prEN 1186-15

SLOVENSKI STANDARD
oSIST prEN 1186-15:2006
01-december-2006
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Materials and articles in contact with foodstuffs - Plastics - Part 15: Alternative test
methods to migration into fatty food simulants by rapid extraction into iso-octane and/or
95 % ethanol
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 15:
Alternative Prüfverfahren zur Migration in fettige Prüflebensmittel durch Schnellextraktion
in Iso-Octan und/oder 95%iges Ethanol
Matériaux et objets en contact avec les denrées alimentaires - Plastiques - Partie 15 :
Méthodes de remplacement pour la vérification de la migration dans les simulants gras
par extraction rapide dans l'iso-octane et/ou l'éthanol aqueux a 95 %
Ta slovenski standard je istoveten z: prEN 1186-15
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
oSIST prEN 1186-15:2006 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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EUROPEAN STANDARD
DRAFT
prEN 1186-15
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2006
ICS 67.250 Will supersede EN 1186-15:2002
English Version
Materials and articles in contact with foodstuffs - Plastics - Part
15: Alternative test methods to migration into fatty food
simulants by rapid extraction into iso-octane and/or 95 %
ethanol
Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires - Matière plastique - Partie 15 : Méthodes - Kunststoffe - Teil 15: Alternative Prüfverfahren zur
d'essai alternatives pour la migration dans les simulants Migration in fettige Prüflebensmittel durch Schnellextraktion
alimentaires gras par extraction rapide dans l'iso-octane in Iso-Octan und/oder 95%iges Ethanol
et/ou l'éthanol à 95 %
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.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
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 1186-15:2006: E
worldwide for CEN national Members.

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prEN 1186-15:2006 (E)
Contents Page
Foreword.3
1 Scope.5
2 Normative references.5
3 Method A Alternative test method to migration into fatty food simulants by rapid
extraction into iso-octane and/or 95 % ethanol by total immersion.6
3.1 Principle.6
3.2 Reagents.6
3.3 Apparatus.7
3.4 Preparation of test specimens .7
3.5 Procedure.8
3.6 Expression of results.10
3.7 Test report.10
4 Method B Alternative test method to migration into fatty food simulants by rapid
extraction into iso-octane and/or 95 % ethanol in the single side mode by cell .11
4.1 Principle.11
4.2 Reagents.11
4.3 Apparatus.11
4.4 Preparation of test specimens .12
4.5 Procedure.12
4.6 Expression of results.15
4.7 Test report.15
Annex A (informative) Precision data.16
Annex ZA (informative)  Relationship of this European Standard with Regulation 1935/2004 and
Commission Directive 2002/72/EC and associated Directives .17
Bibliography .19

