Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants

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.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 27: Bestimmung von 2,4,6-Triamino-1,3,5-Triazin in Prüflebensmitteln

Diese Technische Spezifikation, Teil von EN 13130, legt ein Analyseverfahren zur Bestimmung von 2,4,6 Triamino-1,3,5 Triazin in den Prüflebensmitteln destilliertes Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung und rektifiziertes Olivenöl fest. Der ermittelte Gehalt an monomerem 2,4,6 Triamino-1,3,5 Triazin wird in Milligramm je Kilogramm Prüflebensmittel angegeben. Das Verfahren eignet sich zur quantitativen Bestimmung von 2,4,6 Triamino-1,3,5 Triazin im angenäherten Konzentrationsbereich des Analyten von 2 mg/kg bis 60 mg/kg Prüflebensmittel.
ANMERKUNG   Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebensmittel, z. B. Sonnenblumenöl, Maiskeimöl oder eine Mischung synthetischer Triglyceride, anwendbar sein.

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 27 : Détermination de la 2,4,6-triamino-1,3,5-triazine dans les simulants d'aliments

Cette Spécification technique, qui fait partie de l'EN 13130, spécifie un mode opératoire d'analyse pour la détermination de la 2,4,6 triamino 1,3,5 triazine dans les quatre simulants d'aliments suivants : eau distillée, solution aqueuse d'acide acétique a 3 % (m/v), solution aqueuse d'éthanol a 15 % (v/v) et huile d'olive rectifiée. La teneur en monomere de 2,4,6 triamino 1,3,5 triazine est exprimée en milligrammes par kilogramme de simulant d'aliments. Cette méthode convient pour la détermination quantitative de la 2,4,6 triamino 1,3,5 triazine pour une gamme de concentrations d'analyte comprises approximativement entre 2 mg/kg et 60 mg/kg de simulant d'aliments.
NOTE    Il convient que la méthode puisse également etre appliquée a d'autres simulants aqueux ainsi qu'a d'autres simulants gras, tels que l'huile de tournesol, l'huile de mais ou un mélange de triglycérides synthétiques.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 27. del: Določevanje 2,4,6-triamino-1,3,5-triazina (melamina) v modelnih raztopinah za živila

General Information

Status
Published
Publication Date
31-Mar-2005
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Apr-2005
Due Date
01-Apr-2005
Completion Date
01-Apr-2005

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SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-27:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHWULDPLQRWULD]LQD
PHODPLQD YPRGHOQLKUD]WRSLQDK]DåLYLOD
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 27: Bestimmung von 2,4,6-Triamino-1,3,5-Triazin
in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 27 : Détermination de la 2,4,6-
triamino-1,3,5-triazine dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-27:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-27:2005 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 13130-27:2005

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SIST-TS CEN/TS 13130-27:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-27
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 27: Determination of
2,4,6-triamino-1,3,5-triazine 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 27 : Détermination de la unterliegen - Teil 27: Bestimmung von 2,4,6-Triamino-
2,4,6-triamino-1,3,5-triazine dans les simulants d'aliments 1,3,5-Triazin 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 13130-27:2005: E
worldwide for CEN national Members.

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)
Contents
page
Foreword. 3
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Principle . 6
4 Reagents . 6
5 Apparatus . 8
6 Samples . 9
7 Procedure . 10
8 Expression of results. 11
9 Confirmation. 12
10 Test report . 13
Bibliography . 14

2

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)
Foreword
This document (CEN/TS 13130-27:2005) 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
3

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)
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.
4

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)
Introduction
2,4,6-triamino-1,3,5-triazine, (C H N ), PM/Ref. No 25420, is a monomer used in the manufacture of
3 6 6
certain plastics materials and articles intended to come into contact with foodstuffs. Other frequently
used names for 2,4,6-triamino-1,3,5-triazine are melamine and 2,4,6-triamino-s-triazine. After
manufacture residual 2,4,6-triamino-1,3,5-triazine can remain in the finished product and may migrate
into foodstuffs coming into contact with that product.
The method has been pre-validated by a collaborative trial with two laboratories.
5

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)

1 Scope
This document, part of EN 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.
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
The level of 2,4,6-triamino-1,3,5-triazine in food simulants is determined by high performance liquid
chromatography (HPLC) using UV detection at 230 nm. The aqueous food simulants are analyzed
directly by HPLC. The olive oil test samples are extracted with water/isopropanol and the resultant
solutions analyzed by HPLC. Quantification is achieved by means of external standard calibration
using relevant food simulant samples fortified with known amounts of 2,4,6-triamino-1,3,5-triazine.
Confirmation of 2,4,6-triamino-1,3,5-triazine is carried out by diode array detection and peak ratio
measurement at various wavelengths.
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analyte
2,4,6-triamino-1,3,5-triazine, (C H N ), purity > 99 %.
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6

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SIST-TS CEN/TS 13130-27:2005
CEN/TS 13130-27:2005 (E)
4.2 Chemicals
4.2.1 Acetonitrile, HPLC grade.
4.2.2 Isopropanol
4.2.3 Iso-octane
4.2.4 Water deionized, HPLC quality,
4.2.5 Sodium dihydrogen phosphate monohydrate
4.2.6 Sodium hydroxide
4.3 Solutions
4.3.1 Stock solution of 2,4,6-triamino-1,3,5-triazine in water (1 mg/ml)
Weigh to the nearest 0,1 mg approximately 50 mg of 2,4,6-triamino-1,3,5-triazine (4.1) in a 50 ml
volumetric flask and add 40 ml water (4.2.4). Place the flask for 15 min to 30 min in an ultrasonic
water-bath at 70 °C to dissolve the 2,4,6-triamino-1,3,5-triazine. Cool the solution to room
temperature and fill the volumetric flask up to the mark with water (4.2.4).
Calculate the actual concentration in milligrams of 2,4,6-triamino-1,3,5-triazine per millilitre of solution.
Repeat the procedure to obtain a second stock solution.
Store the solution in a well closed container in dark for a maximum period of 3 months at any
temperature between - 20 °C and + 20 °C.
2,4,6-triamino-1,3,5-triazine is only slightly soluble in water, therefore assure that all 2,4,6-triamino-
1,3,5-triazine is dissolved. Preparation of more concentrated stock solutions is not feasible.
4.3.2 Diluted standard solutions of 2,4,6-triamino-1,3,5-triazine in aqueous food simulants
(0,1 mg/ml)
Pipette 5 ml of the stock solution (4.3.1) into a 50 ml volumetric flask. Make up to the mark with the
appropriate food simulant.
Calculate the actual concentration in milligrams of 2,4,6-triamino-1,3,5-triazine per millilitre of solution.
Repeat the procedure using the second standard stock solution to obtain a second set of diluted
standard solutions.
4.3.3 Standard solution of 2,4,6-triamino-1,3,5-triazine in isopropanol/water
Pipette, into a series of 25 ml volumetric flasks, 0 ml, 0,5 ml, 1 ml, 2 ml, 4 ml and 8 ml of the stock
solution (4.3.1). Add 12,5 ml isopropanol (4.2.2) and make up to the mark with water (4.2.4).
The standard solutions thus obtained contain 0 µg/ml, 20 µg/ml, 40 µg/ml, 80 µg/ml, 160 µg/ml, and
3
...

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