SIST EN 13130-2:2004
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 2: Determination of terephthalic acid in food simulants
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 2: Determination of terephthalic acid in food simulants
This part of this European Standard specifies methods for the determination of the monomer terephthalic acid in food simulants; distilled water, 3 % w/v acetic acid aqueous solution, 15 % v/v ethanol aqueous solution and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil. The methods are capable of determining terephthalic acid in the food simulants at the level of the specific migration limit of 7,5 mg of terephthalic acid per kilogram of food simulants.
NOTE This method was developed for the determination of terephthalic acid 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 2: Bestimmung von Terephtalsäure in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 2 : Détermination de l'acide téréphtalique dans les simulants d'aliments
La présente partie de cette Norme européenne spécifie les méthodes de détermination de l'acide téréphtalique monomere dans les simulants d'aliments : eau distillée, solution aqueuse d'acide acétique a 3 % (m/v), solution aqueuse d'éthanol a 15 % (v/v) et huile d'olive et autres simulants d'aliments gras, simulants D (mélange de triglycérides synthétiques, huile de tournesol ou huile de mais par exemple). Ces méthodes permettent de déterminer l'acide téréphtalique dans les simulants alimentaires au niveau de la limite de migration spécifique, qui s'éleve a 7,5 mg d'acide téréphtalique par kilogramme de simulants d'aliments.
NOTE Cette méthode a été élaborée pour déterminer la quantité d'acide téréphtalique présente 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 - 2. del: Določevanje tereftalne kisline 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 2: Bestimmung von Terephtalsäure in PrüflebensmittelnMatériaux et objets en contact avec les denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 2 : Détermination de l'acide téréphtalique dans les simulants d'alimentsMaterials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 2: Determination of terephthalic acid in food simulants67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 13130-2:2004SIST EN 13130-2:2004en,fr,de01-september-2004SIST EN 13130-2:2004SLOVENSKI
STANDARDSIST ENV 13130-2:20001DGRPHãþD
SIST EN 13130-2:2004
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13130-2May 2004ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 2: Determination ofterephthalic acid in food simulantsMatériaux et objets en contact avec les denréesalimentaires - Substances dans les matières plastiquessoumises à des limitations - Partie 2 : Détermination del'acide téréphtalique dans les simulants d'alimentsWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschränkungenunterliegen - Teil 2: Bestimmung von Terephtalsäure inPrüflebensmittelnThis 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 13130-2:2004: ESIST EN 13130-2:2004
EN 13130-2:2004 (E) 2 Contents
Foreword.3 1 Scope.6 2 Normative references.6 3 Principle.6 4 Reagents.6 5 Apparatus.7 6 Samples.8 7 Procedure.8 7.1 Preparation of standards.8 7.2 Preparation of calibration graphs.9 7.3 Validation of preparation of standard solutions.9 7.4 Suitability of orthophthalic acid as an internal standard.9 7.5 Extraction of olive oil simulant migration test samples.9 7.6 Preparation of aqueous simulant migration samples.10 7.7 Injection of samples.10 8 Expression of results.10 8.1 Method of calculation.10 8.2 Precision.10 9 Confirmation of terephthalic acid.12 9.1 Requirement for confirmation.12 9.2 Re-analysis using an ion exchange column.12 9.3 Multi-wavelength measurements/diode array spectra analysis.12 10 Test report.13 Annex A (normative) Reagents for confirmation of terephthalic acid.14 A.1 Reagents for confirmation of terephthalic acid.14 Bibliography.15
SIST EN 13130-2:2004
EN 13130-2:2004 (E) 3 Foreword This document (EN 13130-2:2004) 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 13130-2 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 3: Determination of acrylonitrile in food and food simulants Part 4: Determination of 1,3-butadiene in plastics
Part 5: Determination of vinylidene chloride in food simulants 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
SIST EN 13130-2:2004
EN 13130-2:2004 (E) 4 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 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 13130-2:2004
EN 13130-2:2004 (E) 5 Introduction Terephthalic acid (TA) is a comonomer used in the manufacture of polyester plastics.
Residues of terephthalic acid can be present in the plastics after processing to form materials and articles intended to come into contact with foodstuffs.
When these plastics are in contact with foodstuffs, the residual terephthalic acid monomer can migrate into the foodstuff. SIST EN 13130-2:2004
EN 13130-2:2004 (E) 6
1 Scope This part of this European Standard specifies methods for the determination of the monomer terephthalic acid in food simulants; distilled water, 3 % (w/v) acetic acid aqueous solution, 15 % (v/v) ethanol aqueous solution and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil.