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prEN 1186-15:2006 (E)
Foreword
This document (prEN 1186-15:2006) 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 1186-15:2002.
WARNING — Both iso-octane and ethanol are volatile flammable solvents. Take care to ensure that
the test specimens are well stoppered, closed and covered to prevent solvent volatilizing into the
interior of the oven, incubator or refrigerator and generating an explosive mixture. Care should be
taken at all times when handling these solvents to prevent contact with sources of ignition.
Read EN 1186-15 in conjunction with EN 1186-1.
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 simulants by article filling
Part 10 Test methods for overall migration into olive oil (modified method for use in cases where
incomplete extraction of olive oil occurs)
14
Part 11 Test methods for overall migration into mixtures of C-labelled synthetic triglyceride
Part 12 Test methods for overall migration at low temperatures
Part 13 Test method for overall migration at high temperatures
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prEN 1186-15:2006 (E)
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
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prEN 1186-15:2006 (E)
1 Scope
This European Standard specifies two alternative test methods, in the sense of an extraction test with a 'more
severe' test character, for the assessment of the overall migration into fatty food simulants.
Method A is based on the determination of the extraction of migrateable substances from plastics which are
intended to come into contact with foodstuffs, by total immersion in non-polar, iso-octane, and/or polar,
ethanol, solvents depending on the polarity of the packaging material. According to results obtained by this
method (see [1], [2], [3], [4], [5]) and taking physio-chemical considerations into account, the obtained
extraction efficiency has, generally, been found to be equivalent to or higher than overall migration results
obtained under the test conditions, 10 days at 40 °C, 2 h at 70 °C, 1 h at 100 °C, 30 min at 121 °C and 30 min
at 130 °C.
To ensure as complete as possible extraction of the potential migrants, a strong interaction, e.g. swelling, of
the sample by the extraction solvent is necessary. For this purpose, iso-octane is used as an extraction
solvent for plastics materials and articles containing non polar food contact layers, such as polyolefins. For
test samples made from polar food contact plastics such as polyamide and polyethylene terephthalate, 95 %
(v/v) aqueous ethanol is used. For polystyrenes, plasticized polyvinyl chloride and other polymers where the
identification or polarity of the polymer is not clear, two parallel extraction tests should be conducted using
both of the proposed extraction solvents and taking the higher value obtained as the relevant result.
NOTE 1 In case of multilayer structures such as plastics laminates and co-extruded plastics, the nature of the food
contact layer determines the selection of the extraction solvent(s).
This test method should only be applied to flexible packagings which are less than 300 µm in thickness. When
the result does not exceed the allowed overall migration limit then the material can be considered to be in
compliance with EC regulations. If the test result exceeds the allowed overall migration limit the following
options may be applied chronologically with respect to further migration testing:
1) single-sided extraction test using a cell, if technically feasible (see 15B of this standard);
2) conventional migration test using olive oil or other fatty food simulants;
NOTE 2 The overall migration limit is specified in Commission Directive 2002/72/EC [7] and the conditions of test in
Council Directive 82/711/EEC [8] and its subsequent amendments, [9], [10].
Method B is applicable in those cases where the total immersion test, EN 1186-15 Method 15A, yields total
extraction values that exceed the overall migration or may be technically unsuitable, i.e. in the case of
multilayer structures, such as plastics laminates and co-extruded films. This test method should primarily only
be applied to flexible packagings with a physical barrier layer (for instance of aluminium or other material to
prevent penetrative loss of extraction solvent) and which have a thinner food contact layer than 300 µm. If the
result does not exceed the allowed overall migration limit then the material can be considered to be in
compliance with EC regulations. If the test result exceeds the allowed overall migration limit then the following
option may be applied with respect to further migration testing:
- conventional migration test using olive oil or other fatty food simulants.
NOTE 3 Methods A and B are not applicable to test materials intended for applications over 130 °C.
NOTE 4 Test materials intended for applications over 70 °C should be checked for their physical suitability at the
intended time and temperature of use.
