prEN 1186-2

SLOVENSKI STANDARD
oSIST prEN 1186-2:2020
01-april-2020

Materiali in predmeti v stiku z živili - Polimerni materiali - 2. del: Preskusne metode

Materials and articles in contact with foodstuffs - Plastics - Part 2: Test methods for

Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

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 CEN-CENELEC

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 1186-2:2020 E

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Test methods .................................................................................................................................................... 5

4.1 Principle ............................................................................................................................................................. 5

4.2 Reagents ............................................................................................................................................................. 6

4.3 Materials and apparatus ............................................................................................................................... 7

4.4 Preparation of test specimens ................................................................................................................. 10

4.5 Procedure........................................................................................................................................................ 13

4.6 Expression of results ................................................................................................................................... 22

5 Test report ...................................................................................................................................................... 24

Annex A (normative) Contact time and temperature tolerances............................................................. 26

Annex B (normative) Determination of the suitability of oil as the fatty food simulant and of

triheptadecanoin as the internal standard ......................................................................................... 28

Annex C (normative) Determination of the need for sample conditioning .......................................... 30

determination of the mass of moisture sensitive test specimens, by cacuum drying ......... 31

Annex E (informative) Typical chromatograms and calibration graph ................................................ 33

Annex F (informative) Precision data ................................................................................................................ 36

Bibliography ................................................................................................................................................................. 37

This document (prEN 1186-2:2020) has been prepared by Technical Committee CEN/TC 194 “Utensils

This document implements European Commission Regulation on plastic materials and articles intended

to come into contact with food with regards to the determination of the overall migration in food

simulants. This regulatory text is subject to change it is therefore strongly recommended that users of

this document refer to the latest relevant published regulatory texts before commencement of any of the

test or tests described in this document, looking to the European Commission website.

This document will supersede EN 1186-2:2002, EN 1186-4:2002, EN 1186-6:2002, EN 1186-8:2002,

This document specifies methods for measuring overall migration of plastic materials and articles

intended to come into contact with foodstuffs by contacting test specimens with vegetable oils at

The overall migration from a sample of the plastics is determined as the loss in mass of non-volatile

According to the type of materials or articles, contact with the food simulant is carried out on a single

This document does not cover the interpretation of the results which is expected to account for regulatory

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

EN ISO 8442-2:1997, Materials and articles in contact with foodstuffs — Cutlery and table hollowware —

Note 1 to entry: Only terms not included in European Commission regulation on plastic materials are defined

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

thermostatically controlled heat chamber where the air within is heated and this heat is then transferred

to the food through the plastic as opposed to a microwave oven where the food itself is heated directly

receptacle of a defined size, manufactured in the film under test and which, once filled with food simulant,

exposes the side of the film to be in contact with foodstuffs to such a food simulant or to a test medium

pouch manufactured such that the surface to be in contact with foodstuffs is the outer surface

Note 1 to entry: All sides are sealed to prevent inner surfaces from coming into contact with the food simulant.

The reverse pouch is to be completely immersed in the food simulant or in the test medium.

device in which the film under test can be mounted and which, when assembled and filled with food

simulant, exposes the side of the film to be in contact with foodstuffs to such a food simulant or to a test

The overall migration of a material or a ready-to-use article made of plastic in contact with fatty foods,

for which vegetable oils must be used, is determined by putting test specimens in contact with a vegetable

oil in test conditions chosen on the basis of the worst case scenario of use, by weighing test specimens

before and after contact with the vegetable oil, by dosing the oil absorbed by the material by gas

Test specimens of known mass are placed in contact with oil for the exposure time, at temperatures above

4 °C and below 175 °C, then taken from the oil, drained and wiped to remove oil adhering to the surface,

The specimens will usually retain absorbed oil that 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 hydrolyzing the oil with potassium hydroxide.

An internal standard, triheptadecanoin, is added prior to the extraction of the absorbed oil from the test

specimens. This ensures that any active or extractable components of the plastics react with the internal

standard, as well as with the extracted oil. The internal standard is also subjected to the hydrolysis and

methylation reactions, providing compensation for any inefficiencies in the hydrolysis and methylation

Migration into the oil is calculated by subtracting the mass of oil retained by the test specimen from the

mass of the test specimen after removing the oil, then subtracting this mass from the initial mass of the

The total loss in mass is expressed in milligrams per square decimetre of surface area of the test specimen

or in milligrams per kg of oil or in milligrams per article and the overall migration is reported as the mean

According to the type of sample, the tests are conducted based on one of the following contacting methods

at a temperature greater than or equal to 4 °C and less than or equal to 175 °C and for the specified

NOTE In some vegetable oils, this method is also suitable for temperatures above 175 °C. The suitability of

