EN 17134-2:2023
(Main)Textiles and textile products - Determination of biocide additives - Part 2: Chlorophenol-based preservatives, method using gas chromatography
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
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 17134-2:2023
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
SIST EN 17134-2:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 17134-2:2023
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SIST EN 17134-2:2023
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.
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EN 17134-2:2023 (E)
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
2
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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
3
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EN 17134-2:2023 (E)
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:
1
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
2
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.
1
Under preparation. Stage at the time of publication: prEN 17134-1:2023.
2
Under preparation. Stage at the time of publication: prEN 17134-3:2023.
4
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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.
5
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EN 17134-2:2023 (E)
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 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 potassium hydroxide (KOH) solution at a defined
temperature. The extracted CPs are subsequently acetylated and the chlorinated acetates are analysed
13 2
and quantified using GC-MS. The quantitative determination is made by corrections with C- and H-
labelled internal standards.
5 Reagents
Unless otherwise specified, all reagents shall be of a recognized analytical grade.
5.1 Water, grade 3, according to EN ISO 3696.
®3 ®
5.2 Potassium hydroxide (KOH), CAS Registry Number (CAS RN ) 1310-58-3.
®
5.3 Potassium carbonate (K CO ), anhydrous, CAS RN 584-08-7.
2 3
®
5.4 n-Hexane, CAS RN 110-54-3.
3 ® ®
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.
6
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®
5.5 Acetic anhydride, CAS RN 108-24-7.
®
5.6 Tetrachloroguaiacol (TCG), CAS RN 2539-17-5, internal standard (IS).
®
5.7 Acetonitrile, CAS RN 75-05-8.
5.8 Chlorophenols
The following 19 CPs given in Table 1 are probably relevant.
Table 1 — List of probably relevant CPs
®
Substance Abbreviation CAS RN
2-chlorophenol 2-MoCP 95-57-8
3-chlorophenol 3-MoCP 108-43-0
4-chlorophenol 4-MoCP 106-48-9
2,3-dichlorophenol 2,3-DiCP 576-24-9
2,4-dichlorophenol 2,4-DiCP 120-83-2
2,5-dichlorophenol 2,5-DiCP 583-78-8
2,6-dichlorophenol 2,6-DiCP 87-65-0
3,4-dichlorophenol 3,4-DiCP 95-77-2
3,5-dichlorophenol 3,5-DiCP 591-35-5
2,3,4-trichlorophenol 2,3,4-TriCP 15950-66-0
2,3,5-trichlorophenol 2,3,5-TriCP 933-78-8
2,3,6-trichlorophenol 2,3,6-TriCP 933-75-5
2,4,5-trichlorophenol 2,4,5-TriCP 95-95-4
2,4,6-trichlorophenol 2,4,6-TriCP 88-06-2
3,4,5-trichlorophenol 3,4,5-TriCP 609-19-8
2,3,4,5-tetrachlorophenol 2,3,4,5-TeCP 4901-51-3
2,3,4,6-tetrachlorophenol 2,3,4,6-TeCP 58-90-2
2,3,5,6-tetrachlorphenol 2,3,5,6-TeCP 935-95-5
Pentachlorophenol PCP 87-86-5
7
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5.9 Isotope labelled chlorophenols
The following 4 isotope labelled CPs given in Table 2 can be relevant as internal standards (IS).
Table 2 — List of probably relevant isotope labelled chlorophenols
®
Substance Abbreviation CAS RN
2-chlorophenol-D 2-MoCP-D 93951-73-6
4 4
2,4-dichlorophenol-D 2,4-DiCP-D 93951-74-7
3 3
13 13
2,3,4,6-tetrachlorophenol- C 2,3,4,6-TeCP- C 1246820-81-4
6 6
13 13
Pentachlorophenol- C PCP- C 85380-74-1
6 6
Instead of the isotope-labelled derivatives of tetra-, di- and monochlorophenol mentioned, other isotope-
labelled analogues of the same chlorination levels, for example 4-chlorophenol-D , may be used as
4
internal standards.
5.10 Potassium hydroxide (KOH) solution (c = 1 mol/l)
Prepare an aqueous KOH solution at a concentration of 1 mol/l.
EXAMPLE Weigh 56,1 g KOH (5.2) into a 1 l volumetric flask and dissolve with 100 ml water (5.1) (WARNING:
heat generation!). After cooling to room temperature fill up to 1 l with water (5.1).
