Textiles and textile products - Determination of biocide additives - Part 2: Chlorophenol-based preservatives, method using gas chromatography

This document specifies a test method using gas chromatography with a mass selective detector (GC-MS) for detection and quantification of chlorophenols (CPs), which are either freely present or released from salts and esters: pentachlorophenol (PCP), tetrachlorophenol- (TeCP), trichlorophenol- (TriCP), dichlorophenol- (DiCP) and monochlorophenol- (MoCP) isomers. The method is applicable to textile fibres, yarns, fabrics, coated fabrics, printed fabrics, plastic, and wooden parts of textile products (for example buttons).

Textilien und textile Erzeugnisse - Bestimmung von Biozid-Zusatzstoffen - Teil 2: Konservierungsmittel auf Chlorphenolbasis, Verfahren mittels Gaschromatographie

Dieses Dokument legt ein Prüfverfahren zur Bestimmung und Quantifizierung von Chlorphenolen (CP), die entweder frei vorhanden sind oder aus Salzen und Estern freigesetzt werden, mittels Gaschromatographie mit massenselektivem Detektor (GC MS) fest: Pentachlorphenol  (PCP), Tetrachlorphenol  (TeCP), Trichlorphenol  (TriCP), Dichlorphenol  (DiCP) und Monochlorphenol  (MoCP) Isomere. Das Verfahren ist anwendbar für Textilfasern, Garne, Gewebe, beschichtetes Gewebe, bedrucktes Gewebe sowie Kunststoff  und Holzteile von Textilerzeugnissen (beispielsweise Knöpfe).

Textiles et produits textiles - Détermination des additifs biocides - Partie 2 : Conservateurs à base de chlorophénol, méthode par chromatographie en phase gazeuse

Le présent document spécifie une méthode d’essai utilisant la chromatographie en phase gazeuse à détecteur sélectif de masse (CG-SM) pour la détection et la quantification des chlorophénols (CP), qui sont soit présents librement, soit libérés à partir de sels et d’esters : isomères de pentachlorophénol (PCP), tétrachlorophénol (TeCP), trichlorophénol (TriCP), dichlorophénol (DiCP) et monochlorophénol (MoCP). La méthode est applicable aux fibres textiles, aux fils, aux étoffes, aux étoffes enduites, aux étoffes imprimées, au plastique et aux parties en bois des produits textiles (par exemple, boutons).

Tekstilije in tekstilni izdelki - Določevanje biocidnega dodatka - 2. del: Konzervansi na osnovi klorofenola, metoda z uporabo plinske kromatografije

Ta dokument določa preskusno metodo za določanje vsebnosti konzervansov na osnovi klorofenola v tekstilnih materialih in kosih, ki jih sestavljajo tekstilni izdelki, pri kateri se uporablja kromatografija.

General Information

Status
Published
Publication Date
18-Jul-2023
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
19-Jul-2023
Due Date
29-Aug-2022
Completion Date
19-Jul-2023

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SLOVENSKI STANDARD
01-september-2023
Tekstilije in tekstilni izdelki - Določevanje biocidnega dodatka - 2. del: Konzervansi
na osnovi klorofenola, metoda z uporabo plinske kromatografije
Textiles and textile products - Determination of biocide additives - Part 2: Chlorophenol-
based preservatives, method using gas chromatography
Textilien und textile Erzeugnisse - Bestimmung von Biozid-Zusatzstoffen - Teil 2:
Konservierungsmittel auf Chlorphenolbasis, Verfahren mittels Gaschromatographie
Textiles et produits textiles - Détermination des additifs biocides - Partie 2 :
Conservateurs à base de chlorophénol, méthode par chromatographie en phase
gazeuse
Ta slovenski standard je istoveten z: EN 17134-2:2023
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17134-2
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2023
EUROPÄISCHE NORM
ICS 59.080.01 Supersedes EN 17134:2019
English Version
Textiles and textile products - Determination of biocide
additives - Part 2: Chlorophenol-based preservatives,
method using gas chromatography
Textiles et produits textiles - Détermination des Textilien und textile Erzeugnisse - Bestimmung von
additifs biocides - Partie 2 : Conservateurs à base de Biozid-Zusatzstoffen - Teil 2: Konservierungsmittel auf
chlorophénol, méthode par chromatographie en phase Chlorphenolbasis, Verfahren mittels
gazeuse Gaschromatographie
This European Standard was approved by CEN on 12 June 2023.

