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 - Določevanje spojin na osnovi klorobenzenov in klorotoluenov

General Information

Status
Not Published
Publication Date
30-Oct-2024
Current Stage
5020 - Submission to Vote - Formal Approval
Start Date
11-Jul-2024
Due Date
13-Nov-2024
Completion Date
11-Jul-2024

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SLOVENSKI STANDARD
01-september-2023
Tekstilije - Določevanje 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: prEN 17137
ICS:
59.080.01 Tekstilije na splošno Textiles in general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
prEN 17137
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2023
ICS Will supersede EN 17137:2018
English Version
Textiles - Determination of the content of compounds
based on chlorobenzenes and chlorotoluenes
Textiles - Détermination de la teneur de composés à Textilien - Bestimmung des Gehaltes von
base de chlorobenzènes et chlorotoluènes Verbindungen auf der Basis von Chlorbenzol und
Chlortoluol
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 248.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17137:2023 E
worldwide for CEN national Members.

prEN 17137:2023 (E)
Contents Page
European foreword . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Reagents . 5
6 Apparatus . 7
7 Sampling . 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
A.1 False positives . 10
A.2 Occurrences of chlorobenzenes and chlorotoluenes . 10
A.3 Examples of false positives (not exhaustive) . 10
A.3.1 α-Chlorotoluene (benzyl chloride) as a degradation product of quaternary
ammonium salts . 10
[2]
A.3.2 1,2-Dichlorobenzene findings from synthesis residues . 10
A.3.3 Chlorobenzenes and chlorotoluenes released by dyestuff as degradation products . 11
Annex B (informative) Test procedures if false positive results of benzyl chloride derived
from benzalkonium chloride are suspected . 12
B.1 Confirmation of benzyl chloride derived from benzalkonium chloride by LC-DAD . 12
B.1.1 Principle . 12
B.1.2 Reagents . 12
B.1.2.1 Water, grade 3 according to EN ISO 3696 or LC-MS grade. . 12
B.1.2.2 Methanol, LC-MS grade, CAS number 67-56-1 . 12
B.1.2.3 Ammonium formate, CAS number 540-69-2 . 12
B.1.2.4 Benzyl chloride, CAS number 100-44-7 . 12
B.1.2.5 Benzalkonium Chloride, CAS number 63449-41-2 (for qualitative screening) . 12
prEN 17137:2023 (E)
B.1.3 Apparatus . 12
B.1.3.1 Liquid Chromatograph with Diode-Array Detection (LC-DAD). . 12
B.1.4 Procedure . 12
B.1.4.1 Sampling Procedure . 12
B.1.4.2 Extraction . 12
B.1.4.3 Calculation . 13
B.1.4.4 Chromatography parameters (example) . 13
B.2 Removal of benzalkonium chloride by water extraction with subsequent GC-MS
analysis . 14
Annex C (informative) Parameter for instrumental analyses . 15
C.1 Gas chromatograph/single quad mass spectrometer (GC-MS) . 15
C.2 Gas chromatograph/triple quad mass spectrometer (GC-MS/MS) . 17
Annex D (informative) Reliability of the method . 19
D.1 General . 19
D.2 Accuracy . 19
D.3 Detection Limit (LOD) and Quantification Limit (LOQ) . 20
D.4 Repeatability . 21
D.5 Reproducibility . 22
D.6 Robustness . 23
D.7 Selectivity . 24
D.8 Extraction Efficiency . 25
Bibliography . 26

prEN 17137:2023 (E)
European foreword
This document (prEN 17137:2023) has been prepared by Technical Committee CEN/TC 248 “Textiles
and textile products”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 17137:2018.
prEN 17137:2023 includes the following significant technical changes with respect to EN 17137:2018:
– The clauses have been reorganised and renamed according to CEN/CENELEC Internal Regulations
Part 3:2019;
– Clause 1: The scope has been extended to α-chlorinated toluenes and rephrased;
– Clause 2: EN ISO 4787 has been added;
– Subclauses 3.1 and 3.2 have been deleted;
– Clause 4 has been rephrased;
– Clause 5 has been reorganised and rephrased;
– Subclause 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;
– Subclause 6.6: Triple-quadrupole mass spectrometer has been added as a suitable detector;
– Clause 7 has been reorganised and rephrased;
– Clause 8 has been reorganised and rephrased;
– Subclause 9.2: A clause on how to calculate the sum of chlorobenzenes and chlorotoluenes has been
added;
– Subclause 9.3: The limit of quantification of the test method is given;
– Clause 10 has been reorganised and rephrased;
– Annex A: A description on the occurrence of false positives has been added;
– Annex B: Test procedure if false positives are suspected has been added;
– Annex C: Former Annex A has become Annex C,
– Annex 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;
– Bibliography: Further references have been added.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Republic of North Macedonia, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands,
Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
the United Kingdom.
prEN 17137:2023 (E)
1 Scope
This document specifies a test method using gas chromatography with mass selective detector (GC-
MSD) for detection and quantification of chlorobenzenes, chlorotoluenes, and α-chlorinated toluenes in
fibres, yarns, fabrics, coated fabrics and plastics.
NOTE 1 CEN/TR 16741 defines which materials are applicable to this test method.
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 3696, Water for analytical laboratory use - Specification and test
...

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