Textiles and textile products - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes

This document specifies a test method using gas chromatography with mass selective detector (GC-MS) for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in fibres, yarns, fabrics, coated fabrics and plastics.

Textilien und textile Erzeugnisse - Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzolen und Chlortoluolen

Dieses Dokument legt ein auf Gaschromatographie mit massenselektivem Detektor (GC MS) beruhendes Prüfverfahren für den Nachweis und die quantitative Bestimmung von Chlorbenzolen, Chlortoluolen und α chlorierten Toluolen in Fasern, Garnen, textilen Flächengebilden, beschichteten Geweben und Kunststoffen fest.

Textiles et produits textiles - Détermination de la teneur de composés à base de chlorobenzènes et chlorotoluènes

Le présent document spécifie une méthode d’essai utilisant la chromatographie en phase gazeuse avec détecteur sélectif de masse (GC MS) pour la détection et la quantification des chlorobenzènes, des chlorotoluènes et des toluènes α chlorés dans les fibres, les fils, les supports textiles, les supports textiles revêtus et les matières plastiques.

Tekstilije - Določanje spojin na osnovi klorobenzenov in klorotoluenov

General Information

Status
Published
Publication Date
05-Nov-2024
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
06-Nov-2024
Due Date
05-Mar-2025
Completion Date
06-Nov-2024

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SLOVENSKI STANDARD
01-januar-2025
Tekstilije - Določanje spojin na osnovi klorobenzenov in klorotoluenov
Textiles - Determination of the content of compounds based on chlorobenzenes and
chlorotoluenes
Textilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von
Chlorbenzolen und Chlortoluolen
Textiles et produits textiles - Détermination de la teneur de composés à base de
chlorobenzènes et chlorotoluènes
Ta slovenski standard je istoveten z: EN 17137:2024
ICS:
59.080.01 Tekstilije na splošno Textiles in general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17137
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2024
EUROPÄISCHE NORM
ICS 59.080.01 Supersedes EN 17137:2018
English Version
Textiles and textile products - Determination of the
content of compounds based on chlorobenzenes and
chlorotoluenes
Textiles et produits textiles - Détermination de la Textilien und textile Erzeugnisse - Bestimmung des
teneur de composés à base de chlorobenzènes et Gehaltes von Verbindungen auf der Basis von
chlorotoluènes Chlorbenzolen und Chlortoluolen
This European Standard was approved by CEN on 6 October 2024.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17137:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Reagents . 5
6 Apparatus . 7
7 Preparation of test specimens . 7
8 Procedure . 8
8.1 Extraction . 8
8.2 Determination by GC-MS or GC-MS/MS . 8
9 Expression of results . 8
9.1 Calculation . 8
9.2 Sum of chlorobenzenes and chlorotoluenes . 9
9.3 Reliability of the method . 9
10 Test report . 9
Annex A (informative) “False positives” . 10
Annex B (informative) Test procedures if “false positive” results of benzyl chloride derived from
benzalkonium chloride are suspected . 12
Annex C (informative) Parameter for instrumental analyses . 15
Annex D (informative) Reliability of the method . 19
Bibliography . 21

European foreword
This document (EN 17137:2024) has been prepared by Technical Committee CEN/TC 248 “Textiles and
textile products”, the secretariat of which is held by BSI.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by May 2025, and conflicting national standards shall be
withdrawn at the latest by May 2025.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 17137:2018.
— The clauses have been reorganised and renamed according to CEN/CENELEC Internal Regulations
Part 3:2022;
— Clause 1: The scope has been extended to α-chlorinated toluenes and rephrased;
— Clause 2: EN ISO 4787 has been added;
— 3.1 and 3.2 have been deleted;
— Clause 4 has been rephrased;
— Clause 5 has been reorganised and rephrased;
— 5.2: Several α-chlorinated toluenes have been added in Table 1, and Table 1 has been reorganised;
— Clause 6 has been reorganised and rephrased;
— 6.6: Triple-quadrupole mass spectrometer has been added as a suitable detector;
— Clause 7 and Clause 8 have been reorganised and rephrased;
— 9.2: A clause on how to calculate the sum of chlorobenzenes and chlorotoluenes has been added;
— 9.3: The limit of quantification of the test method has been given;
— Clause 10 has been reorganised and rephrased;
— a new Annex A: with description on the occurrence of “false positives” has been added;
— a new Annex B with test procedure if “false positives” are suspected has been added;
— Annex C: Former Annex A has become Annex C;
— Table C.1: The description of the injection temperature has been amended;
— Table C.2: Examples of quantifier and qualifier ions have been revised and retention times have been
removed;
— C.2: Instrumental conditions and characteristic masses for quantification with mass
chromatograph/triple quad mass spectrometer (GC-MS/MS) have been added;
— Annex D: Former Annex B has become Annex D, has been revised and statistical data have been
adopted from the reports on two proficiency tests by the Institute for Interlaboratory Studies;
— Bibliography: Further references have been added.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
1 Scope
This document specifies a test method using gas chromatography with mass selective detector (GC-MS)
for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in fibres,
yarns, fabrics, coated fabrics and plastics.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 ISO 4787, Laboratory glass and plastic ware — Volumetric instruments — Methods for testing of
capacity and for use (ISO 4787)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp/
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
The sample is cut into small pieces and extracted with dichloromethane in a sealed vial at a defined
temperature in an ultrasonic bath. An aliquot of the extract is analysed for the compounds listed in
Table 1 using a GC-MS.
NOTE CEN/TR 16741 specifies which materials are applicable to this test method.
5 Reagents
Unless otherwise specified, all reagents shall be of a recognized analytical grade.
®1 ®
5.1 Dichloromethane, CAS Registry Number (CAS RN ) 75-09-2.
5.2 Reference compounds.
Reference compounds are listed in Table 1.
Table 1 — Reference compounds
Compound ®
Compound CAS RN
number
Chlorobenzenes
1 Chlorobenzene 108–90–7
2 1,2-Dichlorobenzene 95–50–1
3 1,3-Dichlorobenzene 541–73–1

