EN 1186-10

BRITISH STANDARD BS EN 1186-10:2002 Materials and articles in contact with foodstuffs — Plastics — Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) The European Standard EN 1186-10:2002 has the status of a British Standard ICS 67.250 ����������� � ��� � ������������������� ��������� ��� ���������� ��� Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. --`,,,,`,,`,,,,,,,``,`,,,``,``-`-`,,`,,`,`,,`--- BS EN 1186-10:2002 This British Standard, 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 14 October 2002 © BSI 14 October 2002 ISBN 0 580 40573 7 National foreword This British Standard is the official English language version of EN 1186-10:2002. It supersedes DD ENV 1186-10:1994 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials and articles in contact with foodstuffs, to Subcommittee CW/47/1, Migration from plastics, which has the responsibility to: A list of organizations 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 Correspondence 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 itself 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 promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 13 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. --`,,,,`,,`,,,,,,,``,`,,,``,``-`-`,,`,,`,`,,`--- EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN 1186-10 September 2002 ICS 67.250 English version Materials and articles in contact with foodstuffs - Plastics - Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) Matériaux et objets en contact avec les denrées alimentaires - Matière plastique - Partie 10: Méthodes d'essai pour la migration globale dans l'huile d'olive (méthode modifiée à utiliser en cas d'extraction incomplète de l'huile d'olive) Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 10: Prüfverfahren für die Gesamtmigration in Olivenöl (Modifiziertes Verfahren für die Andwendung bei unvollständiger Extraktion von Olivenöl) This European Standard was approved by CEN on 2 May 2002. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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 translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. 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 STANDARDIZATION C O M I T É E U R O P É E N D E N O R M A LI S A T I O N EUR OP ÄIS C HES KOM ITEE FÜR NOR M UNG Management Centre: rue de Stassart, 36 B-1050 Brussels © 2002 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1186-10:2002 E Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. - - ` , , , , ` , , ` , , , , , , , ` ` , ` , , , ` ` , ` ` - ` - ` , , ` , , ` , ` , , ` - - - EN 1186-10:2002 (E) 2 Contents page Foreword......................................................................................................................................................................3 1 Scope ..............................................................................................................................................................4 2 Normative references ....................................................................................................................................4 3 Principle ..........................................................................................................................................................5 4 Reagents .........................................................................................................................................................5 5 Apparatus .......................................................................................................................................................6 6 Preparation of test specimens......................................................................................................................6 7 Procedure .......................................................................................................................................................6 7.1 General............................................................................................................................................................6 7.2 Initial weighing of test specimens................................................................................................................6 7.3 Exposure to food simulant............................................................................................................................6 7.4 Final weighing of test specimens.................................................................................................................6 7.5 Extraction of absorbed olive oil ...................................................................................................................6 7.6 Determination of extracted olive oil .............................................................................................................7 7.6.1 Preparation of fatty acid methyl esters .......................................................................................................7 7.6.2 Determination of fatty acid methyl esters ...................................................................................................8 8 Expression of results ....................................................................................................................................8 8.1 Method of calculation ....................................................................................................................................8 8.2 Precision .........................................................................................................................................................8 9 Test report ......................................................................................................................................................8 Annex A (normative) Determination of the suitability of olive oil as the fatty food simulant and of triheptadecanoin as the internal standard ..................................................................................................9 A.1 Principle ..........................................................................................................................................................9 A.2 Procedure .......................................................................................................................................................9 A.3 Conclusions....................................................................................................................................................9 Annex B (informative) Precision ..............................................................................................................................10 Annex ZA (informative) Relationship of this European Standard with Council Directive 89/109/EEC and Commission Directive 90/128/EEC and associated Directives ...............................................................11 Bibliography ..............................................................................................................................................................13 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. - - ` , , , , ` , , ` , , , , , , , ` ` , ` , , , ` ` , ` ` - ` - ` , , ` , , ` , ` , , ` - - - EN 1186-10:2002 (E) 3 Foreword This document EN 1186-10:2002 has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which is held by BSI. 