SIST-TS CEN/TS 13130-17:2005

SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-17:2005
01-april-2005
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Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 17: Determination of carbonyl chloride in plastics
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 17: Bestimmung von Carbonylchlorid in
Kunststoffen
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 17: Détermination du chlorure de
carbonyle dans les matieres plastiques
Ta slovenski standard je istoveten z: CEN/TS 13130-17:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-17:2005 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 13130-17:2005

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SIST-TS CEN/TS 13130-17:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-17
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 17: Determination of
carbonyl chloride 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 17: Détermination du unterliegen - Teil 17: Bestimmung von Carbonylchlorid in
chlorure de carbonyle dans les matières plastiques Kunststoffen
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 13130-17:2005: E
worldwide for CEN national Members.

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SIST-TS CEN/TS 13130-17:2005
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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 . 11
8 Precision . 14
9 Confirmation. 14
10 Test report . 15
Bibliography . 16

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SIST-TS CEN/TS 13130-17:2005
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Foreword
This document (CEN/TS 13130-17:2005) 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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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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Introduction
Carbonyl chloride or phosgene, CCl O, PM/Ref. No 14380, is a monomer used in the manufacture of
2
certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture,
residual carbonyl chloride can remain in the polymer and may migrate into foodstuffs coming into
contact with the plastics material or article.
The method has been pre-validated by a 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 carbonyl
chloride monomer in polymers. The method is applicable to polycarbonate as well as to other
polymers and copolymers where these are soluble in methylene chloride. The level of carbonyl
chloride monomer determined is expressed as milligrams of carbonyl chloride per kilogram of polymer.
The method is appropriate for the quantitative determination of carbonyl chloride at a minimum level
of 0,3 mg per kilogram 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 carbonyl chloride in the polymer is determined by dissolution of the polymer and
concurrent derivatization with 2-aminophenol. The resulting 2-benzoxazolinone is analyzed by high
performance liquid chromatography (HPLC) with ultra violet (UV) detection. Quantification is achieved
by standard addition of carbonyl chloride to the test polymer. Confirmation of the identity of carbonyl
chloride is carried out by diode array detection.
4 Reagents
NOTE 1 Carbonyl chloride reacts rapidly with moisture. Suitable precautions should be taken to protect
carbonyl chloride solutions from moisture. The carbonyl chloride derivative is not sensitive to moisture.
NOTE 2 All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analytes
4.1.1 Carbonyl chloride, CCl O, molecular weight, 98,9, commercially available as a 20 % (w/w)
2
solution in toluene, density at 20 °C 0,935 kg per litre, corresponding to a concentration of 1,93 mole
per litre or 191 g per litre.
Store the commercial carbonyl chloride solution in a closed container for up to 6 months at + 1 °C in
the dark.
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4.1.2 2-benzoxazolinone, C H NO molecular weight: 135,1, purity 98 %.
7 5 2,
4.2 Chemicals
4.2.1 2-aminophenol (2-hydroxyanilin), C H NO, molecular weight: 109,1, purity 98 %.
6 7
4.2.2 Dichloromethane (DCM), dried over a bed of molecular sieve (5Å), H O < 0,005 %,
2
purity > 99,5 %.
4.2.3 Toluene, dried over a bed of molecular sieve (5Å), H O < 0,005 %, purity > 99,5 %.
2
NOTE The water content of the toluene should be as low as possible. Toluene dried over a molecular sieve
can be obtained from chemical suppliers. Alternatively, toluene can be dried before use, in which case the
molecular sieve should be activated for maximum water absorption.
4.2.4 Methanol
4.2.5 Acetone
4.2.6 Acetonitrile, purity > 99,5 %, HPLC grade
4.2.7 Distilled water, HPLC grade
4.2.8 Sodium dihydrogen orthophosphate, NaH PO . 2H O
2 4 2
4.2.9 Glacial acetic acid
4.2.10 Hydrochloric acid, 1 N
4.2.11 Sodium sulfate, anhydrous
4.2.12 Mobile phase for high performance liquid chromatography, prepared as follows.
Dissolve 7,5 g of sodium dihydrogen orthophosphate (4.2.8) in 700 ml of water (4.2.7), add 250 ml
acetonitrile (4.2.6) using a measuring cylinder and adjust to pH (3,6 ± 0,1) with glacial acetic acid
(4.2.9).
NOTE 1 Approximately 5 ml should be sufficient.
Make up to 1 l with water (4.2.7).
NOTE 2 Degassing the mobile phase may be necessary with some HPLC equipment.
4.3 Solutions
4.3.1 Standard solution of carbonyl chloride in toluene, 95,5 mg/l
Pipette into a 20 ml vial (5.3) 20,0 ± 0,1ml of toluene (4.2.3) and close with the septum and cap. Using
a 10 µl syringe (5.5), add 10 µl of the 20 % carbonyl chloride solution (4.1.1) by injection through the
septum and dispensing after the needle has immersed into the toluene. Remove the syringe and mix.
NOTE 1 The exact concentration of this standard solution is 95,5 mg/l.
Repeat the procedure to provide a second standard solution.
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NOTE 2 This standard solution can be stored at + 4 °C for up to 4 weeks in the dark.
4.3.2 Derivatization reagent solution, 500 µg/ml
Accurately weigh 25 mg ± 0,2 mg of 2-aminophenol (4.2.1) into a 50 ml volumetric flask and add
approximately 45 ml dichloromethane (4.2.2). Close and dissolve the derivatization reagent using an
ultrasonic vibration bath at room temperature. Finally make up to the mark with dichloromethane
(4.2.2), mix and close.
Prepare fresh derivatization reagent solution on the day when required.
4.3.3 Preparation of 2-benzoxazolinone standards in acetonitrile at defined concentrations
between 0,4 µg per millilitre and 7 µg per millilitre
NOTE 1 Preparation and use of benzoxazolinone standards is optional, but are advised when the method is
used for the first time and when problems are experienced in the HPLC determination or the derivatization
procedure.
NOTE 2 The standards of the carbonyl chloride derivative are particularly useful to establish the analytical
system and to check linearity of detector response as well as for the recovery check (7.4.3).
NOTE 3 Benzoxazolinone concentrations can be converted into carbonyl chloride equivalent concentrations
by multiplying by 0,732.
Weigh 22 mg + 2 mg to an accuracy of 0,1 mg into a 10 ml volumetric flask and make up to the mark
with acetonitrile (4.2.6). Close and mix to obtain a standard stock solution of approx 2,2 mg per
millilitre.
Pipette into each of five 10 ml vials 10,0 ml acetonitrile (4.2.6). Add by micro-syringe 2 µl, 6 µl, 10 µl,
20 µl and 30 µl of the 2,2 mg per millilitre benzoxazolinone stock solution, close and mix. The
resulting standard solutions contain approximately 0,44 µg, 1.32 µg, 2,20 µg, 4,40 µg and 6,60 µg
benzoxazolinone per millilitre solution corresponding to 0,32 µg/ml, 0,97 µg/ml, 1,61 µg/ml, 3,22 µg/ml
and 4.83 µg carbonyl chloride equivalents per millilitre of solution.
Calculate the exact concentrations of carbonyl chloride equivalents in milligrams per litre of solution.
NOTE 4 These standard solutions can be stored for maximum 8 weeks at temperatures up to + 10 °C in the
dark.


5 Apparatus
NOTE An instrument or item of apparatus is listed only wher
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