oSIST prEN 1186-13:2006

SLOVENSKI STANDARD
01-december-2006
Materiali in predmeti v stiku z živili - Polimerni materiali - 13. del: Preskusna
metoda za celotno migracijo pri visokih temperaturah
Materials and articles in contact with foodstuffs - Plastics - Part 13: Test method for
overall migration at high temperatures
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 13:
Prüfverfahren für die Gesamtmigration bei hohen Temperaturen
Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie
13 : Méthodes d'essai pour la migration globale a températures élevées
Ta slovenski standard je istoveten z: prEN 1186-13
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
DRAFT
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2006
ICS 67.250 Will supersede EN 1186-13:2002
English Version
Materials and articles in contact with foodstuffs - Plastics - Part
13: Test method for overall migration at high temperatures
Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires - Matière plastique - Partie 13 : Méthodes - Kunststoffe - Teil 13: Prüfverfahren für die
d'essai pour la migration globale à hautes températures Gesamtmigration bei hohen Temperaturen
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/TC 194.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
: This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
Warning
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 1186-13:2006: E
worldwide for CEN national Members.

Contents Page
Foreword.3
Introduction .5
1 Scope.6
2 Normative references.6
3 Method A – total immersion in olive oil.6
3.1 Principle.6
3.2 Reagents.7
3.3 Apparatus.7
3.4 Preparation of test specimens .7
3.5 Procedure.7
3.6 Expression of results.9
3.7 Test report.10
4 Method B – adsorption by modified polyphenylene oxide.10
4.1 Principle.10
4.2 Reagents.10
4.3 Apparatus.11
4.4 Sample preparation.11
4.5 Procedure.12
4.6 Expression of results.15
4.7 Test report.15
Annex A (informative)  Aluminium block .17
Annex B (informative)  Precision data.18
Annex ZA (informative)  Relationship of this European Standard with Regulation 1935/2004 and
Commission Directive 2002/75/EC and associated Directives .19
Bibliography .21

Foreword
This document (prEN 1186-13:2006) has been prepared by Technical Committee CEN/TC 194 “Utensils in
contact with food”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association, and supports essential requirements of EU Directive(s).
For relationship with EU Directive(s), see informative Annex ZA, which is an integral part of this document.
This document will supersede EN 1186-13:2002.
This European Standard has been prepared as one of a series of methods of test for plastics materials and
articles in contact with foodstuffs.
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 1186-13 Method A and Method B should be read in conjunction with EN 1186-1. Also, EN 1186-13
Method A should be read in conjunction with EN 1186-2.
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 10 Test methods for overall migration into olive oil (modified method for use in case where
incomplete extraction of olive oil occurs)
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 14 Test methods for 'substitute tests' for overall migration from plastics intended to come into
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
Introduction
Migration testing with olive oil at high temperatures introduces a number of analytical difficulties. Experience
has shown that it is difficult to achieve reproducible results owing to different laboratories having different
equipment which give rise to variations in the time taken to reach the exposure temperature. A method is
described for determining overall migration by total immersion using an aluminium block with a consistent
thermal capacity. Other analytical difficulties with olive oil include possible oxidation of oil at elevated
temperatures and the hazard to personnel working with hot oil. Replacement of olive oil by an appropriate
adsorbent material, in principal, can solve or reduce these problems and offers further experimental
advantages.
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
temperatures from 100 °C up to and including, 175 °C for selected times. Also described is a procedure with
a substitute test medium. In this substitute procedure the mass of components adsorbed on modified
polyphenylene oxide (MPPO) is taken as a measure for the assessment of the overall migration into olive oil.
NOTE 1 The total immersion 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 A comparative migration test carried out with polypropylene and polyethylene terephthalate high temperature
application containers as test samples at conditions 2 h at 100 °C and 2 h at 175 °C, respectively, in contact with C-
labelled synthetic triglyceride and MPPO provided test results comparable within the analytical tolerance of the methods.
NOTE 3 To obtain reproducible and repeatable results using the MPPO method it may be necessary to measure the
temperature of the test specimen before starting the migration period. An appropriate method for measuring the
temperature of the test specimen needs to be established.
The described methods are most suitable for food contact articles in the form of sheets and films, but can also
be applied to a wide range of articles and containers.
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 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
3 Method A – total immersion in olive oil
3.1 Principle
The overall migration from a sample of the plastics is determined as the loss in mass per unit of surface area
intended to come into contact with foodstuffs.
The selection of the conditions of test 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 immersed in olive oil for the exposure time, at temperatures from 100 °C
up 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 and determined quantitatively by
means of 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. An
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