CEN/TC 194/SC 1/WG 2 - Methods of test for monomers

This document, part of EN 13130, specifies a procedure for the determination of 1,3-benzenedimethanamine (also known as 3-(aminomethyl)-benzylamine or m-xylylene diamine (m-XDA)) monomer, hereinafter referred to as m-XDA, in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of m-XDA monomer determined is expressed as milligrams of m-XDA per kilogram of food simulant in the above mentioned food simulants.
NOTE   In addition to the instability of m-XDA observed in olive oil, the test laboratory could not detect any
m-XDA peak from the olive oil work-up procedure. Based on some control checks, the assumption of the test laboratory was that the extraction from the olive oil does not work. Therefore, it is recommended that the food simulant 95 % ethanol or iso-octane be applied as substitute fatty simulants instead of olive oil.  It is believed that 95 % ethanol and iso-octane can be treated in the same way as 15 % v/v aqueous ethanol and olive oil simulant, respectively. Corresponding investigations were not possible within the project.

This document, part of EN 13130, specifies an analytical procedure for the determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved substitute.  The level of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone determined, is expressed as milligrams of
3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone per kilogram of food or food simulant.  The method is applicable to the quantitative determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in an approximate analyte concentration range of 0,18 mg/kg to 4/ kg of food simulants.
NOTE 1   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. a mixture of synthetic triglycerides or sunflower oil.
NOTE 2   The suitability of the fat simulant should be assessed prior to setting up migration tests. Olive oil has been found to give unacceptable interference in some cases.

This document, part of EN 13130, specifies an analytical procedure for the determination of 4-methyl-1-pentene in food simulants distilled water, 3 % (w/v) aqueous acetic acid aqueous solution, 15 % (v/v) aqueous ethanol aqueous solution and rectified olive oil. The level of
4-methyl-1-pentene monomer determined is expressed as milligrams per kilogram of food simulant. In principle, the method is appropriate for the quantitative determination of 4-methyl-1-pentene at a minimum level of 0,005 mg/kg in all of the four food simulants. However, in the case of interferences, which have been observed for some olive oil batches, the detection limit can be compromised correspondingly.
NOTE   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants such as corn oil, sunflower oil and a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the determination of vinyl acetate in the four conventional EU food simulants, water, 10 % (v/v) ethanol aqueous solution; 3 % (w/v) acetic acid aqueous solution and olive oil or an approved substitute. The level of vinyl acetate monomer determined is expressed as milligrams of vinyl acetate per kilogram of food simulant. The method is appropriate for the quantitative determination of vinyl acetate in approximate analyte concentration range of 1,2 mg/kg to 24 mg/kg food simulant.
NOTE 1   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants such as sunflower oil and a mixture of synthetic triglycerides.
NOTE 2   The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or a mixture of synthetic triglycerides if unacceptable interferences are found with olive oil.

This document, part of EN 13130, specifies an analytical procedure for the determination of residual epichlorohydrin in coatings.
The method is appropriate for the quantitative determination of epichlorohydrin in the analyte concentration range of 5 ng/ml to 80 ng/ml of extract.  In general this allows for the detection of epichlorohydrin at the level of 1 mg/kg of polymer or in the case of coatings, where the amount of polymer cannot be determined, detection of 1 µg epichlorohydrin per square decimetre of coating is feasible.
In order to obtain reliable and reproducible results, it is essential that the method described in this part of EN 13130 is followed as closely as possible.

This document, part of EN 13130, specifies an analytical procedure for the determination of maleic acid in the four conventional food simulants, water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved substitute. The level of maleic acid determined is expressed as milligrams of maleic acid per kilogram of food or food simulant. The method is appropriate for the quantitative determination of maleic acid in approximate analyte concentration range of 5 mg/kg to 60 mg/kg in the above mentioned food simulants.
This method is also suitable for the determination of maleic anhydride in the four food simulants as the anhydride is hydrolyzed rapidly and completely to maleic acid during sample preparation. The level of maleic anhydride is then expressed as milligrams of maleic acid per kilogram of food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants, e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or HB 307 if unacceptable interferences are found with olive oil.