1 ® ®
CAS Registry Number (CAS RN ) is a trademark of the American Chemical Society (ACS). This information is
given for the convenience of users of this document and does not constitute an endorsement by CEN of the product
named. Equivalent products may be used if they can be shown to lead to the same results.
Compound ®
Compound
CAS RN
number
4 1,4-Dichlorobenzene 106–46–7
5 1,2,3-Trichlorobenzene 87–61–6
6 1,2,4-Trichlorobenzene 120–82–1
7 1,3,5-Trichlorobenzene 108–70–3
8 1,2,3,4-Tetrachlorobenzene 634–66–2
9 1,2,3,5-Tetrachlorobenzene 634–90–2
10 1,2,4,5-Tetrachlorobenzene 95–94–3
11 Pentachlorobenzene 608–93–5
12 Hexachlorobenzene 118–74–1
Chlorotoluenes
13 2-Chlorotoluene 95–49–8
14 3-Chlorotoluene 108–41–8
15 4-Chlorotoluene 106–43–4
16 2,3-Dichlorotoluene 32768–54–0
17 2,4-Dichlorotoluene 95–73–8
18 2,5-Dichlorotoluene 19398–61–9
19 2,6-Dichlorotoluene 118–69–4
20 3,4-Dichlorotoluene 95–75–0
21 3,5-Dichlorotoluene 25186–47–4
22 2,3,4-Trichlorotoluene 7359–72–0
23 2,3,5-Trichlorotoluene 56961–86–5
24 2,3,6-Trichlorotoluene 2077–46–5
25 2,4,5-Trichlorotoluene 6639–30–1
26 3,4,5-Trichlorotoluene 21472–86–6
27 2,3,4,5-Tetrachlorotoluene 1006–32–2
28 2,3,4,6-Tetrachlorotoluene 875–40–1
29 2,3,5,6-Tetrachlorotoluene 1006–31–1
30 Pentachlorotoluene 877–11–2
α-chlorinated toluenes
31 α-Chlorotoluene 100–44–7
32 α,α- Dichlorotoluene 98–87–3
33 α,α,α -Trichlorotoluene 98–07–7
34 α,α,2,6-Tetrachlorotoluene 81–19–6
35 α,α,α,2-Tetrachlorotoluene 2136–89–2
36 α,α,α,4-Tetrachlorotoluene 5216–25–1
Internal standard (IS)
37 2,4,5,6-Tetrachloro-m-xylene 877–09–8
5.3 Standard solutions
5.3.1 Target compound stock solutions
Based on its tasks, a laboratory shall decide which compounds from Table 1 need to be determined. Based
on this decision, standard stock solutions for each compound (for example, c = 100 μg/ml for each
compound) shall be available either as commercially available certified mixes or individual components
in solution or as self-prepared individual or mixed standard stock solutions of each compound (Table 1)
in dichloromethane (5.1).
EXAMPLE For standard stock solutions with concentrations of 100 μg/ml, 25,0 mg of each compound
(Table 1) is weighed into a 250 ml volumetric flask, filled up to the mark with dichloromethane (5.1) and mixed
thoroughly to dissolve the compound completely.
5.3.2 Target compound working solution
Prepare a mixed working solution containing all required compounds in a suitable concentration for the
GC-MS system used (for example, c = 10 µg/ml).
5.3.3 Internal standard solution
Prepare an internal standard (IS) solution of a suitable concentration for the GC-MS system used (for
example, c = 1 µg/ml) by dissolving 2,4,5,6-tetrachloro-m-xylene (Table 1, Compound number 37) in
dichloromethane (5.1).
6 Apparatus
The usual laboratory apparatus and laboratory glassware, according to EN ISO 4787, shall be used, in
addition to the following:
6.1 Analytical balance, with a resolution of at least 0,1 mg.
6.2 Glass vials with tight closure, for example, 40 ml.
6.3 Ultrasonic bath.
...

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