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
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prEN 1186-15:2006 (E)
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
ISO 648, Laboratory glassware - One mark pipettes
ISO 4788, Laboratory glassware - Graduated measuring cylinders
3 Method A
Alternative test method to migration into fatty food simulants by rapid extraction into
iso-octane and/or 95 % ethanol by total immersion
3.1 Principle
The migrateable substances extracted from a sample of the plastics is determined as the mass of non-volatile
residue after evaporation of the solvent following immersion. Test specimens of at least 1 dm² (single side
considered) are immersed in the extraction solvent for 24 h at 40 °C or 50 °C and then removed. The
extraction solvent is evaporated to dryness, the mass of the non-volatile residue is determined and expressed
as milligrams per square decimetre of surface area of the test specimen. The measured value is compared to
the EC-official overall migration limit and taking the analytical tolerance of this method (± 1 mg/dm²) into
account.
3.2 Reagents
NOTE For details of preparation and quality of these reagents, see clause 4 of EN 1186-1:2002.
3.2.1 Ethanol 95 % (v/v) in aqueous solution.
3.2.2 Iso-octane (2,2,4-trimethylpentane)
NOTE The extraction solvents given in 3.2.1 and 3.2.2 are selected according to the nature of the polymer test
sample as given by Table 1, see 3.5.1.
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prEN 1186-15:2006 (E)
3.3 Apparatus
3.3.1 Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens,
250 mm x 250 mm is suitable.
3.3.2 Tweezers, stainless steel, blunt nosed.
3.3.3 Cutting implement, scalpel, scissors or sharp knife or other suitable device.
3.3.4 Metal template, (100 mm ± 0,2 mm) x (100 mm ± 0,2 mm) (square).
3.3.5 Rule, graduated in mm, and with an accuracy of 0,1 mm.
3.3.6 Analytical balance capable of determining a change in mass of 0,1 mg.
3.3.7 Extraction containers; glass weighing jars with ground joints, tall form, of a capacity of approx. 60 ml.
3.3.8 Thermostatically controlled oven or incubator capable of maintaining a temperature within the
range of + 40 °C to + 50 °C and meeting temperature tolerance values within those specified for the test
temperature, see annex B of EN 1186-1:2002.
WARNING The interior / sample space of the oven or incubator should not have any exposed heating elements, to
minimise safety hazards arising from any loss of flammable test media during the test period.
3.3.9 Dishes, of stainless steel, nickel, platinum, platinum alloy or gold, 50 mm to 90 mm diameter and of
maximum mass 100 g, for evaporation of solvents and weighing of residues. Glass, glass ceramic, ceramic or
aluminium dishes may be used provided that their surface characteristics are such that the mass of the dishes
after evaporation of any specified solvent followed by conditioning in the desiccator used achieves a
constancy of
± 0,5 mg.
3.3.10 Steam bath, hot plate, distillation apparatus or rotary evaporator.
3.3.11 Desiccator with anhydrous calcium chloride or self indicating silica gel.
3.3.12 Measuring cylinder, 50 ml capacity, conforming to the minimum requirements of ISO 4788.
3.3.13 Round-bottom flask, 250 ml capacity [for distillation method (see 3.5.3.3) only].
3.4 Preparation of test specimens
3.4.1 General
It is essential that test specimens are clean and free from surface contamination (many plastics can readily
attract dust due to static charges). Before preparing test specimens, remove any surface contamination from
the sample by gently wiping it with a lint free cloth, or by brushing with a soft brush. Under no circumstances
wash the sample with water or solvent. If it is specified in the instructions for use of the article that it should be
washed or cleaned before use see 8.1 of EN 1186-1:2002. Minimize handling of the samples and where
necessary, wear cotton gloves.
To ensure that test pieces are well separated and that the surfaces are freely exposed to the extractant during
the period of the test, insert a piece of fine stainless steel gauze between the cut test pieces.
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prEN 1186-15:2006 (E)
3.4.2 Number of test specimens
Three replicate test specimens are required.
3.4.3 Cutting and preparation of specimen
Lay the sample on the cutting slab (3.3.1) and cut the test specimens of 1 dm² (see 8.3 of EN 1186-1:2002),
using the 100 mm x 100 mm template (3.3.4). Check, using the rule (3.3.5), that the dimensions of the
specimen are within the specified tolerance (1 mm). Fold the test specimens into a fan-like shape or cut into
strips approximately 2 cm wide and 5 cm long. Place in the extraction containers (3.3.7).
3.5 Procedure
3.5.1 Selection of extraction solvent
Select the appropriate extraction solvent(s) (see 3.2.1 and 3.2.2) according to the nature of the polymer test
sample as given in Table 1.
Table 1 — Use of extraction solvents and test conditions – Method A