This document, part of EN 13130, specifies two methods as follows.
Method A is an analytical procedure for the determination of the monomers 1,2-DHB,
1,3-DHB and 1,4-DHB in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The levels of monomer determined are expressed in milligrams of monomer per kilogram of food simulant. The method is appropriate for the quantitative determination of 1,2-DHB and 1,3-DHB at a minimum level of 0,15 mg/kg in food simulants and, of 1,4-DHB at a minimum level of 0,10 mg/kg in food simulants.
Method B is an analytical procedure for the determination of DHBphen and DHBiph in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The method is appropriate for the quantitative determination of DHBphen or DHBiph at minimum levels of 0,2 mg/kg and 0,25 mg/kg, respectively, in food simulants.
NOTE   The methods should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the determination of dimethylaminoethanol in food simulants: distilled water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil. The method is appropriate for the quantitative determination of dimethylaminoethanol in an approximate analyte concentration range of 3,4 mg/kg to 36 mg per kilogram of food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil and a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies a method for the determination of Bisphenol A in the food simulants water, 3 % w/v acetic acid aqueous, 15 % v/v ethanol aqueous solution and rectified olive oil. The level of Bisphenol A monomer determined is expressed as milligrams Bisphenol A per kilogram of food simulant. The method is applicable to the quantitative determination of Bisphenol A at a minimum level of 0,2 mg/kg to 0,7 mg per kilogram of food simulants.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants, sunflower oil and a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the chemical conversion of HMTA to formaldehyde and the determination of formaldehyde in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil.
The method is appropriate for the quantitative determination of formaldehyde in approximate analyte concentration range of 3,0 mg to 30 mg formaldehyde per kilogram of food simulant, which corresponds to
2,3 mg to 23,3 mg hexamethylenetetramine per kilogram of food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the determination of carbonyl chloride monomer in polymers. The method is applicable to polycarbonate as well as to other polymers and copolymers where these are soluble in methylene chloride. The level of carbonyl chloride monomer determined is expressed as milligrams of carbonyl chloride per kilogram of polymer. The method is appropriate for the quantitative determination of carbonyl chloride at a minimum level of 0,3 mg per kilogram of polymer.

This document, part of EN 13130, specifies an analytical procedure for the determination of EDA monomer and HMDA monomer in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil as well as in the substitute food simulants 95 % v/v ethanol and iso-octane. The level of EDA monomer and HMDA monomer determined are expressed as milligram EDA per kilogram of food simulant and as milligrams HMDA per kilogram of food simulant. The method is appropriate for the quantitative determination of EDA at a minimum level of 1 mg per kilogram of food simulants and for the quantitative determination of HMDA at a minimum level of 0,5 mg per kilogram of food simulants.
The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants sunflower oil and a mixture of synthetic triglycerides.

This document, part of EN 13031,13130, specifies an analytical procedure for the determination of 2,4,6-triamino-1,3,5-triazine in food simulants distilled water, 3 % (w/v) acetic acid aqueous solution, 15% (v/v) ethanol aqueous solution and rectified olive oil. The level of
2,4,6-triamino-1,3,5-triazine monomer determined is expressed as milligrams per kilogram food simulant. The method is appropriate for the quantitative determination of 2,4,6-triamino-1,3,5-triazine in approximate analyte concentration range of 2 mg/kg to 60 mg/kg food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies analytical procedures for the determination of 1-octene and THF in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of 1-octene and THF monomer determined is expressed as milligrams of monomer per kilogram of food simulant. The methods are appropriate for the quantitative determination of 1-octene in the range of 2 mg/kg to 30 mg/kg in food simulants and of THF in the range of 0,06 mg/kg to 1,5 mg/kg in food simulants.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

This Technical Specification, part of EN 13031, specifies an analytical procedure for the determination of acrylamide in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and fat simulant. The level of acrylamide monomer determined is expressed as milligrams of acrylamide/kg of food simulant. The method is appropriate for the quantitative determination of acrylamide in approximate analyte concentration range of 0,01 mg/kg to 0,1 mg/kg of food simulants.
The method should also be applicable to other fat simulants.
NOTE   The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or a mixture of synthetic triglycerides if unacceptable interferences are found with olive oil.

