CEN/TS 13130-23:2005

SLOVENSKI STANDARD
01-april-2005
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Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 23: Bestimmung von Formaldehyd und
Hexamethylentetramin in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 23 : Détermination du
formaldéhyde et de l'hexaméthylenetétramine dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-23:2005
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 13130-23
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 23: Determination of
formaldehyde and hexamethylenetetramine 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 23 : Détermination du unterliegen - Teil 23: Bestimmung von Formaldehyd und
formaldéhyde et de l'hexaméthylènetétramine dans les Hexamethylentetramin in Prüflebensmitteln
simulants d'aliments
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 13130-23:2005: 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.8
6 Samples.9
7 Procedure.10
8 Precision .12
9 Confirmation .13
10 Test report.15
Bibliography.16

Foreword
This document (CEN/TS 13130-23:2005) 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
Formaldehyde, CH O, PM/Ref. No 17260, and hexamethylenetetramine, C H N , PM/Ref. No 18670, are
2 6 12 4
monomers used in the manufacture of certain plastics materials and articles intended to come into contact
with foodstuffs. After manufacture residual formaldehyde or residual hexamethylenetetramine (HMTA) can
remain in the finished product and may migrate into foodstuffs coming into contact with that product.
Since migration of HMTA is limited as formaldehyde, this method allows the determination of formaldehyde,
liberated from HMTA, in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and
rectified olive oil.
The chemical conversion of HMTA to formaldehyde is as follows:
C H N + 6 H O → 6 CH O + 4 NH
6 12 4 2 2 3
The method allows the determination of HMTA and formaldehyde at the same time.
The method has been pre-validated by collaborative trial with two laboratories. The confirmation procedure
was found to be quantitative. In collaborative trials with three laboratories comparable results using the
chromotropic acid method and the acetyl acetone method were found for the detection limits, repeatability,
recovery and migration of formaldehyde. Therefore the method of determination and the confirmation
procedure are interchangeable.
1 Scope
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.
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
HMTA is treated with acid and heated to release formaldehyde.
Formaldehyde in food simulant is determined by spectrophotometry. Formaldehyde reacts with chromotropic
acid in the presence of sulfuric acid. This solution is measured in a spectrophotometer at the wavelength of
574 nm, with cells of an optical path length of 10 mm. Quantification is achieved using an external standard.
Confirmation of formaldehyde is carried out by spectrophotometer. Formaldehyde reacts with
pentane-2,4-dione in the presence of ammonium acetate to form 3,5-diacetyl-1,4-dihydrolutidine. The
absorption of this extract is measured at 410 nm, with a spectrophotometer with cells of an optical path length
of 10 mm.
NOTE The confirmation procedure is also a quantitative method and can therefore be used as the method of
determination. In that case the method with chromotropic acid should be used as the confirmation procedure.
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analyte
Formaldehyde solution, CH O, minimum 37 % (w/v), stabilized with approximately 10 % methanol.
CEN/TS 13130-23
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