SIST EN 13130-5:2004
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 5: Determination of vinylidene chloride in food simulants
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 5: Determination of vinylidene chloride in food simulants
This part of this European Standard specifies a method for the determination of vinylidene chloride monomer in food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil. The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of food simulant. The method is appropriate for the quantitative determination of vinylidene chloride at a level of 0,05 mg/kg.
NOTE This method was developed for the determination of vinylidene chloride in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out. However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 5: Bestimmung von Vinylidenchlorid in Prüflebensmitteln
Matériaux et objets en contact avec des denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 5 : Détermination du chlorure de vinylidene dans les simulants d'aliments alimentaires
La présente partie de la présente norme spécifie une méthode de détermination du monomere de chlorure de vinylidene dans les simulants d'aliments. La méthode s'applique aux simulants d'aliments aqueux, aux simulants d'aliments gras tels que l'huile d'olive et autres simulants gras, aux simulants D, par exemple un mélange de triglycérides synthétiques, huile de tournesol ou huile de mais. La concentration de chlorure de vinylidene déterminée est exprimée en milligrammes de chlorure de vinylidene par kilogramme de simulant d'aliment. La méthode convient a la détermination quantitative du chlorure de vinylidene a un niveau de 0,05 mg/kg.
NOTE Cette méthode a été élaborée pour déterminer la quantité de chlorure de vinylidene dans de l'éthanol aqueux a 15 % v/v, conformément aux réglementations en vigueur au moment ou le travail de mise au point a été effectué. Cependant, cette méthode, élaborée pour de l'éthanol aqueux a 15 % (v/v), devrait pouvoir s'appliquer a la détermination dans de l'éthanol aqueux a 10 % (v/v).
Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 5. del: Določevanje vinilidenklorida v modelnih raztopinah za živila
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 5: Bestimmung von Vinylidenchlorid in PrüflebensmittelnMatériaux et objets en contact avec des denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 5 : Détermination du chlorure de vinylidene dans les simulants d'aliments alimentairesMaterials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 5: Determination of vinylidene chloride in food simulants67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 13130-5:2004SIST EN 13130-5:2004en,fr,de01-september-2004SIST EN 13130-5:2004SLOVENSKI
STANDARDSIST ENV 13130-5:20001DGRPHãþD
SIST EN 13130-5:2004
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13130-5May 2004ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 5: Determination ofvinylidene chloride in food simulantsMatériaux et objets en contact avec des denréesalimentaires - Substances dans les matières plastiquessoumises à des limitations - Partie 5 : Détermination duchlorure de vinylidène dans les simulants d'alimentsalimentairesWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschränkungenunterliegen - Teil 5: Bestimmung von Vinylidenchlorid inKunststoffenThis European Standard was approved by CEN on 24 March 2004.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 Central Secretariat 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 Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13130-5:2004: ESIST EN 13130-5:2004
EN 13130-5:2004 (E) 2 Contents
page Foreword.3 1 Scope.6 2 Normative references.6 3 Principle.6 4 Reagents.6 4.1 Analyte and internal standard.7 4.1.1 Analyte.7 4.1.2 Internal standard.7 4.2 Chemicals.7 4.3 Solutions of standards and internal standard.7 4.3.1 Preparation of stock solutions of vinylidene chloride.7 4.3.2 Intermediate solutions of vinylidene chloride.7 4.3.3 Internal standard stock solution.7 4.3.4 Intermediate internal standard solution.7 5 Apparatus.8 6 Samples.9 6.1 Laboratory samples.9 6.2 Preparation of test samples.9 6.2.1 General.9 6.2.2 Aqueous food simulants.9 6.2.3 Fatty food simulant.9 6.3 Preparation of blank samples.9 6.4 Preparation of calibration samples.9 7 Procedure.10 8 Expression of results.10 8.1 Method of calculation.10 8.1.1 GC interferences.10 8.1.2 Graphical determination using internal standard.10 8.1.3 Graphical determination via external standardization.11 8.1.4 Calculation of the concentration using a response factor.11 8.1.5 Calculation of the specific migration.11 8.2 Precision.11 8.2.1 Validation.11 8.2.2 Repeatability and reproducibility.12 8.2.3 Detection limit.12 9 Confirmation.13 9.1 Requirement for confirmation.13 9.2 Confirmation by combined gas chromatography-mass spectrometry.13 9.3 Confirmation by analysis on a GC column of different polarity.13 10 Test report.13 Annex A (normative)
Method of standard addition.15 Annex B (normative)
Manual sample injection.17 Bibliography.18 SIST EN 13130-5:2004
EN 13130-5:2004 (E) 3 Foreword This document (EN 13130-5:2004) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which is held by BSI. This document was prepared by Subcommittee SC1 of TC 194 as one of a series of analytical test methods for plastics materials and articles in contact with foodstuffs. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2004, and conflicting national standards shall be withdrawn at the latest by November 2004. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This standard is intended to support Directives 2002/72/EC [1], 89/109/EEC [2], 82/711/EEC [3] and its amendments 93/8/EEC [4] and 97/48/EC [5], and 85/572/EEC [6]. At the time of preparation and publication of this part of EN 13130 the European Union legislation relating to plastics materials and articles intended to come into contact with foodstuffs is incomplete. Further Directives and amendments to existing Directives are expected which could change the legislative requirements which this standard supports. It is therefore strongly recommended that users of this standard refer to the latest relevant published Directive(s) before commencement of a test or tests described in this standard.
