SIST-TS CEN/TS 13130-19:2005

Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 19: Determination of dimethylaminoethanol in food simulants

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.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 19: Bestimmung von Dimethylaminoethanol in Prüflebensmitteln

Diese Technische Spezifikation, Teil der EN 13130, legt ein Analyseverfahren zur Bestimmung von Dimethylaminoethanol in den Prüflebensmitteln destilliertes Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung und rektifiziertes Olivenöl fest. Das Verfahren eignet sich zur quantitativen Bestimmung von Dimethylaminoethanol im angenäherten Konzentrationsbereich des Analyten von 3,4 mg/kg bis 36 mg je Kilogramm Prüflebensmittel.
ANMERKUNG   Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebensmittel, wie z. B. Sonnenblumenöl und 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 19 : Détermination du diméthylaminoéthanol dans les simulants d'aliments

Le présent document qui fait partie de l'EN 13130, spécifie un mode opératoire d'analyse pour la détermination des résidus de diméthylaminoéthanol dans les 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. Cette méthode convient pour la détermination quantitative du diméthylaminoéthanol dans une gamme de concentrations en analyte comprise approximativement entre 3,4 mg et 36 mg par kilogramme 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 ou un mélange de triglycérides synthétiques.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 19. del: Določevanje dimetilaminoetanola v modelnih raztopinah za živila

General Information

• Status: Published
• Publication Date: 31-Mar-2005
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: EPO - Packaging - sales and grouped
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Apr-2005
• Due Date: 01-Apr-2005
• Completion Date: 01-Apr-2005
• Ref Project: CEN/TS 13130-19:2005 - Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 19: Determination of dimethylaminoethanol in food simulants

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-19:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHGLPHWLODPLQRHWDQRODYPRGHOQLK
UD]WRSLQDK]DåLYLOD
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 19: Determination of dimethylaminoethanol in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 19: Bestimmung von Dimethylaminoethanol in
Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 19 : Détermination du
diméthylaminoéthanol dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-19:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-19:2005 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 13130-19:2005

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SIST-TS CEN/TS 13130-19:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-19
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 19: Determination of
dimethylaminoethanol 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 19 : Détermination du unterliegen - Teil 19: Bestimmung von
diméthylaminoéthanol dans les simulants d'aliments Dimethylaminoethanol 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 13130-19:2005: E
worldwide for CEN national Members.

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SIST-TS CEN/TS 13130-19:2005
CEN/TS 13130-19:2005 (E)
Contents
page
Foreword. 3
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Principle . 6
4 Reagents . 7
5 Apparatus . 8
6 Samples . 9
7 Procedure . 11
8 Precision . 13
9 Confirmation. 13
10 Test report . 14
Bibliography . 15