The methods are capable of determining terephthalic acid in the food simulants at the level of the specific migration limit of 7,5 mg of terephthalic acid per kilogram of food simulants.
NOTE This method was developed for the determination of terephthalic acid 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 EN ISO 1042; Laboratory glassware – One-mark volumetric flasks (ISO 1042:1998). ISO 385 (all parts); Laboratory glassware – Burettes. ISO 648; Laboratory glassware – One-mark pipettes. ISO 835 (all parts); Laboratory glassware – Graduated pipettes. ISO 4788, Laboratory glassware – Graduated measuring cylinders. 3 Principle The aqueous simulant test samples are directly analysed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection.
The olive oil test samples are extracted with dilute sodium hydrogen carbonate and the resultant aqueous solution is acidified and analysed by HPLC. 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 can 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. NOTE During the analysis, unless otherwise stated, only reagents of recognized analytical grade and only distilled water of equivalent purity should be used. SIST EN 13130-2:2004
EN 13130-2:2004 (E) 7 4.1 Methanol (HPLC grade).
4.2 Sodium acetate, trihydrate.
4.3 Orthophthalic acid.
4.4 Terephthalic acid.
4.5 Orthophosphoric acid 85 % (w/v). 4.6 Water (HPLC grade). 4.7 Sodium hydrogen carbonate solution 0,1 % (w/v). 4.8 Acetic acid, 50 % (v/v) in water.
4.9 Propan-2-ol. 4.10 Heptane. 4.11 pH 3,6 buffer solution.
Dissolve 25,0 g of sodium acetate, trihydrate in 350 ml of water, add 5,0 ml ± 0,1 ml of orthophosphoric acid and adjust to pH (3,6 ± 0,2) with glacial acetic acid (approximately 50 ml).
Make up to 500 ml with water. 4.12 Weigh accurately about 0,05 g terephthalic acid and, by continuous stirring, dissolve in about 90 ml of methanol.
Make up to 100 ml with methanol in a volumetric flask.
Prepare a second terephthalic acid standard stock solution for validation purposes, see 7.3.
NOTE The solution can be warmed to 50 °C to facilitate dissolution of the terephthalic acid, which takes at least 1 h. 4.13 Orthophthalic acid internal standard stock solution.
Weigh about 0,1 g of orthophthalic acid and dissolve in propan-2-ol.
Make up to 100 ml with propan-2-ol in a volumetric flask.
4.14 Mobile phase for high performance liquid chromatography.
Using a measuring cylinder add 150 ml of methanol to 150 ml of pH 3,6 buffer and dilute to 1 l with water.
NOTE Degassing the mobile phase can be necessary with some HPLC equipment.
5 Apparatus 5.1 Analytical balance capable of weighing accurately to 0,1 mg. 5.2 pH meter with an accuracy of ± pH 0,1. 5.3 Volumetric flasks, of 25 ml, 50 ml and 100 ml capacity, conforming to the minimum requirements of EN ISO 1042. 5.4 Measuring cylinders, of 5 ml, 25 ml, 50 ml, 100 ml and 250 ml capacity, conforming to the minimum requirements of ISO 4788. 5.5 Pipettes, of 5 ml and 50 ml capacity, conforming to the minimum requirements of ISO 648. 5.6 Graduated pipette, of 2 ml capacity, conforming to the minimum requirements of ISO 835. SIST EN 13130-2:2004
EN 13130-2:2004 (E) 8 5.7 Separating funnels, of 250 ml capacity. 5.8 Glass syringe, of 50 ml capacity. 5.9 Octadecylsilyl silica (ODS) 400 mg, C18 reverse phase disposable cartridges. 5.10 HPLC 0,2 µm membrane filters. 5.11 Burette, of 25 ml capacity, conforming to the minimum requirements of ISO 385. 5.12 High performance liquid chromatograph with a 10 µl injection loop, and a variable wavelength UV detector, set to 242 nm, connected to a strip chart recorder or integrator.
The column shall be capable of fully resolving terephthalic acid from orthophthalic acid, isophthalic acid and peaks arising from injection media.
NOTE The following column has been found to be suitable: ODS 5 µm 250 mm x 4,6 mm column, with a pre-column.
With a flow rate of 1,
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