Polymer type of food contact layer Extraction solvent to be Extraction conditions to be
applied applied

Polyolefines and copolymers iso-octane 24 h at 40 °C

Polyamides 95 % ethanol 24 h at 40 °C

Polystyrene iso-octane and 95 % ethanol 24 h at 40 °C

Polyethylene terephthalate 95 % ethanol 24 h at 50 °C

Polyvinyl chloride (plasticized) iso-octane and 95 % ethanol 24 h at 40 °C

Polyvinyl chloride (rigid) 95 % ethanol 24 h at 50 °C


3.5.2 Exposure to solvent
Take three extraction containers or jars (3.3.7), measure by measuring cylinder (3.3.12) 50 ml of the solvent
into each of these jars and immerse the test specimens in the solvent. Ensure that the test specimens are
totally immersed in the solvent. If the evaporation method is to be used (3.5.3.2) measure into a further two
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jars by measuring cylinder the same amount of solvent, plus 10 ml ± 2 ml, to provide blanks. If the distillation
method (3.5.3.3) is to be used measure into those further two jars by measuring cylinder the same amount of
solvent in contact with the test specimens to provide blanks. Stopper the jars. Mark the jars for identification.
Mark the liquid level on the outside of each jar with a suitable marker.
The extraction conditions are to be selected from Table 1 according to the nature of the polymer test samples.
Place the five jars in the thermostatically controlled oven or incubator (3.3.8), set at the test temperature and
observe the temperature, leave the jars for the test period of 24 h after the air bath of the thermostatically
controlled oven or incubator has reached the set temperature and taking the permitted time and temperature
tolerances into account (see annex B of EN 1186-1:2002). Take the jars from the oven or incubator and allow
them to cool down to room temperature. Check the level of solvent in each. If this has fallen to more than 5
mm below the mark, or has exposed any part of the test pieces, repeat the test using fresh test specimens. If
the level of solvent in a jar is less than 5 mm below the mark, remove the test specimen from the jar, and
allow the solvent adhering to the test specimen and support to drain back into the jar. Recover at least 90 % of
the original volume of solvent, including the blanks, or repeat the test.
WARNING Both iso-octane and ethanol are volatile flammable solvents. Care should be taken to avoid any loss of
solvent into the interior of the thermostatting device. Place the jars, if possible, in a drip container serving as a possible
solvent reservoir in case of leakage. Do not allow the temperature to exceed 60 °C.
3.5.3 Determination of extracted substances
3.5.3.1 Preparation of dishes
Take five dishes (3.3.9), marked for identification, place the dishes in an oven maintained at 105 °C to 110 °C,
for a period of 30 min ± 5 min, to dry. Remove the dishes from the oven, place in a desiccator and allow to
cool to ambient temperature. Weigh and record the individual masses of each dish. Replace the dishes in the
oven and repeat the cycle of heating, cooling and weighing until individual consecutive masses differ by not
more than
0,5 mg. Record their final masses.
3.5.3.2 Evaporation method
For each jar, including the two blank jars, containing the solvent, pour 20 ml to 25 ml into a prepared dish. By
means of a steam bath, hot plate or other form of heating evaporate to a low volume (3.3.10), taking care to
avoid loss of residue, in particular, by sputtering or overheating.
NOTE 1 The evaporation should be carried out in a fume cupboard.
When most of the solvent has evaporated, pour the remaining solvent from each of the jars into the respective
dishes and continue the evaporation. Rinse each of the jars which had contained test specimens with two lots
of  5 ml ± 1 ml of fresh solvent and pour these washings into the respective dishes.  Continue the
evaporation.
NOTE 2 A stream of nitrogen may be used to facilitate evaporation.
When the solvent has almost completely evaporated, place the dish in an oven maintained at 105 °C to
110 °C, for a period of 30 min ± 5 min, to complete the evaporation and dry the residue. Remove the dishes
from the oven, place in a desiccator (3.3.11) and allow to cool to ambient temperature. Weigh and record the
individual masses of each dish and residue. Replace the dishes in the oven and repeat the cycle of heating,
cooling and weighing until individual consecutive masses differ by not more than 0,5 mg. Determine the mass
of the residue by subtracting the original mass of the dish from the final mass of the dish and residue.
3.5.3.3 Distillation method
For each jar, transfer the contents to a round bottom flask (3.3.13). Rinse each jar twice, including the blank
jars, with 20 ml ± 2 ml of fresh solvent, add these rinses to the respective flasks. Place the flasks in an
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electric heating mantle and connect to a side arm distillation arrangement or rotary evaporator. Distil off the
solvents until approximately 15 ml to 25 ml remains in the flask. Transfer the remaining solvents to an
evaporating dish. Rinse the flask with 10 ml ± 1 ml of fresh solvent and add the rinses to the appropriate
dishes. Continue the evaporation of the solvent by means of a steam bath, hot plate or other form of heating,
proceeding as in 3.5.3.2.
NOTE The evaporation should be carried out in a fume cupboard.
3.6 Expression of results
3.6.1 Method of calculation
Express the extraction as milligrams of residue per square decimetre of the surface of the sample which is
intended to come into contact with foodstuffs, calculated for each test specimen using the following formula :