Test specimens of known mass and surface are immersed in oil; this method is most suitable for plastics

in the form of films and sheets, but can also be applied to a wide range of articles or containers from which

Test specimens of known mass are placed in contact with oil in a cell; this method is most suitable for

plastics in the form of films or sheets in which only one surface is to be in contact with foodstuffs (printed,

Test specimens of known mass and in the form of pouches are filled with oil; this method is suitable for

plastics in the form of films or sheets in which the surface to be in contact with foodstuffs (printed, multi-

Test specimens of known mass and in the form of reverse pouches are immersed in oil; this method is

suitable for plastics in the form of films or sheets in which both surfaces can be sealed by applying heat

or pressure to form reverse pouches. This method, whenever possible, shall be preferred over those using

fillable pouches when the oil temperature is above 70°C due to the pressure from the oil that may damage

Test specimens of known mass are filled with oil; this method is suitable for plastics in the form of

containers and articles that can be filled. Testing samples by this method enables testing of non-

homogeneous articles provided they are not too large. If the article is large, to avoid handling and

weighing problems or using excessive amounts of oil, it may be preferable to cut it

4.2.2 Oil: Vegetable oils used as simulant shall be rectified and contain less than 1 % of unsaponifiable

4.2.3.1 Pentane is the solvent recommended for the first extraction for all type of plastic materials.

4.2.3.3 A 95/5 by volume azeotropic mixture of pentane 98 % and ethanol 96 % is the solvent

NOTE 1 Due to the low boiling points of these solvents, cooled condenser water can be required to prevent undue

4.2.4 Triheptadecanoin (glyceryl trimargarate) CAS No. 2438-40-6 solution, 2 mg/ml in cyclohexane

NOTE Other internal standards can be used, such methyl cinnamate (CAS: 103–26–4) or glyceryl

The constituent materials of the materials and apparatus used and the condition thereof shall make it

possible to prevent contamination of the samples, reagents and solutions under analysis.

4.3.2.2 Conventional oven (thermostatically controlled oven, incubator, refrigerator, etc.) capable of

4.3.2.6 Conditioning containers, for conditioning test specimens at 50 % ± 5 % and 80 % ± 5 % relative

NOTE For 50 % relative humidity, 43 % w/v sulphuric acid solution in water is suitable and for 80 % relative

The solutions should be freshly prepared by adding a weighed amount of acid to a suitable volume of

water, cooling to room temperature and making up to the required volume. It is recommended that

relative humidity and temperature be maintained during the conditioning period. Therefore, the

containers should be placed in a conventional oven, at a temperature of approximately 20°C, the set

4.3.2.8 Soxhlet type extractors, capable of holding test specimens on the supports, with flasks of

NOTE Alternative extractors capable of satisfactorily extracting absorbed oil from the test specimens can be

4.3.2.10 Rotary evaporator or distillation apparatus, for evaporation and collection of the extraction

NOTE Artificially cooled water can be necessary for efficient condensation of a low boiling point solvent.

4.3.2.11 Flasks, 50 ml, long neck with condensers to fit, for methyl ester preparations.

4.3.2.12 Gas chromatograph, with flame ionization detector or other suitable detector equipped with

For olive oil: When using a polar column, the major peaks of the olive oil, such as C16:0, methyl

hexadecanoate (methyl palmitate), C16:1, methyl 9-hexadecenoate (methyl palmitoate), C18:0, methyl

octadecanoate (methyl stearate), C18:1, methyl 9-octadecenoate (methyl oleate), C18:2, methyl 9,12-

octadecadienoate (methyl linoleate) and the internal standard C17:0, methyl heptadecanoate (methyl

margarate) shall demonstrate baseline separation. Optionally, a non-polar column can be used which

shall give baseline separation of the methyl esters with 16 and 18 carbon numbers and the internal

— Column 1, polar column, WCOT fused silica column, length 50 m, internal diameter 0,25 mm, coated

— Column 2, non polar column, BP1, length 25 m, internal diameter 0,32 mm, with a 1 micron film

— Column 3, polar column, stainless steel column 2 mm to 3 mm internal diameter and 2 m to 3 m

length with a packing of 10 % to 20 % by mass of polyestersuccinate on a stationary phase of

For other vegetable oils: The condition for separation of the main fatty acid esters should be checked.

