SIST-TS CEN/TS 13130-22:2005

SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-22:2005
01-april-2005
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Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 22: Determination of ethylene oxide and propylene oxide in plastics
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 22: Bestimmung von Ethylenoxid und
Propylenoxid in Kunststoffen
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 22 : Détermination des oxydes
d'éthylene et de propylene dans les matieres plastiques
Ta slovenski standard je istoveten z: CEN/TS 13130-22:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-22:2005 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 13130-22:2005

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SIST-TS CEN/TS 13130-22:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-22
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 22: Determination of
ethylene oxide and propylene oxide in plastics
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 22 : Détermination des unterliegen - Teil 22: Bestimmung von Ethylenoxid und
oxydes d'éthylène et de propylène dans les matières Propylenoxid in Kunststoffen
plastiques
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 13130-22:2005: E
worldwide for CEN national Members.

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SIST-TS CEN/TS 13130-22:2005
CEN/TS 13130-22:2005 (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 . 10
8 Precision . 12
9 Confirmation. 12
10 Test report . 13
Annex A (normative)  Calibration via external standardization . 15
Annex B (normative)  Manual sample injection . 16
Bibliography . 17

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SIST-TS CEN/TS 13130-22:2005
CEN/TS 13130-22:2005 (E)
Foreword
This document (CEN/TS 13130-22:2005) 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 13130-22:2005 (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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CEN/TS 13130-22:2005 (E)
Introduction
Ethylene oxide, C H O, PM/Ref. No 17020, and propylene oxide, C H O, PM/Ref. No 24010 are
2 4 3 6
monomers used in the manufacture of certain plastics materials and articles intended to come into
contact with foodstuffs. After manufacture residual ethylene oxide 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.
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1 Scope
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.
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 ethylene oxide and propylene oxide in polymers is determined by headspace gas
chromatography. Quantification is achieved using diethyl ether as an internal standard with calibration
against polymer samples fortified with ethylene oxide or propylene oxide according to the standard
addition procedure.
Confirmation of ethylene oxide is carried out using another column with different polarity.
Confirmation of propylene oxide is carried out by combined gas chromatography/mass spectrometry
(GC/MS).
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SIST-TS CEN/TS 13130-22:2005
CEN/TS 13130-22:2005 (E)
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analytes
4.1.1 Ethylene oxide, C H O of purity greater than 99 % (w/w).
2 4
4.1.2 Propylene oxide, C H O of purity greater than 99 % (w/w).
3 6
4.1.3 Diethyl ether, C H O containing no impurity greater than 1 % by peak area or peak height,
4 10
which elutes at the same retention time as ethylene oxide or propylene oxide.
4.2 Chemical
N,N-dimethylacetamide, distilled, C H NO free of any interferences (< 1 % area) with the ethylene
4 9
oxide or propylene oxide and diethyl ether peak.
4.3 Solutions
4.3.1 Stock solutions of ethylene oxide or propylene oxide in dimethylacetamide
4.3.1.1 Stock solutions of ethylene oxide in dimethylacetamide (2 mg/ml to 6 mg/ml)
Add 50,0 ml dimethylacetamide (4.2) into a 50 ml sample vial and determine the mass including septa
and cap to within 0,1 mg. Introduce 0,1g to 0,3 g ethylene oxide (4.1.1) by bubbling the ethylene oxide
gas (4.1.1) through the dimethylacetamide. Weigh the vial to an accuracy of 0,1 mg. Calculate the
actual concentration in milligrams of ethylene oxide per millilitre of solution.
Repeat the procedure to provide a second stock solution.
NOTE The stock solution can be stored at – 20 °C for up to 3 months protected from light in septum capped
glass vials with minimum headspace or at + 4 °C for up to 8 weeks.
Start by comparing the two stock solutions by making just one dilution of each stock solution. If the
response factor, calculated from the detector response, and the concentration of the solution agree to
within 5 % of one another, further diluted standards shall be made from only one of the stock solutions.
4.3.1.2 Stock solution of propylene oxide in dimethylacetamide (1 mg/ml)
Weigh to the nearest 0,1 mg approximately 50 mg of propylene oxide (4.1.2) into a 50 ml volumetric
flask, which contains approximately 30 ml of dimethylacetamide (4.2). Fill the flask to the mark with
dimethylacetamide and mix carefully.
Calculate the actual concentration in milligrams of propylene oxide per millilitre of solution.
Repeat the procedure to provide a second stock solution.
NOTE The stock solution can be stored at – 20 °C for up to 3 months protected from light in septum capped
glass vials with minimum headspace or at + 4 °C for up to 8 weeks.
Start by comparing the two stock solutions by making just one dilution of each stock solution. If the
response factor, calculated from the detector response, and the concentration of the solution agree to
within 5 % of one another, further diluted standards shall be made from only one of the stock solutions.
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SIST-TS CEN/TS 13130-22:2005
CEN/TS 13130-22:2005 (E)
4.3.2 Diluted standard solution of ethylene oxide or propylene oxide in dimethylacetamide
4.3.2.1 Diluted standard solutions of ethylene oxide in dimethylacetamide (4 µµg/ml to
µµ
40 µµµµg/ml)
Add approximately 8 ml dimethylacetamide into a series of five 10 ml volumetric flasks. Transfer, by
microsyringe, from the stock solution (4.3.1.1) suitable amounts so that the received standard
solutions contain 4 µg/ml, 10 µg/ml, 20 µg/ml, 30 µg/ml and 40 µg/ml solution (0,04 µg/10µl,
0,1 µg/10µl, 0,2 µg/10µl, 0,3 µg/10µl and 0,4 µg/10 µl). Fill the flask to the mark with
dimethylacetamide. Calculate the actual concentrations in micrograms per millilitre of solution.
NOTE The diluted standard solutions can be stored at – 20 °C for up to 3 months protected from light in
septum capped glass vials with minimum headspace or at + 4 °C for up to 8 weeks.
4.3.2.2 Diluted standard solutions of propylene oxide in dimethylacetamide (4 µg /ml to
40 µg/ml)
Add approximately 7 ml dimethylacetamide into a series of five 10 ml volumetric flasks. Transfer,
using a microsyringe, 40 µl, 100 µl, 200 µl, 300 µl and 400 µl from the stock solution (4.3.1
...