CEN/TS 13130-12:2005

Material and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 12: Determination of 1,3-benzenedimethanamine in food simulants

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.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 12: Bestimmung von 1,3-Benzendimethanamin in Prüflebensmitteln

Diese Technische Spezifikation, Teil der EN 13130, legt ein Verfahren zur Bestimmung von monomerem 1,3-Benzendimethanamin (auch bekannt als 3 (Aminomethyl)-Benzylamin oder m Xylylendiamin (m XDA)), im Folgenden bezeichnet als m XDA, in den Prüflebensmitteln Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung und Olivenöl fest. Der ermittelte Gehalt an monomerem m XDA wird in Milligramm m XDA je Kilogramm Prüflebensmittel in den vorstehend erwähnten Prüflebensmitteln angegeben.
ANMERKUNG   Außer der beobachteten Instabilität von m XDA in Olivenöl, konnte das Prüflaboratorium keinen aus dem Aufarbeitungsverfahren von Olivenöl stammenden m XDA Peak nachweisen. Die Annahme des Prüflaboratoriums, dass keine Extraktion aus dem Olivenöl erfolgt, beruht auf einigen Kontrollprüfungen. Deshalb wird empfohlen, anstelle von Olivenöl als fettige Ersatzprüflebensmittel 95%iges Ethanol oder Isooctan zu verwenden. Es wird davon ausgegangen, dass 95%iges Ethanol und Isooctan auf dieselbe Art und Weise wie die entsprechenden Prüflebensmittel 15%iges (Volumenanteil) Ethanol in wässriger Lösung und Olivenöl behandelt werden können. Im Rahmen des Projektes waren keine entsprechenden Untersuchungen möglich.

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matières plastiques soumises à des limitations - Partie 12 : Détermination du 1,3-benzénediméthanamine dans les simulants d'aliments

Le présent document, qui fait partie de l'EN 13130, spécifie une procédure de détermination du 1,3-benzénediméthanamine (également connu sous le nom de 3-(aminométhyl)-benzylamine ou m-xylylène diamine (m-XDA), ci-après désigné m-XDA) dans les simulants d'aliments suivants : eau, solution aqueuse d'acide acétique à 3 % (m/v), solution aqueuse d'éthanol à 15 % (v/v) et huile d'olive. La teneur en monomère de m-XDA déterminée est exprimée en milligrammes de m-XDA par kilogramme de simulant d'aliments (l'un des simulants décrits ci-avant).
NOTE   Outre l'instabilité du m-XDA dans le simulant à base d'huile d'olive, le laboratoire d'essai n'a pas réussi à détecter de pic de m-XDA à l'aide de la méthode utilisée pour l'huile d'olive. Sur la base de plusieurs vérifications, le laboratoire a conclu que l'extraction à partir de l'huile d'olive ne fonctionne pas. Il est par conséquent recommandé de remplacer l'huile d'olive par le simulant à base d'éthanol à 95 % ou d'iso-octane. L'éthanol à 95 % et l'iso-octane peuvent en principe être traités respectivement comme la solution aqueuse d'éthanol à 15 % (v/v) et le simulant à base d'huile d'olive. Il n'a pas été possible de vérifier ce point dans le cadre du projet.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 12. del: Določevanje 1,3-benzendimetanamina v modelnih raztopinah za živila

General Information

• Status: Published
• Publication Date: 22-Feb-2005
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: CEN/TC 194 - Utensils in contact with food
• Drafting Committee: CEN/TC 194/SC 1/WG 2 - Methods of test for monomers
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 23-Feb-2005
• Completion Date: 23-Feb-2005
• Ref Project: SIST-TS CEN/TS 13130-12:2005 - Material and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 12: Determination of 1,3-benzenedimethanamine in food simulants

Overview

CEN/TS 13130-12:2005 specifies an analytical procedure for the determination of 1,3-benzenedimethanamine (also known as m-xylylene diamine, m-XDA) migrating from plastics into food simulants. The method reports m‑XDA levels as milligrams per kilogram of food simulant and covers testing in: water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The technique is based on derivatization with fluorescamine and analysis by HPLC with fluorescence detection.