EN 13130-5 should be read in conjunction with EN 13130-1 Further parts of EN 13130, under the general title Materials and articles in contact with foodstuffs - Plastics substances subject to limitation, have been prepared, and others are in preparation, concerned with the determination of specific migration from plastics materials into foodstuffs and food simulants and the determination of specific monomers and additives in plastics. The other parts of
EN 13130 are as follows.
Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants Part 2: Determination of terephthalic acid in food simulants Part 3: Determination of acrylonitrile in food and food simulants Part 4: Determination of 1,3-butadiene in plastics Part 6: Determination of vinylidene chloride in plastics Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants Part 8: Determination of isocyanates in plastics Part 9: Determination of acetic acid, vinyl ester in food simulants Part 10: Determination of acrylamide in food simulants
Part 11: Determination of 11-aminoundecanoic acid in food simulants
Part 12: Determination of 1,3-benzenedimethanamine in food simulants Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants SIST EN 13130-5:2004
EN 13130-5:2004 (E) 4 Part 14:
Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants Part 15: Determination of 1,3-butadiene in food simulants
Part 16: Determination of caprolactam and caprolactam salt in food simulants Part 17: Determination of carbonyl chloride in plastics
Part 18: Determination of 1,2-dihydroxybenzene, 1,3- dihydroxybenzene, 1,4- dihydroxybenzene, 4,4’-dihydroxybenzophenone and 4,4’dihydroxybiphenyl in food simulants Part 19:
Determination of dimethylaminoethanol in food simulants Part 20:
Determination of epichlorohydrin in plastics Part 21:
Determination of ethylenediamine and hexamethylenediamine in food simulants Part 22:
Determination of ethylene oxide and propylene oxide in plastics Part 23:
Determination of formaldehyde and hexamethylenetetramine in food simulants Part 24:
Determination of maleic acid and maleic anhydride in food simulants Part 25: Determination of 4-methyl-pentene in food simulants Part 26: Determination of 1-octene and tetrahydrofuran in food simulants Part 27:
Determination of 2,4,6-triamino-1,3,5-triazine in food simulants Part 28:
Determination of 1,1,1-trimethylopropane in food simulants
Parts 1 to 8 are European Standards.
Parts 9 to 28 are Technical Specifications, prepared within the Standards, Measurement and Testing project, MAT1-CT92-0006, “Development of Methods of Analysis for Monomers”. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 13130-5:2004
EN 13130-5:2004 (E) 5 Introduction Vinylidene chloride (VdC) (1,1-dichloroethylene), H2C=CCl2, is a monomer used in the manufacture of certain plastics films and coatings intended to come into contact with foodstuffs.
During the manufacture of vinylidene chloride polymers and copolymers, residual vinylidene chloride monomer can remain in the polymer and can migrate into food coming into contact with the polymer. The method described in this part of the standard should be used in conjunction with part 1 of this standard which describes the procedures required prior to the determination of vinylidene chloride. SIST EN 13130-5:2004
EN 13130-5:2004 (E) 6
1 Scope This part of this European Standard specifies a method for the determination of vinylidene chloride monomer in food simulants.
The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil.
The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of food simulant.
The method is appropriate for the quantitative determination of vinylidene chloride at a level of 0,05 mg/kg. NOTE This method was developed for the determination of vinylidene chloride in 15 % (v/v) aqueous ethanol, as required by the regulations in force at the time the development work was carried out.
However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision.
For undated references the latest edition of the publication referred to applies (including amendments).
EN 13130-1:2004, Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants 3 Principle The level of vinylidene chloride in a food simulant is determined by headspace gas chromatography with automated sample injection and using either electron capture or flame ionization detection.
Quantification is achieved using 1-chloropropane (1-CP) as internal standard with calibration against blank samples of simulant fortified with vinylidene chloride.
