espace de tête statique - Partie 1:Méthodes absoluesVerpackung - Flexible Packstoffe - Bestimmung derRestlösemittel durch statische Dampfraumanalyse mittelsGaschromatographie - Teil 1: Absolute 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 13628-1:2002 ESIST EN 13628-1:2003

EN 13628-1:2002 (E)2ContentspageForeword......................................................................................................................................................................31Scope..............................................................................................................................................................42Normative references....................................................................................................................................43Principle..........................................................................................................................................................44Reagents.........................................................................................................................................................45Apparatus.......................................................................................................................................................56Sampling.........................................................................................................................................................87Test specimens..............................................................................................................................................88Incubation of the test specimens.................................................................................................................89Procedure.......................................................................................................................................................910Precision data...............................................................................................................................................1611Test report....................................................................................................................................................16SIST EN 13628-1:2003

EN 13628-1:2002 (E)3ForewordThis document EN 13628-1:2002 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 methodsAccording 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 13628-1:2003

EN 13628-1:2002 (E)41 ScopeThis part of this European Standard specifies methods for the quantitative determination of residual solvents inflexible packaging by static headspace chromatography where the chemical identities of the residual solvents to bedetermined are known before commencing the analysis. Residues from thermal decomposition products are notwithin 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 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. Quantificationis achieved by the multiple headspace extraction (MHE) procedure using external or internal standards;b) manually or automatically by using a heated gastight syringe or a loop without pressurization of the heatedvials. Quantification is achieved by the standard addition method.NOTEA prerequisite for a quantitative determination of residual solvents by headspace gas chromatography is that apartition equilibrium for the solvent between the gas phase and the solid phase has been reached before an aliquot of theheadspace is withdrawn and transferred into the gas chromatograph.During the analysis, there may be interferences from possible products of thermal decomposition. Additional peaksdue to these products shall not be considered for evaluation of residual solvents.4 Reagents4.1 GeneralAll reagents shall be of a recognized analytical reagent grade.NOTEGrades stated as being suitable for chromatography are commercially available and are recommended for use asreference for standard calibration solutions. Appropriate safety precautions should be used when handling toxic and/orflammable solvents.SIST EN 13628-1:2003

EN 13628-1:2002 (E)54.2 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, cyclohexanone, 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. Examplesfor suitable columns and operation conditions are:a) Packed column:length: 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 °C at 1,5 °C/min; held for 16 min;NOTE 1A corresponding chromatogram obtained for a mixture of solvents is shown in Figure 1.SIST EN 13628-1:2003

EN 13628-1:2002 (E)6Key14,23 methanol26,67 ethanol39,25 acetone417, 06 ethyl acetate519,1 butanol623,34 trichloroethylene728,4 isobutyl acetate833,87 methyl isobutylketone941,86 toluene1064.06 xyleneARetention time (min)BPeak heightFigure 1 — Example of chromatogram obtained with a packed columnorb) Capillary column (fused silica):length: 30 m;internal diameter: 0,32 mm;stationary phase: Poly(dimethylsiloxane), film thickness 3 µm;carrier gas: He, 1,7 ml/min;SIST EN 13628-1:2003

EN 13628-1:2002 (E)7carrier gas split ratio: 1:20;injector temperature: 230 °C;detector (flame ionization) temperature: 280 °C;temperature programme: 50 °C held for 5 min; raised to 100 °C at 5 °C/min raised to 250 °C at 10 °C/min.NOTE 2A corresponding chromatogram for a mixture of solvents is shown in Figure 2.Key1Methanol2Ethanol3Isopropanol4Methylethyl ketone5Ethyl acetate6Isobutanol7Isopropyl acetate8n-propyl acetate9Methylisobutyl ketone10Ethoxypropanol11Toluene12n-butyl acetate13Xylene14Butyl cellosolveARetention time (min)BPeak heightFigure 2 — Example of chromatogram obtained with a capillary columnSIST EN 13628-1:2003

EN 13628-1:2002 (E)8NOTE 3Other apparatus which is more specific to the alternative methods is identified under the relevant clauses.6 SamplingSamples of packaging materials that are to be analysed shall be handled and stored so as to prevent either loss ofvolatile solvents or contamination by absorption of volatile solvents that may be present in the surroundingatmosphere. Sampling and analysis shall be done in a place where the air is solvent-free in order to reduce theproblem of contamination of the samples from their surroundings due to the low concentrations of residual solventsin the samples.NOTESamples should be in tightly packed roll form if possible. Sheet samples can be prepared from the roll by cutting outa square window (several layers of sheets) with a knife. At least the first five layers should be discarded. When in the form ofsheets they should be stacked tightly together to form a compact "block" and wrapped tightly in a barrier material, preferablyaluminium foil with a thickness of 30 µm to 40 µm. For storage periods of more than one hour the wrapped samples should bestored at temperatures below 5 °C and in an atmosphere free of volatile contaminants.7 Test specimens7.1 Specimen area in relation to vial volumeThe specimen area to be cut out shall depend on the vial volume and the level of residual solvents to bedetermined in the material. The ratio between the specimen area (in cm²) and the vial volume (in ml) shall bebetween three and five. The specimens shall be cut out using an appropriate template (5.5).NOTEAs an example for a vial with a volume of 6 ml to 9 ml a specimen of 30 cm² (2 cm × 15 cm) can be used orproportional dimensions for other volumes.7.2 Test specimens from sheetsFrom the top of the sample take a block of about 15 to 20 sheets out without separating them. Immediately putback the remaining part of the sample in its packaging under the conditions specified in clause 6.Prepare a first vial; after withdrawal of at least one layer (or more depending on the number of specimens to beprepared from the block) from the top of the block take the following sheet and rapidly cut the first specimen using atemplate (5.5). Coil the specimen rapidly and immediately put it into the vial. Crimp the vial immediately to seal it.Prepare further specimens in the same way.The following precautions shall be taken.The different steps of the preparation shall be done very rapidly to avoid evaporation of the solvents.The sample sheet from which the specimen is cut shall be taken out of the block immediately before preparation.The specimens shall always be cut at a defined place e.g. on the same drawing printed on the same place in thewidth and the template for cutting shall always be placed in the same manner.8 Incubation of the test specimens8.1 GeneralIncubation time and temperature shall be optimized for each individual system in order to achieve a partitionequilibrium of the residual solvents between the solid phase and the gas phase. With a certain temperatureselected an optimum heatin

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