Important practical note: m‑XDA is unstable in olive oil under migration test conditions and the laboratory that validated this method observed poor recovery. The standard therefore recommends using 95 % ethanol or iso‑octane as substitute fatty simulants where appropriate.

Key topics and technical requirements

• Analyte: 1,3-benzenedimethanamine (m‑XDA / m-xylylene diamine).
• Principle: Bis‑derivatization of m‑XDA with fluorescamine followed by HPLC–fluorescence quantification; identity confirmation via mono‑derivatization and comparison with authentic standards.
• Food simulants covered: water; 3 % w/v acetic acid; 15 % v/v ethanol; olive oil (with caveats and substitutes recommended).
• Quantification: external calibration against prepared standard solutions; results expressed in mg m‑XDA per kg simulant.
• Reagents and consumables: fluorescamine, borate buffer (pH ≈ 9.2), HPLC grade solvents and standard stock solutions of m‑XDA; storage and stability conditions for standards are specified.
• Apparatus: HPLC system with fluorescence detector and suitable column able to resolve derivatized m‑XDA from interferences.
• Quality considerations: recovery checks for olive oil (or substitute simulants) and confirmation steps to avoid false negatives due to instability or extraction failures.

Applications and who uses it

• Regulatory and compliance testing: laboratories verifying specific migration limits for plastics in contact with food under EU directives supported by the EN 13130 series.
• Manufacturers and raw‑material suppliers: quality control of polymers and monitoring residual monomer (m‑XDA) levels after production.
• Accredited testing labs and research groups: method implementation for migration studies, method validation, and inter‑laboratory comparisons.
• Product safety and QA teams: to assess food contact materials for potential consumer exposure to amine monomers.

Related standards

• Part of the EN 13130 series (Materials and articles in contact with foodstuffs - Plastics substances subject to limitation).
• Should be used in conjunction with EN 13130‑1 (Guide to test methods and selection of exposure conditions).
• Supports EU legislation referenced in the specification (e.g., 2002/72/EC and earlier directives cited).

Keywords: CEN/TS 13130-12:2005, 1,3-benzenedimethanamine, m‑XDA, m-xylylene diamine, food simulants, migration testing, HPLC, fluorescamine, plastics food contact, specific migration.

Standards Content (Sample)

SLOVENSKI STANDARD
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHEHQ]HQGLPHWDQDPLQDY
PRGHOQLKUD]WRSLQDK]DåLYLOD
Material and articles in contact with foodstuffs - Plastics substances subject to limitation -
Part 12: Determination of 1,3-benzenedimethanamine in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 12: Bestimmung von 1,3-Benzendimethanamin in
Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 12 : Détermination du 1,3-
benzénediméthanamine dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-12:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL SPECIFICATION
CEN/TS 13130-12
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Material and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 12: Determination of 1,3-
benzenedimethanamine in food simulants
Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires - Substances dans les matières plastiques - Substanzen in Kunststoffen, die Beschränkungen
soumises à des limitations - Partie 12 : Détermination du unterliegen - Teil 12: Bestimmung von 1,3-
1,3-benzénediméthanamine dans les simulants d'aliments Benzendimethanamin in Prüflebensmitteln
This Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 13130-12:2005: E
worldwide for CEN national Members.

Contents
page
Foreword. 3
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Principle . 6
4 Reagents . 6
5 Apparatus . 9
6 Samples . 9
7 Procedure . 10
8 Expression of results. 12
9 Confirmation. 13
10 Test report . 14
Bibliography . 15