4.3.2.13 Glass containers with stoppers, of a volume of approximately 10 ml, for storing the heptane

4.3.2.14 Conventional oven under vacuum or vacuum desiccator, capable of maintaining a temperature

of 60 °C ± 2 °C. The conventional oven or the desiccator shall be equipped with or connected to a

vacuum pump capable of achieving a vacuum of 1,3 kPa or less. The vacuum pump shall be provided

NOTE If a conventional oven under vacuum is not available, a vacuum desiccator placed in an oven at 60°C can

4.3.2.15 Disposable plastic syringes with luer fitting, 1 ml or 10 ml and wide gauge luer needles

4.3.3.1 Cutting slab, clean smooth glass, metal or plastic slab of sufficient area to prepare test

4.3.3.3 Cutting implement, scalpel, scissors, sharp knife or other suitable device

4.3.3.6 Glass containers equipped with an inert sealing system (stopper, lid, etc.) for containing the oil

and test specimens, for example test tubes, ground neck, with an internal diameter of approximately

4.3.3.8 Pipettes, 50 ml and 100 ml, conforming to the requirements of ISO 648 Class B or automatic

4.3.4.1 Specimen supports, for example made of stainless steel, capable of holding and keeping the test

4.3.4.2 Gauze, for example, fine stainless steel gauze, mesh size 1 mm, approximately 25 mm x 100 mm

4.3.4.3 Glass rods, for example 2 mm to 3 mm in diameter and approximately 100 mm long, for

4.3.6 Materials for method 3 (fillable pouch) and for the method 4 (reverse pouch)

The test specimens shall be 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, or with a compressed

As a general rule, do not wash the sample with water or solvent. However, if the articles are accompanied

by instructions for use intended for the user advising cleaning before use, these instructions should be

followed for the test, unless they advise rubbing the article with oil: in this case, the instructions should

Seven test specimens are required for samples, in the form of thin films, sheets, cut sections from

containers or similar articles. Nine test specimens, similar dimensionally to one another, are required for

b) one test specimen to determine the suitability of the oil as the fatty food simulant and

c) a minimum of one test specimens to check for possible loss of volatiles if the sample does not undergo

d) two test specimens for determination of the surface area, in the case of samples of irregular shape.

If the conditioning test in Annex D is used, one additional test specimen is required.

If previous testing has established that interference in the gas chromatography procedure is unlikely and

A minimum of three valid test results is required to calculate the mean. Testing in triplicate is allowed

If the result is to be expressed in mg/kg, determine the contact surface area and the volume of the article

To obtain three validated results and allow for inaccuracies which may arise during the procedure and

which may be difficult to detect, due for example to contamination or loss of oil during the sample

handling stages, four determinations should be carried out on the sample allowing for the result from one

NOTE The two test specimens, c), are used to check whether the sample loses mass from the evaporation of

volatiles, such as solvents, during the test period. If the vacuum drying procedure in Annex D is used, these test

specimens are not required as during the vacuum drying any volatiles will have been removed from the test

It is recommended to use surface of 1dm and a volume of 100 ml. Deviations should be recorded and

The test specimens shall be clean and free from surface contamination (many plastics can readily attract

Cut out test specimens measuring 1 dm ± 0,01 dm using using the tool of 4.3.3.4. If this is not possible,

cut out pieces suitable for obtaining test specimens having a surface area of approximately 1 dm .

Ensure that the test pieces are well separated and that their surfaces are freely exposed to the oil during

If the area of the edges of the test specimen exceeds 10 % of the area of the test specimen measured, this

Cut each test specimen into four pieces 25 mm x 100 mm using the tool of 4.3.3.5.

Cut sections from the walls of the container or article to give test specimens each of area approximately

1 dm . For articles with individual areas less than 1 dm , use a sufficient number of articles to provide

each test specimen. Measure the dimensions of each test specimen to the nearest 1 mm, using a suitable

Calculate the area of each test specimen to the nearest 0,01 dm and record. If necessary, cut each test

specimen into smaller pieces to enable them to fit into the glass containers. The test specimens or pieces

are placed on the specimen supports or, if the test specimens or pieces are sufficiently rigid, they can be

Select representative portions of the article, or multiples of the article for small articles, to give five

dimensionally identical test specimens, with a total surface area of at least 1 dm . Measure only the

surface area intended to come into contact with foodstuffs of two of these test specimens to the nearest

0,05 dm using the Schlegel Method, as described in EN ISO 8442-2:1997, Annex B, the method described

by Mieth and Hoekstra (JRC-2013) or any other suitable method. Record the surface area of each test

Lay the sample on the cutting slab with the surface to be in contact with the oil uppermost.

Cut out the test specimen of suitable dimensions for the cell using the cutting implement.

Prepare a pouch suitable for obtaining an internal contact area of 2 dm and containing a suitable volume

For example, fold over a sheet measuring 120 mm by 240 mm, with the surface under test facing inward,

and seal the 3 other sides such that the area inside the seals defines a square measuring 100 mm by

100 mm, then cut one corner of the pouch in order to be able to fill it with oil (after filling, the corner of

An alternative method consists of only sealing 2 sides and sealing the final side after filling with oil.

Another alternative method consists of using two sheets measuring 120 mm by 120 mm and creating 4

If required, remove any air bubbles liable to be present in the oil before sealing the filled pouch for the