5.11 Internal standard stock solution of isotope-labelled chlorophenols
Based on its requirements a laboratory shall decide which isotope-labelled CPs are required in an internal
standard stock solution.
Table 3 shows which isotope-labelled CPs shall be used as internal standards (IS) for the quantification
of CPs with particular chlorination levels. Alternative IS as outlined in 5.9 may be used.
Table 3 — Assignment of the isotope-labelled CPs to the CP groups
Isotope-labelled CP CP group
2-chlorophenol-D MoCP
4
2,4-dichlorophenol-D DiCP, TriCP
3
13
2,3,4,6-tetrachlorophenol- C6 TeCP
13
Pentachlorophenol- C PCP
6
Prepare a stock solution of the isotope-labelled CPs required at a concentration suitable for the used
analytical system, for example c = 0,1 mg/ml.
EXAMPLE To get a stock solution of isotope-labelled CPs at concentrations of 0,1 mg/ml, dissolve 10 mg of
each required isotope-labelled internal standard (5.9) in 100 ml KOH solution (5.10).
5.12 Extraction solution
The concentration of isotope-labelled CPs shall be adapted to the respective calibration range of the CPs
(see solutions 5.16).
EXAMPLE To prepare 1 l extraction solution with a concentration of each isotope-labelled CP (5.11) of
0,1 µg/ml, transfer 1,0 ml stock solution isotope-labelled CPs (5.11) in a 1 l volumetric flask and fill it up with KOH
8
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solution (5.10). If a more sensitive measuring instrument is used and the calibration is lowered, reduce the
concentration of isotope-labelled internal CPs in the KOH accordingly.
5.13 Potassium carbonate (K CO ) solution (c = 0,1 mol/l).
2 3
Prepare an aqueous K CO solution at a concentration of 0,1 mol/l.
2 3
EXAMPLE Weigh 13,82 g K CO into a 1 l volumetric flask, dissolve with water (5.1) and fill up to the mark.
2 3
5.14 Tetrachloroguaiacol (TCG) solution
Prepare a TCG solution in acetonitrile as internal standard solution for injection control at a
concentration suitable for the used analytical system, for example c = 1 μg/ml.
EXAMPLE Dissolve 10 mg TCG (5.6) in 100 ml acetonitrile (5.7). Take 1,0 ml from this solution and dilute to
100 ml with acetonitrile (5.7).
5.15 CPs standard stock solution
Based on its requirements a laboratory shall decide which CPs from Table 1 in 5.8 need to be determined.
Based on this decision, standard stock solutions at a concentration suitable for the analytical system used
are required. CP standard stock solutions, either as single substance or mixed substance solutions (for
example, c = 50 µg/ml in acetone), are available commercially as certified standard solutions or may be
prepared from certified reference substances.
5.16 CPs calibration solutions
Prepare at least three calibration solutions of CPs from the CP standard stock solution(s) (5.15) at
suitable concentrations for the analysis. Transfer the required volume of CP standard stock solution(s)
(5.15) into a volumetric flask and fill it up to the mark with acetonitrile (5.7). Examples of concentrations
that have been found suitable are provided in Table 4.
Table 4 — Examples of calibration solutions
Volume of
Concentration of CPs
CPs working solution (5.15) Volume of volumetric flask
in calibration solution
(for example c = 50 µg/ml)
µg/ml µl ml
0,15 30
2,0 400 10
4,0 800
15 600
2
25 1 000
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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, weighing with an accuracy of 0,1 mg.
6.2 Gas-tight glass vial, for example 20 ml headspace vial.
6.3 Heating block, sand bath or oven, suitable to maintain the KOH solution at a temperature of
(90 ± 1) °C.
6.4 GC vials, for example 2 ml.
6.5 Pasteur pipettes, graduated pipettes, suitable autopipettes.
6.6 Vortex shaker.
−1
6.7 Horizontal shaker, capable of at least 200 min .
6.8 Centrifuge.
6.9 Gas chromatograph with mass selective detector (GC-MS).
7 Preparation of test samples and test specimens
Dismantle the textile product and separate the different material types.
Each test specimen shall consist of a single material type, which is tested separately. If fabrics and prints
cannot be separated, they may be tested together. Up to three test specimens (of equal mass) of the same
material type may be tested together, taking into consideration the limits of detection (LoD) and
quantification (LoQ).