Foreword
This document (CEN/TS 13130-12:2005) has been prepared by Technical Committee CEN/TC 194
“Utensils in contact with food”, the secretariat of which is held by BSI.
This part of EN 13130 has been prepared within the Standards, Measurement and Testing project,
MAT1-CT92-0006, “Development of Methods of Analysis for Monomers” and has been prepared by
Subcommittee (SC 1) of TC 194 "Utensils in contact with food" as one of a series of test methods for
plastics materials and articles in contact with foodstuffs.
This standard is intended to support Directives 2002/72/EC [1], 89/109/EEC [2], 82/711/EEC [3] and
its amendments 93/8/EEC [4] and 97/48/EC [5], and 85/572/EEC [6].
At the time of preparation and publication of this part of EN 13130 the European Union legislation
relating to plastics materials and articles intended to come into contact with foodstuffs is incomplete.
Further Directives and amendments to existing Directives are expected which could change the
legislative requirements which this standard supports. It is therefore strongly recommended that users
of this standard refer to the latest relevant published Directive(s) before commencement of a test or
tests described in this standard.
This part of EN 13130 should be read in conjunction with EN 13130-1.
Further parts of EN 13130, under the general title Materials and articles in contact with foodstuffs -
Plastics substances subject to limitation, have been prepared, and others are in preparation,
concerned with the determination of specific migration from plastics materials into foodstuffs and food
simulants and the determination of specific monomers and additives in plastics. The parts of
EN 13130 are as follows.
Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food
simulants and the determination of substances in plastics and the selection of conditions of exposure
to food simulants
Part 2: Determination of terephthalic acid in food simulants
Part 3: Determination of acrylonitrile in food and food simulants
Part 4: Determination of 1,3-butadiene in plastics
Part 5: Determination of vinylidene chloride in food simulants
Part 6: Determination of vinylidene chloride in plastics
Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants
Part 8: Determination of isocyanates in plastics
Part 9: Determination of acetic acid, vinyl ester in food simulants
Part 10: Determination of acrylamide in food simulants
Part 11: Determination of 11-aminoundecanoic acid in food simulants
Part 12: Determination of 1,3-benzenedimethanamine in food simulants
Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants
Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants
Part 15: Determination of 1,3-butadiene in food simulants
Part 16: Determination of caprolactam and caprolactam salt in food simulants
Part 17: Determination of carbonyl chloride in plastics
Part 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene,
1,4-dihydroxybenzene, 4,4’-dihydroxybenzophenone and 4,4’dihydroxybiphenyl in food simulants
Part 19: Determination of dimethylaminoethanol in food simulants
Part 20: Determination of epichlorohydrin in plastics
Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants
Part 22: Determination of ethylene oxide and propylene oxide in plastics
Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants
Part 24: Determination of maleic acid and maleic anhydride in food simulants
Part 25: Determination of 4-methyl-pentene in food simulants
Part 26: Determination of 1-octene and tetrahydrofuran in food simulants
Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants
Part 28: Determination of 1,1,1-trimethylolpropane in food simulants
Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications.
WARNING All chemicals are hazardous to health to a greater or lesser extent. It is beyond
the scope of this Technical Specification to give instructions for the safe handling of all
chemicals, that meet, in full, the legal obligations in all countries in which this Technical
Specification may be followed. Therefore, specific warnings are not given and users of this
Technical Specification should ensure that they meet all the necessary safety requirements in
their own country.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus,
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Introduction
1,3-benzenedimethanamine (also known as 3-(aminomethyl)-benzylamine or m-xylylene diamine
(m-XDA)), C H N , PM/Ref-No. 13000, hereinafter referred to as m-XDA, is a monomer used in the
8 12 2
manufacture of certain plastics materials and articles intended to come into contact with foodstuffs.
After manufacture, residual m-XDA monomer can remain in the polymer and may migrate into
foodstuffs coming into contact with the plastics material or article.
NOTE However the following should be taken into account when carrying out a migration test: Stability tests