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SIST-TS CEN/TS 13130-19:2005
CEN/TS 13130-19:2005 (E)
Foreword
This document (CEN/TS 13130-19:2005) 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
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CEN/TS 13130-19:2005 (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.
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SIST-TS CEN/TS 13130-19:2005
CEN/TS 13130-19:2005 (E)
Introduction
Dimethylaminoethanol (DMAE), C H NO, PM/Ref. No 16150, is a monomer used in the manufacture of
4 11
certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture
residual dimethylaminoethanol can remain in the finished product and may migrate into foodstuffs
coming into contact with that product.
The method has been pre-validated by collaborative trial with two laboratories using food simulants.
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SIST-TS CEN/TS 13130-19:2005
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1 Scope
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.
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
Dimethylaminoethanol (DMAE) is extracted from the food simulants by means of solid phase extraction
on a strong cation exchanger. The absorbed DMAE is removed from the absorbent with triethylamine
and the resulting solution is submitted to gas chromatography to determine the amount of DMAE in the
simulants. For quantification purposes an internal standard is added. Calibration is achieved by analysis
of relevant simulants containing known amounts of DMAE.
Confirmation of dimethylaminoethanol is established by combined gas chromatography/mass
spectrometry.
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SIST-TS CEN/TS 13130-19:2005
CEN/TS 13130-19:2005 (E)
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analytes
4.1.1 Dimethylaminoethanol (DMAE), N,N-dimethylethanol-amine, C HNO or
4 11
(CH ) NCH CH OH molecular weight 89,14; boiling point 134 °C; density: 0,886 6 g per millilitre, purity:
3 2 2 2
> 99 % (GC).
4.1.2 Diethylaminoethanol (DEAE), (N,N-diethyl-ethanolamine) C H NO or (C H ) NCH CH OH
6 15 2 5 2 2 2
Molecular weight 117,19; boiling point 163 °C; density: 0,8921 g per millilitre, purity: > 99 % (GC).
4.2 Chemicals
4.2.1 Water, deionized or HPLC grade.
4.2.2 Acetic acid, 100 %.
4.2.3 Methanol, HPLC grade.
4.2.4 Isopropanol, HPLC grade.
4.2.5 n-Pentane, 95 %.
4.2.6 Triethylamine, > 99 %, GC.
4.3 Solid phase extraction cartridges, loaded with 100 mg of a strong cation exchanger
(propylsulfonic acid) and a volume of 3 ml.
4.4 Solutions
4.4.1 Triethylamine in methanol, 5 % (v/v)
Measure 2,0 ml triethylamine (4.2.6) and add methanol to a final volume of 50 ml in a volumetric flask.
4.4.2 Standard stock solution of DMAE in isopropanol at a defined concentration of
approximately 2,22 g/l
Pipette exactly 0,250 ml or weigh accurately approximately 222 mg of DMAE (4.1.1) into a 100 ml
volumetric flask and fill to the mark with isopropanol.
Calculate the exact concentration of DMAE in milligrams per millilitre using the specific mass of DMAE
or the actual mass taken.
Repeat the procedure to obtain a second standard stock solution.
NOTE The stock solutions can be stored in a well closed containers in the dark for a maximum period of
three months at any temperature between - 20 °C and + 20 °C.
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CEN/TS 13130-19:2005 (E)
4.4.3 Internal standard stock solution of diethylaminoethanol (DEAE) in isopropanol at a
defined concentration of approximately 2,22 g/l
Pipette exactly 0,250 ml or weigh accurately approximately 222 mg of DEAE (4.1.2) into a 100 ml
volumetric flask and fill to the mark with isopropanol.
Calculate the exact concentration of DEAE in mg/ml using the specific mass of DEAE or the actual mass
taken.
NOTE The stock solutions can be stored in a well closed container in dark for a maximum period of three
months at any temperature between - 20 °C and + 20 °C.
4.4.4 Diluted standard solution of DMAE in isopropanol (0,22 mg/ml)
Pipette 2,5 ml of the DMAE standard stock solution 4.4.2 into a 25 ml volumetric flask and fill to the mark
with isopropanol. This solution contains approximately 222 µg DMAE per millilitre of isopropanol.
Calculate the exact concentration of DMAE in micrograms per millilitre of solution.
Repeat the procedure using the second stock solution.
NOTE The solution can be stored in a well closed container in dark for a maximum period of three months at
any temperature between - 20 °C and + 20 °C.
4.4.5 Diluted internal standard solution of DEAE in isopropanol (0,222 mg/ml)
Pipette 2,5 ml of the DEAE internal standard stock solution 4.4.3 into a 25 ml volumetric flask and fill to
the mark with isopropanol. This solution contains approximately 222 µg DEAE per millilitre of
isopropanol.
Calculate the exact concentration of DEAE in µg/ml solution.
NOTE The solution can be stored in a well closed container in the dark for a maximum period of three
months at any temperature between - 20 °C and + 20 °C.
5 Apparatus
NOTE An instrument or item of apparatus is listed only where it is special or made to a particular
specification, usual laboratory glassware and equipment being assumed to be available.
5.1 Gas chromatograph, equipped with a flame ionization detector (FID) and preferably with an
automatic injection sampler, capable of separating DMAE fully from DEAE as well as from peaks
originating from simulants and/or solvents used.
Appropriate operating conditions shall be established for the specific equipment used for the
determination.
NOTE The following chromatographic columns and conditions have been found to be satisfactory:
Column 1
25 m x 0,32 mm fused silica WCOT provided with a 0,5 µm thick layer of dimethylpolysiloxane.
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SIST-TS CEN/TS 13130-19:2005
CEN/TS 13130-19:2005 (E)
GC parameters
Column oven In
...