CEN/TC 194/SC 1/WG 1 - Overall migration

This European Standard describes test methods for the determination of the overall migration into fatty food simulants from plastics materials and articles into a mixture of 14C-labelled synthetic triglycerides at temperatures above 20 °C and up to, and including, 121 °C for selected times.
These methods are suitable for plastics in the form of films and sheets, a wide range of articles or containers from which test pieces of a suitable size can be cut and containers and articles that can be filled.
The test methods described are applicable to all plastics.

This European Standard describes 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 14C-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.

This part of this European Prestandard provides a guide to the selection of the appropriate conditions and methods of test for the determination of overall migration into food simulants from plastics which are intended to come into contact with foodstuffs.

This Technical Specification gives guidelines for the selection of the appropriate conditions and test methods for the determination of overall migration into food simulants and test media from polymeric coatings on metal substrates which are intended to come into contact with foodstuffs and a test method for overall migration into aqueous simulants by article filling from polymeric coatings on food and beverage cans and non-stick coatings.
NOTE   Polymeric coatings on metal substrates are not yet included in the scope of any European Union Directive. This Technical Specification has been prepared to assist in the development of such a Directive.

This Technical Specification specifies test methods for 'alternative tests' and 'substitute tests' performed with volatile test media, iso-octane and a volume fraction of 95 % aqueous ethanol, for the determination of overall migration from polymeric coatings on paper and board intended to come into contact with fatty foodstuffs.
NOTE 1   It also includes guidance for the application of Council Directive 82/711/EEC [1], as last amended by Commission Directives  93/8/EC and  97/48/EC [2] [3] as regards the determination of the specific and overall migration into fatty food simulants (fat test) and includes a glossary to clarify the terminology used, see annex B.
NOTE 2   The iso-octane and a volume fraction of 95 % aqueous ethanol volatile test media used in these test methods are those specified for 'substitute tests' in Council Directive 82/711/EEC and its subsequent amendments. In addition to the use of iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Council Directive 82/711/EEC and its subsequent amendments specifies the use of modified polyphenylene oxide as a test medium for use at temperatures of 100 °C and above.  A test method for overall migration from polymeric coatings intended to come into contact with fatty foodstuffs using modified polyphenylene oxide (MPPO) is in preparation.

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 European Standard describes 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 14C-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.

This European Standard describes test methods for 'substitute tests' performed with volatile test media, iso-octane and 95 % v/v aqueous ethanol, for the determination of overall migration from plastics intended to come into contact with fatty foodstuffs at all temperatures and for any period of time.
These test methods are suitable for plastics samples in a wide variety of forms.
NOTE 1   The iso-octane and 95 % v/v aqueous ethanol volatile test media used in these test methods are those specified for 'substitute tests' in Commission Directive 82/711/EEC [3]and its subsequent amendments [4], [5].  In addition to the use of iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Commission Directive 82/711/EEC and its subsequent amendments specifies the use of modified polyphenylene oxide as a test medium for use at temperatures of 100 °C and above.  For a test method for overall migration from plastics intended to come into contact with fatty foodstuffs using modified polyphenylene oxide as a test medium, see EN 1186-13.  
NOTE 2   These test methods can also be used for the 'alternative tests' described in Council Directive 82/711/EEC and its subsequent amendments, when the chosen volatile test media are iso-octane and 95 % aqueous ethanol, provided equivalence is shown with olive oil, see prEN 1186-1:2001.

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 part of this European Prestandard describes a method of test for the determination of the overall migration into aqueous based food simulants from plastics which are intended to come into contact with foodstuffs, by filling articles with aqueous food simulant for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. This method is most suitable for plastics in the form of containers and articles that can be filled.

This part of this European Prestandard describes a method of test for the determination of the overall migration from one surface only of plastics in the form of sheet and film, which are intended to come into contact with foodstuffs, into aqueous based food simulants, by exposure in a standard cell for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. This method is most suitable for plastics in the form of films and sheets, but is particularly applicable to those materials consisting of more than one layer or of surfaces that differ in their migration characteristics,...