This document, part of EN 13130, specifies a method for the determination of
11-aminoundecanoic acid in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol, olive oil and iso-octane. The level of 11-aminoundecanoic acid determined is expressed as milligrams per kilogram of food simulant.
The method is appropriate for the quantitative determination of 11-amino-undecanoic acid in approximate analyte concentration range of 0,5 mg/kg to 10 mg/kg of food simulants.

This document, part of EN 13130, specifies an analytical procedure for the determination of caprolactam in the food simulants distilled water, 3 % w/v aqueous acetic acid,
15 % v/v aqueous ethanol and rectified olive oil. The level of caprolactam monomer determined is expressed as mg caprolactam/kg of food or food simulant. The method is appropriate for the quantitative determination of caprolactam in an approximate analyte concentration range of 1,5mg/kg to 30 mg per kilogram of food simulant.
This method is also applicable to the determination of the specific migration of caprolactam sodium salt, PM/Ref No 14230, as caprolactam sodium salt instantaneously hydrolyzes to caprolactam when in contact with aqueous media.
NOTE   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil, a mixture of synthetic triglycerides and volatile substitutes for fat simulants.

This document, part of EN 13130, specifies an analytical procedure for the determination of butadiene monomer in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of butadiene monomer determined is expressed as mg butadiene/kg of food. The method is appropriate for the quantitative determination of butadiene at a range of 0,01 mg/kg to 0,1 mg/kg in food simulants.
NOTE   The method should also be applicable to other aqueous food simulants and to the other fatty food simulants such as sunflower oil and a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the determination of 1,1,1-trimethylolpropane in food simulants distilled water, 3 % (w/v) acetic acid aqueous solution, 15 % (v/v) ethanol aqueous solution and rectified olive oil. The method is appropriate for the quantitative determination of 1,1,1-trimethylolpropane in approximate analyte concentration range of 0,6 mg/kg to 12 mg/kg food simulant.
NOTE   The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

This document, part of EN 13130, specifies an analytical procedure for the determination of ethylene oxide (EO) or propylene oxide (PO) in polymers.
The method is appropriate for the quantitative determination of ethylene oxide or propylene oxide in an analyte concentration range of approximately 0,2 mg/kg to 2 mg/kg of polymer.

This part of this European Standard provides a guide to the selection of the appropriate conditions of contact of food simulants with the test article before the determination of specific migration of those substances subject to a migration limit.
NOTE   According to Directive 90/128/EEC[2] the determination of the migration of specified components in foodstuffs instead of the use of simulants is permitted.  However, in that situation there is no need to give guidance on the test conditions of time and temperature as contact conditions shall be equal to conditions applied in real.
Also general guidance is given for the determination of the amount of the substance in the final plastics material or article.

This part of this European Standard specifies methods for the determination of the monomer terephthalic acid in food simulants; distilled water, 3 % w/v acetic acid aqueous solution, 15 % v/v ethanol aqueous solution and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil.  The methods are capable of determining terephthalic acid in the food simulants at the level of the specific migration limit of 7,5 mg of terephthalic acid per kilogram of food simulants.
NOTE   This method was developed for the determination of terephthalic acid in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out.  However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.

This part of this European Standard specifies a method for the determination of vinylidene chloride monomer in food simulants.  The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil.  The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of food simulant.  The method is appropriate for the quantitative determination of vinylidene chloride at a level of 0,05 mg/kg.
NOTE   This method was developed for the determination of vinylidene chloride in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out.  However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.

This part of this European Standard specifies a method for the determination of vinylidene chloride (VdC) in plastics materials and articles.
The method is applicable to poly(vinylidene chloride) (PVdC) films, PVdC coated films, and laminates and coextruded materials containing PVdC.  The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of polymer.  The method is appropriate for the quantitative determination of vinylidene chloride at a level of 5 mg/kg in plastics materials and articles.

This part of this European Standard specifies a method for the determination of butadiene monomer in polymers.
The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer.  The method is appropriate for the quantitative determination of 1,3-butadiene at a level of 0,1 mg/kg in the polymer.