Each material type is cut into pieces of about 0,3 cm to 0,5 cm edge length.
8 Procedure
8.1 Extraction with KOH
Weigh approximately 1 g (minimum sample mass 0,2 g) of the cut test specimen (7) (to the nearest
0,01 g) in a glass vial (6.2). Add 10 ml extraction solution (5.12). After closing, the vial is transferred to a
heating apparatus (6.3) and left for 16 h ± 15 min at (90 ± 1) °C. The temperature in the vials is checked
in a vial (6.2) with blank KOH extraction solution (5.12).
If the test specimen to be examined is too voluminous to be completely covered with KOH solution for
the period of extraction, the test specimen shall be weighed down with glass balls or a comparable inert
object to ensure complete wetting. Alternatively, a larger amount of extraction solution shall be added.
Thereby, the different specimen mass to solution ratio shall be considered in the calculation (9.2).
NOTE Deviations from the specified extraction time and temperature can lead to significant variations in the
result.
By applying KOH extraction, MoCPs and DiCPs can be released from unknown compounds, for example
dyes. If it is only required to test for free MoCPs and DiCPs the procedure described in Annex C can be
applied.
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8.2 Acetylation of extracted CPs
8.2.1 General procedure of acetylation
To get a limit of quantification (LoQ) of 0,1 mg/kg use the following procedure: After extraction, the
solution shall be cooled down to room temperature and shaken vigorously for approximately 1 min with
a vortex shaker (6.6) or for approximately 10 min with a horizontal shaker (6.7).
Transfer 4 ml of the extract into a new glass vial (6.2) and add 6 ml potassium carbonate solution (5.13),
2 ml n-hexane (5.4), 250 μl TCG solution (5.14) and 1 ml acetic anhydride (5.5).
8.2.2 Preparation for GC analysis
−1
Close the vial and shake it for (30 ± 1) min at a shaking rate of at least 200 min on a horizontal shaker
(6.7). An efficient mixing of the phases shall be ensured.
Let the two phases of the solution separate and centrifuge the vial, if required, before opening it. Open
the vial carefully (WARNING: There can be an overpressure in the vial!) and transfer an aliquot from the
upper phase into a GC vial (6.4) for analysis.
If a higher LoQ is required, it is possible to use less extract and/or more n-hexane (5.4). Perform a
validation of the method with these changed conditions.
By reducing the mass of the test specimen higher limit values can be covered.
8.2.3 Acetylation in case of low recovery rates
For test specimens with very low recovery rates of the isotope-labelled internal standards, take the whole
extract with the test specimen (8.1) and add 5 ml n-hexane (5.4), 625 μl TCG solution (5.14) and 2,5 ml
acetic anhydride (5.5) instead of the above-mentioned volumes. The n-hexane phase will contain more
matrix than from the solution without the test specimen. This can affect the instrumental analysis (8.4)
but empirically the recovery rates of the isotope-labelled internal standards improve. Proceed with 8.2.2.
8.3 Acetylation of the calibration standards
Transfer 100 μl of each CP calibration solution (5.16) into new glass vials (6.2). Add 4 ml extraction
solution (5.12), 6 ml potassium carbonate solution (5.13), 2 ml n-hexane (5.4), 250 μl TCG solution (5.14)
and 1 ml of acetic anhydride (5.5) to each vial. Proceed analogous to 8.2.2.
8.4 Gas chromatography with mass selective detection
Determine the compounds listed in Table 1 and acetylated in 8.2 and 8.3 by GC-MS (6.9) as required.
Examples of chromatographic and spectroscopic conditions are given in Annex A.
9 Expression of results
9.1 General
The quantitative determination is made using a multi-point calibration with at least three points. The
calibration curve is constructed by plotting the area against the known standard concentrations with
correction for the related isotope-labelled internal standards (Table 3). From the calibration curve,
interpolate the concentration of chlorophenol (ρ ), in μg/ml.
s
If the recovery of the isotope-labelled internal standards due to matrix effects is lower than the specified
recovery of the laboratory's quality guideline, other valid methods, such as addition procedures, may be
used to quantify the CP concentrations.
If the recovery rates of the isotope-labelled internal standards are very low, perform 8.2.3.