This part of this European Prestandard describes a test method for the determination of the overall migration into aqueous based food simulants from plastics which are intended to come into contact with foodstuffs, by total immersion in aqueous food simulant for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. This method is most suitable for plastics in the form of films and sheets, but can be applied to a wide range of articles or containers from which test pieces of suitable size can be cut.

This part of this European Prestandard describes a method of test for the determination of the overall migration from one surface only of plastics in the form of sheet and film, which are intended to come into contact with foodstuffs, by forming the plastics film or sheet into standard pouches and exposure to the aqueous food simulant for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. A standard pouch is a pouch with the dimensions as described in 6.2. This method is most suitable for plastics in the form of films and sheets which are sealable by heat or pressure.

This European Standard describes 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 prEN 1186-2, prEN 1186-4, prEN 1186-6, prEN 1186-8, prEN 1186-12 and prEN 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 prEN 1186-2, in a cell, as described in prEN 1186-4, in a pouch, as described in prEN 1186-6, and by filling, as described in prEN 1186-8 and to tests carried out at low and high temperature, as described in prEN 1186-12 and prEN 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 prEN 1186 is substituted.
The method may 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.

This part of this European Prestandard describes a method of test for the determination of the overall migration from one surface only of plastics in the form of sheet and film, which are intended to come into contact with foodstuffs, by forming the plastics film or sheet into standard pouches and exposure to olive oil for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. A standard pouch is a pouch with the dimensions as defined in 6.3. This method is most suitable for plastics in the form of films and sheets which are sealable by heat or pressure,...

This part of this European Prestandard describes test methods for the determination of the overall migration from plastics intended to come into contact with a fatty foodstuff, by total immersion in olive oil for 10 days, 24 h or for 2 h at 40 °C or 2 h at 70 °C. This method is most suitable for plastics in the form of films and sheets, but can be applied to a wide range of articles or containers from which test pieces of a suitable size can be cut. The test method described is applicable to most types of plastics, althoug there are some plastics for which it is known not to be applicable.

This part of this European Prestandard describes a method of test for the determination of the overall migration from one surface only of plastics in the form of finished articles, which are intended to come into contact with a fatty foodstuff, by filling the finished article with olive oil and leaving for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. Testing samples by this method enables testing of non-homogeneous articles providing that they are not too large. This method is most suitable for plastics in the form of containers and articles that can be filled.

This part of this European Prestandard describes test methods for the determination of the overall migration from one surface only of plastics in the form of sheet and film, which are intended to come into contact with fatty foodstuffs by exposure to olive oil in a standard cell or equivalent cell for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. This method is most suitable for plastics in the form of films and sheets, but is particularly applicable to those materials consisting of more than one layer or of surfaces that differ in their migration characteristics,...

This part of this European Prestandard describes test methods for the determination of the overall migration from plastics intended to come into contact with foodstuffs at low temperatures, for 0.5 h, 1 h, 2 h, 24 h and 10 days at 5 °C or at 20 °C. These test methods are suitable for plastics samples in a wide variety of forms. The fatty food simulant used in these methods is dewaxed sunflower oil since, unlike olive oil, it remains liquid at the lower test temperatures.

This Part of this European Prestandard describes a substitute procedure for the determination of overall migration into olive oil from articles which are intended to come into contact with foodstuffs at elevated temperatures from 100°C up to and including 175°C.  In order to circumvent a number of analytical difficulties caused by the food simulant olive oil at high temperatures 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.

This Part of this European Prestandard describes test methods for 'substitute tests' performed with volatile test media, iso-octane and 95 % v/v aqueous ethanol, for the determination of overall migration from plastics intended to come into contact with fatty foodstuffs at all temperatures and for any period of time. These test methods are suitable for plastics samples in a wide variety of forms.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision date are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN as ++ soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.

Migrated from Progress Sheet (TC Comment) (2000-07-10): This draft will lead to an ENV as a first step. It is devoted to become an EN ++ as soon as a collaborative study is organized and the precision data are ++ determined.