(m - m )
a b
M =
S
(1)
where
M is the total mass extracted into the solvent, in milligrams per square decimetre of surface area of
sample intended to come into contact with foodstuffs;
m is the mass of the residue from the test specimen after evaporation of the solvent in which it had
a
been immersed, in milligrams;
m is the mass of residue from the solvent from blank only, in milligrams;
b
S is the surface area of the test specimen, in square decimetres, see clause 8 of EN 1186-1:2002.
Calculate the result for each test specimen to the nearest 0,1 mg/dm² and the mean of the individual test
results, to the nearest 0,1 mg/dm².
In cases where both extraction solvents had to be applied (see Table 1), the higher value measured shall be
the relevant one.
3.6.2 Precision
See Annex A.
3.7 Test report
The test report shall include the following (see clause 11 of EN 1186-1:2002):
a) reference to this European Standard, to the Part and the method used for the test procedure;
b) all information necessary for complete identification of the sample such as chemical type, supplier,
trade mark, grade, batch number, thickness;
c) conditions of time and temperature of exposure to extractants;
d) departures from the specified procedure, and reasons for these;
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e) individual test results, and the mean of these, expressed as milligrams of residue per square decimetre
of sample;
f) relevant comments on the test results.
4 Method B
Alternative test method to migration into fatty food simulants by rapid extraction into
iso-octane and/or 95 % ethanol in the single side mode by cell
4.1 Principle
The total migrateable substances extracted from a sample of the plastics is determined as the mass of non-
volatile residue after evaporation of the solvent following immersion.
One surface of the test specimen of at least 1 dm² (single side considered) is exposed in a cell to the
extraction solvent for 24 h at 40 °C or 50 °C and then removed. The extraction solvent is evaporated to
dryness, the mass of the non-volatile residue is determined and expressed as milligrams per square
decimetre of surface area of the test specimen. The measured value is compared to the EC-official overall
migration limit and taking the analytical tolerance of this method (± 1 mg/dm²) into account.
4.2 Reagents
NOTE For details of preparation and quality of these reagents, see clause 4 of EN 1186-1:2002.
4.2.1 Ethanol 95 % (v/v) in aqueous solution.
4.2.2 Iso-octane (2,2,4-trimethylpentane)
The extraction solvents given in 4.2.1 and 4.2.2 are to be selected according to the nature of the polymer test
sample as given in Table 2, see 4.5.1.
4.3 Apparatus
4.3.1 Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens,
250 mm x 250 mm is suitable.
4.3.2 Tweezers, stainless steel, blunt nosed.
4.3.3 Cutting implement, scalpel, scissors or sharp knife or other suitable device.
4.3.4 Analytical balance capable of determining a change in mass of 0,1 mg.
4.3.5 Cell, type A as shown in Figure C.3 of EN 1186-1:2002, either the aluminium (anodized) cells or the
cells with the stainless steel (316 grade) lids and rings, are suitable for the extraction solvents or equivalent
cells.
NOTE For details of equivalent cells see 7.3 of EN 1186-1:2002.
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4.3.6 Glass tubes, ground neck, and stoppers, for retaining the food simulant.
4.3.7 Pipettes, conforming to the minimum requirements of ISO 648, 50 ml and 100 ml.
4.3.8 Thermostatically controlled oven or incubator capable of maintaining a temperature within the
range of + 40 °C to + 50 °C and meeting temperature tolerance values within those specified for the test
temperature, see annex B of EN 1186-1:2002.
WARNING The interior/sample space of the oven or incubator should not have any exposed heating elements, to
minimize safety hazards arising from any loss of flammable test media during the test period.
4.3.9 Dishes, of stainless steel, nickel, platinum, platinum alloy or gold 50 mm to 90 mm diameter and
maximum mass 100 g, for evaporation of solvent
...