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 March 2003, and conflicting national standards shall be withdrawn at the latest by March 2003. This document supersedes ENV 1186-10:1994. This European Standard has been prepared as one of a series of methods of test for plastics materials and articles in contact with foodstuffs. This Part of this European Standard has been prepared by a Subcommittee (SC1) of TC 194 'Utensils in contact with food' as one of a series of methods of test for plastics materials and articles in contact with foodstuffs. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. For relationship with EU Directive(s), see informative annex ZA, which is an integral part of this document. At the time of preparation and publication of this standard 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 any of the test or tests described in this standard. EN 1186-10 should be read in conjunction with EN 1186-1, EN 1186-2, EN 1186-4, EN 1186-6, EN 1186-8, prEN 1186-12 and EN 1186-13. Further Parts of this standard have been prepared concerned with the determination of overall migration from plastics materials into food simulants. Their titles are as follows: EN 1186 Materials and articles in contact with foodstuffs – Plastics – Part 1 Guide to the selection of conditions and test methods for overall migration Part 2 Test methods for overall migration into olive oil by total immersion Part 3 Test methods for overall migration into aqueous food simulants by total immersion Part 4 Test methods for overall migration into olive oil by cell Part 5 Test methods for overall migration into aqueous food simulants by cell Part 6 Test methods for overall migration into olive oil using a pouch Part 7 Test methods for overall migration into aqueous food simulants using a pouch Part 8 Test methods for overall migration into olive oil by article filling Part 9 Test methods for overall migration into aqueous food simulants by article filling Part 11 Test methods for overall migration into mixtures of 14C-labelled synthetic triglyceride Part 12 Test methods for overall migration at low temperatures Part 13 Test methods for overall migration at high temperatures Part 14 Test methods for 'substitute tests' for overall migration from plastics intended to come into Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. - - ` , , , , ` , , ` , , , , , , , ` ` , ` , , , ` ` , ` ` - ` - ` , , ` , , ` , ` , , ` - - - EN 1186-10:2002 (E) 4 contact with fatty foodstuffs using test media iso-octane and 95 % ethanol Part 15 Alternative test methods to migration into fatty food simulants by rapid extraction into iso- octane and/or 95 % ethanol Annex A of this standard is normative where applicable. Annex B is informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries 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. 1 Scope This European Standard specifies test methods for the determination of the overall migration into fatty food simulants from plastics materials and articles, by total immersion of test specimens in a fatty food simulant at any temperatures above 5 ° C up to and including 175 ° C for selected times. When some plastics are tested by the methods in EN 1186-2, EN 1186-4, EN 1186-6, EN 1186-8, prEN 1186-12 and EN 1186-13, the soxhlet extraction process does not achieve complete recovery of the absorbed olive oil from the test specimens. In this method, the olive oil is released from the plastics test specimens by dissolving them in chloroform, toluene, xylene or tetrahydrofuran. This method is suitable for plastics when exposure to olive oil is by total immersion as described in EN 1186-2, in a cell, as described in EN 1186-4, in a pouch, as described in EN 1186-6, and by filling, as described in EN 1186-8 and to tests carried out at low and high temperature, as described in prEN 1186-12 and EN 1186-13. This is provided the plastics are soluble in chloroform, toluene, xylene or tetrahydrofuran and insoluble in methanol and that whenever prEN 1186-2 is referred to in this method the appropriate clause of the relevant part of EN 1186 is substituted. The method can also be suitable for plastics which are only partially soluble in chloroform, toluene, xylene or tetrahydrofuran and insoluble in methanol. NOTE 1 This test method has been written for use with the fatty food simulant, olive oil. The test method can also be used with appropriate modifications with 'other fatty food simulants' called simulant D - a synthetic mixture of triglycerides, sunflower oil and corn oil. These other fatty food simulants will produce different chromatograms for the simulant methyl esters to those of the methyl esters of olive oil. Select suitable chromatogram peaks of the methyl esters of the other fatty food simulants for the quantitative determination of the simulant extracted from the test specimens. NOTE 2 If it has been established that the overall migration into olive oil from the plastics cannot be determined by use of either this method or the methods described in EN 1186-2, EN 1186-4, EN 1186-6 and EN 1186-8 then the use of substitute tests should be considered, see clause 6 of EN 1186-1:2001. 2 Normative references This European Standard incorporates by dated and 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 and 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 (including amendments). EN 1186-1:2002, Materials and articles in contact with foodstuffs – Plastics – Part 1: Guide to the selection of conditions and test methods for overall migration. EN 1186-2:2002, Materials and articles in contact with foodstuffs – Plastics – Part 2: Test methods for overall migration into olive oil by total immersion. Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 00:38:52 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295. - - ` , , , , ` , , ` , , , , , , , ` ` , ` , , , ` ` , ` ` - ` - ` , , ` , , ` , ` , , ` - - - EN 1186-10:2002 (E) 5 3 Principle The overall migration from a sample of the plastic, such as polystyrene, is determined as the loss in mass of specimens after immersion in olive oil. The selection of the test conditions will be determined by the conditions of use, see clauses 4, 5 and 6 of EN 1186-1:2002. Test specimens of known mass are exposed to olive oil for the exposure time, at temperatures varying from 5 ° C to 175 ° C, then taken from the olive oil, blotted to remove oil adhering to the surface, and reweighed. The specimens will usually retain absorbed olive oil which is extracted by a dissolution and precipitation procedure and determined quantitatively by gas chromatography, after conversion to methyl esters. Methylation is carried out by reacting a boron trifluoride/methanol complex with fatty acids formed by hydrolysing the oil with potassium hydroxide. In case the plastic does not dissolve completely, swelling of the plastic in the solvent should be such that the olive oil absorbed can be released from the plastic. Depending on the type of plastic an appropriate organic solvent is selected in order to dissolve or swell the plastic. For chloroform soluble plastics like polystyrene and polycarbonate, chloroform is used to release the olive oil absorbed. For polyolefins, toluene and xylene are used as low density polyethylene shows good solubility in toluene and high density polyethylene and polypropylene dissolve or swell sufficiently in xylene. For polyvinylchloride or polyvinylidene chloride, tetrahydrofuran can be applied. Overall migration into the olive oil is calculated by subtracting the mass of olive oil retained by the test specimen from the mass of the test specimen after removal from the olive oil, and then subtracting this mass from the initial mass of the t