in spiked olive oil food simulant carried out under test conditions 10 d at 40 °C indicated that m-XDA is not stable
in the fat simulant, presumably due to chemical reaction with the olive oil and/or oxygen. Typically a recovery of
only 25 % was obtained under these test conditions. Therefore, even though this analytical method works in
principle with olive oil as a food simulant, the migration test using olive oil or another fat simulant can provide
false-negative results. Therefore, the method should only be applied in case of short exposure periods with olive
oil and if applied, a recovery check with spiked olive oil applying the same time/temperature migration test
conditions is recommended, see also the NOTE in Clause 1.
The method has been tested by a second laboratory.
1 Scope
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.
2 Normative references
The following referenced documents are indispensable for the application 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 13130-1:2004, Materials and articles in contact with foodstuffs – Plastics substances subject to
limitation – Part 1: Guide to test methods for the specific migration of substances from plastics to
foods and food simulants and the determination of substances in plastics and the selection of
conditions of exposure to food simulants.
3 Principle
m-XDA in aqueous simulant test samples is determined, following bis-derivatization with
fluorescamine, by high performance liquid chromatography (HPLC) with fluorescence detection.
m-XDA in olive oil test samples is extracted with 3 % w/v aqueous acetic acid and determined in the
same way. Quantification is relative to external standards. The identity of m-XDA is confirmed by
mono-derivatization with less fluorescamine leading to a second peak in the HPLC chromatograms
obtained from samples, and by comparison with authentic samples.
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analyte
1,3-benzenedimethanamine (also known as 3-(aminomethyl)-benzylamine or m-xylylene diamine
(m-XDA), C H N , purity 99 %.
8 12 2
4.2 Other chemicals
4.2.1 Distilled water (HPLC grade), saturated with nitrogen (4.2.10).
4.2.2 Methanol (HPLC grade).
4.2.3 Tetrahydrofuran (HPLC grade).
4.2.4 Acetone
4.2.5 Heptane
4.2.6 Fluorescamine, C H O , purity 98 %.
17 10 4
.
4.2.7 Disodium tetraborate 10-hydrate, Na B O 10H O.
2 2 7 2
4.2.8 Sodium hydroxide
4.2.9 Acetic acid glacial 100 %
4.2.10 Purified nitrogen, 99,9999 %.
4.3 Solutions
4.3.1 3 % w/v acetic acid in distilled water
Weigh 15,0 g of acetic acid (4.2.9) with an accuracy of 0,1 g into a 500 ml volumetric flask and make
up to the mark with distilled water (4.2.1).
4.3.2 90 % (v/v)Tetrahydrofuran
Pour 90 ml of tetrahydrofuran (4.2.3) into a 100 ml volumetric flask and make up to the mark with
water (4.2.1).
4.3.3 Fluorescamine solution, 2 mg/ml
Weigh 10 mg of fluorescamine (4.2.6) into a 5 ml volumetric flask and make up to the mark with
acetone (4.2.4).
NOTE The solution can be stored for up to 1 week in the dark at 5 ºC.
4.3.4 5 M sodium hydroxide, NaOH
Weigh 20,0 g of sodium hydroxide (4.2.8) into a 100 ml volumetric flask and make up to the mark with
water (4.2.1).
4.3.5 0,15 M borate buffer (pH = 9,2)
Weigh 14,3 g of disodium tetraborate 10-hydrate (4.2.7) into a 250 ml volumetric flask and make up to
the mark with water (4.2.1).
Any precipitate caused by a fall in temperature shall be totally re-dissolved before the solution is used.
4.3.6 0,02 M borate buffer (pH = 9,2)
Transfer 133 ml of 0,15 M borate buffer (4.3.5) to a 1 l volumetric flask, and make up to the mark with
water (4.2.1).
4.3.7 Mobile phase for high performance liquid chromatography, 18/37/45 borate
buffer/water/methanol
Mix 180 ml of 0,02 M borate buffer (4.3.6) with 370 ml of water (4.2.1) and 450 ml of methanol (4.2.2).
NOTE With some HPLC equipment it may be necessary to degas the mobile phase.
4.3.8 Standard stock solution of m-XDA in water at a known concentration of approximately
1 000 mg/l
Under a nitrogen atmosphere, weigh 100 mg ± 2 mg of m-XDA (4.1) into a 100 ml volumetric flask
with an accuracy of 0,1 mg, and make up to the mark with water (4.2.1). Stopper and mix thoroughly.
Calculate the exact concentration of m-XDA in milligrams per litre.
Repeat the procedure to provide a second standard stock solution.
Store the solution for up to 3 months in the dark at 5 °C.
4.3.9 Standard stock solutions of m-XDA at a known concentration of approximately 2 mg/l
for the preparation of aqueous food simulant calibration samples
4.3.9.1 Pipette 2 ml of the standard stock solution of m-XDA (4.3.8) into a 100 ml volumetric flask
and dilute to volume with the appropriate aqueous food simulant, thus obtaining a intermediate
standard solution of m-XDA of approximately 20 mg/l.
4.3.9.2 Pipette 10 ml of the intermediate standard solution obtained in 4.3.9.1 into a 100 ml
volumetric flask and dilute to volume w
...