If blank samples of simulant cannot be obtained then the method of standard addition described in annex A is employed.
If interferences are experienced with the internal standard then calibration is carried out by external standardization. If automated headspace sampling cannot be performed, manual injection as described in annex B shall be applied. Confirmation of vinylidene chloride levels is carried out either by combined gas chromatography/mass spectrometry (GC/MS) or by re-analysis on a second GC column of different polarity. 4 Reagents WARNING:
All chemicals are hazardous to health to a greater or lesser extent.
It is beyond the scope of this standard to give instructions for the safe handling of all chemicals, that meet, in full, the legal obligations in all countries in which this standard may be followed.
Therefore, specific warnings are not given and users of this standard shall ensure that they meet all the necessary safety requirements in their own country. SIST EN 13130-5:2004
EN 13130-5:2004 (E) 7 4.1 Analyte and internal standard 4.1.1 Analyte Vinylidene chloride (VdC), H2C=CCl2, of purity greater than 99 %. 4.1.2 Internal standard 1-Chloropropane (1-CP), CH3(CH2)2Cl, of purity greater than 98 %. 4.2 Chemicals N,N-dimethylacetamide (DMA), CH3CON(CH3)2, of purity greater than 99 %. 4.3 Solutions of standards and internal standard 4.3.1 Preparation of stock solutions of vinylidene chloride a) Stock solution of vinylidene chloride with a defined concentration of approximately 2,5 g/kg.
To a 20 ml flask or vial with cap, add 20 ml N,N-dimethylacetamide (4.2), close and weigh to an accuracy of 0,1 mg.
Add to the N,N-dimethylacetamide a quantity of approximately 40 µl (0,048g) vinylidene chloride (4.1.1) and shake the closed flask.
Weigh to an accuracy of 0,1 mg.
Determine the exact mass of vinylidene chloride added in grams per kilogram. b) Repeat item a) to provide a second stock solution. 4.3.2 Intermediate solutions of vinylidene chloride Intermediate solutions of vinylidene chloride in N,N-dimethylacetamide with defined concentrations in the range 5 mg/kg to 50 mg/kg are prepared as follows: a) To five 10 ml flasks or vials tared with cap, add 10 ml of N,N-dimethylacetamide and weigh to an accuracy of 0,1 mg.
Add respectively 20 µl, 50 µl, 100 µl, 150 µl and 200 µl of the 2,5 g/kg stock solution of vinylidene chloride (4.3.1a).
Cap, re-weigh to an accuracy of 0,1 mg and shake thoroughly.
b) Repeat item a) using the second stock solution prepared in 4.3.1 b) to provide a second set of five intermediate solutions of vinylidene chloride. NOTE The stock and intermediate solutions of vinylidene chloride, can be stored at - 20 °C for up to four weeks, protected from light.
Solutions should be stored in suitable glass, septum-capped vials, with minimal headspace volume. 4.3.3 Internal standard stock solution Prepare a stock solution of 1-chloropropane with a defined concentration of approximately 20 g/kg as follows: To a 10 ml flask or vial tared with cap, add 10 ml N,N-dimethylacetamide.
Close and weigh to an accuracy of 0,1 mg.
Add to the N,N-dimethylacetamide, approximately 0,20 ml of 1-chloropropane and shake the closed flask or vial.
Determine the exact mass of 1-chloropropane added by re-weighing to an accuracy of 0,1 mg. 4.3.4 Intermediate internal standard solution Prepare an intermediate solution of 1-chloropropane with a defined concentration of approximately 200 mg/kg as follows:
SIST EN 13130-5:2004
EN 13130-5:2004 (E) 8 To a 10 ml flask or vial tared with cap, add 10 ml N,N-dimethylacetamide and weigh to an accuracy of 0,1 mg.
Add 100 µl of 1-chloropropane stock solution (4.3.3).
Close, re-weigh to an accuracy of 0,1 mg and shake thoroughly to mix. 5 Apparatus NOTE An instrument or item of apparatus is listed only where it is special, or made to a particular specification, usual laboratory equipment being assumed to be available. 5.1 Gas-chromatograph, equipped with an electron capture detector (ECD) or flame ionization detector (FID) and fitted with an automated headspace sampler. 5.2 Gas-chromatographic column, capable of the separation of N,N-dimethylacetamide from vinylidene chloride and 1-chloropropane such that the peaks of vinylidene chloride and 1-chloropropane do not overlap by more than 1 % peak area with each other and with other compounds. NOTE 1 The following are examples of GC columns known to be suitable for vinylidene chloride analysis: a)
50 m x 0,32 mm internal diamete
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