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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17134-2:2023 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Principle . 6
5 Reagents . 6
6 Apparatus .10
7 Preparation of test samples and test specimens .10
8 Procedure.10
8.1 Extraction with KOH .10
8.2 Acetylation of extracted CPs .11
8.2.1 General procedure of acetylation .11
8.2.2 Preparation for GC analysis .11
8.2.3 Acetylation in case of low recovery rates .11
8.3 Acetylation of the calibration standards .11
8.4 Gas chromatography with mass selective detection .11
9 Expression of results .11
9.1 General .11
9.2 Calculation of the individual chlorophenols .12
9.3 Sum of chlorophenols .12
9.4 Precision of the test method .12
10 Test report .12
Annex A (informative) Example of parameters for GC-MS determination of CPs .13
A.1 Measuring technique .13
A.2 Chromatographic conditions .13
A.3 MS conditions .13
Annex B (informative) Reliability of the method.15
B.1 General .15
B.2 Results of interlaboratory trials .16
B.2.1 Results of the first interlaboratory trial .16
B.2.2 Results of the second interlaboratory trial from one real test specimen and two
spikes of the real test specimen, with 4 laboratories .17
B.3 Influence of standard solutions .24
B.4 Influence of internal standards on the results of pentachlorophenol and other
chlorophenols .29
Annex C (informative) Test method for free mono- and dichlorophenols .37
C.1 General .37
C.2 Reagents . 37
C.3 Apparatus . 37
C.4 Preparation of test samples . 37
C.5 Procedure . 37
C.5.1 Extraction and acetylation of extracted CPs . 37
C.5.2 Acetylation of the calibration standards . 37
C.6 Expression of results . 38
C.7 Test report . 38
Bibliography . 39

European foreword
This document (EN 17134-2:2023) 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 January 2024, and conflicting national standards shall
be withdrawn at the latest by January 2024.
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 17134:2019.
This document is part of a series of documents:
EN 17134-1 , Textiles and textile products — Determination of biocide additives — Part 1: 2-Phenylphenol
and triclosan, method using liquid chromatography
EN 17134-2, Textiles and textile products — Determination of biocide additives — Part 2: Chlorophenol-
based preservatives, method using gas chromatography
EN 17134-3 , Textiles and textile products — Determination of biocide additives — Part 3: Permethrin,
method using liquid chromatography
A list of all parts in a series can be found on the CEN website: www.cencenelec.eu.
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.
Under preparation. Stage at the time of publication: prEN 17134-1:2023.
Under preparation. Stage at the time of publication: prEN 17134-3:2023.
Introduction
In Europe, according to Regulation (EU) 2019/1021 of the European Parliament and of the Council of 20
June 2019 on persistent organic pollutants [1] pentachlorophenol (PCP) and its salts and esters as
constituents of articles are prohibited. According to Commission Delegated Regulation (EU) 2021/277 of
16 December 2020 amending Annex I to Regulation (EU) 2019/1021 of the European Parliament and of
the Council on persistent organic pollutants as regards pentachlorophenol and its salts and esters [2],
articles containing PCP in concentrations equal or lower than 5 mg/kg are allowed.
Further chlorinated phenols are restricted by voluntary specifications (ecolabel criteria, industry
initiatives and standards).
WARNING — The use of this document involves hazardous materials. It does not purport to address all
of the safety or environmental problems associated with its use. It is the responsibility of users of this
document to take appropriate measures to ensure the safety and health of personnel and the
environment prior to application of the document and fulfil statutory and regulatory requirements for
this purpose.
1 Scope
This document specifies a test method using gas chromatography with a mass selective detector (GC-MS)
for detection and quantification of chlorophenols (CPs), which are either freely present or released from
salts and esters: pentachlorophenol (PCP), tetrachlorophenol- (TeCP), trichlorophenol- (TriCP),
dichlorophenol- (DiCP) and monochlorophenol- (MoCP) isomers. The method is applicable to textile
fibres, yarns, fabrics, coated fabrics, printed fabrics, plastic, and wooden parts of textile products (for
example buttons).
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 methods (ISO 3696)
EN ISO 4787, Laboratory glass and plastic ware - Volumetric instruments - Methods for testing of capacity
and for u
...

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