This part of this European Standard describes a method for the determination of individual and total levels of residual isocyanates in plastics materials and articles.
This method is applicable to the analysis of polyurethane polymers.  The total level of isocyanate monomers in materials and articles determined according to the procedure described in this standard is given in milligrams of NCO per kilogram of material or article.  The method is capable of quantitative determination of individual isocyanates measured as NCO at 0,04 mg/kg and total isocyanates at 1,0 mg/kg.
NOTE   The method has been applied to the analysis of 9 isocyanate monomers listed in 3.1.  It has not been applied to the analysis of octadecyl isocyanate, diphenylether-4,4'-diisocyanate or 3,3'-dimethyl-4,4'-diisocyanatobiphenyl as samples of these monomers have not been obtained.  There is no reason to anticipate that the method may not be suitable for the analysis of these monomers also.

This part of this European Standard specifies a method for the determination of acrylonitrile monomer in foods and food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil, as well as to liquid and solid foodstuffs such as beverages and soft margarine.  The level of acrylonitrile monomer determined is expressed as milligrammes of acrylonitrile per kilogram of food or food simulant.
The method is appropriate for the quantitative determination of acrylonitrile monomer at minimum levels of down to 0,01 mg/kg to 0,005 mg/kg, or lower, in food simulant, depending on the applied test conditions (see NOTE in 8.2.3).  With regard to the performance in the mentioned foodstuffs, in general, a direct detection limit of 0,02 mg/kg is achievable.
NOTE   This method was developed for the determination of acrylonitrile in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out.  However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.

This part of this European Standard specifies methods for the determination of monoethylene glycol and diethylene glycol in the food simulants; water, 3 % w/v acetic acid, 15 % v/v ethanol and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil.  The methods are capable of determining monoethylene glycol and diethylene glycol in food simulants separately, or combined, at the specific migration limit SML (T) of 30 mg/kg.
NOTE   This method was developed for the determination of monoethylene glycol and diethylene glycol in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out.  However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.

This Part of this European Prestandard specifies methods for the determination of monoethylene glycol and diethylene glycol in the four conventional EC food simulants; water, 3 % w/v acetic acid, 15 % v/v ethanol and olive oil (or approved substitutes sunflower oil or mixture of synthetic triglycerides).  The methods are capable of determining monoethylene glycol and diethylene glycol in food simulants separately, or combined, at the specific migration limit SML (T) of 30 mg/kg.

This Part of this European Prestandard specifies a method for the determination of vinylidene chloride (VdC) in plastics materials and articles. The method is applicable to poly(vinylidene chloride) (PVdC) films, PVdC coated films, and laminates and coextruded materials containing PVdC.  The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of polymer.

This Part of this European Prestandard describes a method for the determination of individual and total levels of residual isocyanates in plastics materials and articles.  This method is applicable to the analysis of polyurethane polymers. The total level of isocyanate monomers in materials and articles determined according to the procedure described in this prestandard is given in milligrams of NCO per kilogram of material or article.

This Part of this European Prestandard specifies a method for the determination of butadiene monomer in polymers.   The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer.

This Part of this European Prestandard specifies a method for the determination of vinylidene chloride monomer in food simulants.  The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and to the approved alternatives, sunflower oil and a mixture of synthetic triglycerides.  The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of food simulant.

This Part of this European Prestandard specifies methods for the determination of the monomer terephthalic acid in food simulants; distilled water, 3 % w/v acetic acid aqueous solution, 15 % v/v ethanol aqueous solution and olive oil or its approved substitutes, sunflower oil or a mixture of synthetic triglycerides. The methods are capable of determining terephthalic acid in the food simulants at the level of the specific migration limit in Commission Directive 90/128/EEC.

This Part of this European Prestandard provides a guide to the selection of the appropriate conditions and test methods for the determination of specific migration of those substances subject to a limit upon their migration into food and food simulants from plastics which are intended to come into contact with foodstuffs and the determination of substances in plastics.

This Part of this European Prestandard specifies a method for the determination of acrylonitrile monomer in foods and food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and to the approved alternatives sunflower oil and a mixture of synthetic triglycerides, as well as to liquid and solid foodstuffs such as beverages and soft margarine.  The level of acrylonitrile monomer determined is expressed as milligrammes of acrylonitrile per kilogram of food or food simulant.