TCG is used to check whether the acetylation (8.3) and the injection were successful.
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9.2 Calculation of the individual chlorophenols
The contents of CPs are calculated as mass fractions w, in mg/kg, of the test specimen according to
Formula (1):
ρ ××VV
si KOH n-hexane
w = (1)
i
Am×
KOH E
where
w the mass fraction of a CP(i) found, in mg/kg;
i
ρsi the interpolated CP(i) concentration according to 9.1, in μg/ml;
V the volume of the KOH extraction solution according to 8.1, in ml;
KOH
A aliquot of the KOH extraction solution according to 8.2.1 or 8.2.3, in ml;
KOH
V the volume of the added amount of n-hexane according to 8.2.1 or 8.2.3, in ml;
n-hexane
m the mass of the test specimen, in g.
E
9.3 Sum of chlorophenols
In certain cases, the sum of different CPs is requested as a final result. Only CPs that are clearly identified
shall be included in the sum.
The results of the identified CPs (as obtained in 9.2) are added to give the result of the sum. If the result
for a single CP is lower than the limit of quantification (LoQ) of the test method (9.4), this result shall not
be included in the sum.
9.4 Precision of the test method
This method is able to determine the concentrations of the substances listed in Table 1 with a limit of
quantification (LoQ) of 0,1 mg/kg or lower.
For the reliability (precision) of the procedure, see Annex B.
10 Test report
The test report shall include at least the following information:
a) identification of the submitted sample;
b) reference to this document, i.e. EN 17134-2:2023;
c) the mass fraction for each quantified CP, in mg/kg (as calculated in 9.2), rounded to a maximum of 2
significant figures with a maximum of 2 decimal points;
d) if requested, the mass fraction of the sum of CPs in mg/kg (as calculated in 9.3), rounded to a
maximum of 2 significant figures with a maximum of 2 decimal points;
e) any deviations from the procedure;
f) any unusual features observed;
g) the date of the analysis.
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Annex A
(informat
...
SLOVENSKI STANDARD
oSIST prEN 17134-2:2022
01-september-2022
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: prEN 17134-2
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
oSIST prEN 17134-2:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 17134-2:2022
DRAFT
EUROPEAN STANDARD
prEN 17134-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2022
ICS 59.080.01 Will supersede EN 17134:2019
English Version
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
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, Turkey 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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17134-2:2022 E
worldwide for CEN national Members.
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Contents
Page
European foreword . 4
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Abbreviations . 6
5 Principle . 7
6 Apparatus . 7
6.1 Gas chromatograph (GC), with mass selective detector (MSD). . 7
6.2 Analytical balance, weighing with an accuracy of 0,1 mg. . 7
6.3 Heating block, sand bath or drying cabinet, suitable for a temperature of 90 °C ± 1 °C
in the KOH solution. 7
6.4 Gas-tight glass vials, for example headspace vials, (20 ml) . . 7
6.5 GC vials, about 2 ml. . 7
6.6 Pasteur pipettes, graduated pipettes, suitable autopipettes . 7
6.7 Vortex shaker . 7
−1
6.8 Horizontal shaker, capable of at least 200 min . 7
7 Reagents . 7
7.1 General . 7
7.2 Chlorophenol mixture Stock solution . 7
7.3 Tetrachloroguaiacol (tetrachloro-o-methoxyphenol) CAS number: 2539-17-5 . 9
7.4 Isotope labelled internal standards . 9
7.5 n-Hexane, for residue analysis. . 9
7.6 Potassium hydroxide solution (KOH), aqueous solution (1 mol/l). . 9
7.7 Tetrachloroguiacol (TCG) solution, at a concentration of 1 μg/ml in acetonitrile
(internal standard for injection control). 9
7.8 Stock solution isotope-labelled internal standards in KOH solution, each 0,1 mg/ml 9
7.9 Extraction solution (containing isotope-labelled internal standards). 9
7.10 Potassium carbonate (K CO ), aqueous solution (0,1 mol/l). . 9
2 3
7.11 Acetic anhydride (C H O ), for analysis. .10
4 6 3
7.12 Water, grade 3, according to ISO 3696. .10
7.13 Acetone .10
7.14 Acetonitrile .10
7.15 Working solution calibration level 1, for daily calibration .10
7.16 Working solution calibration level 2, for daily calibration .10
7.17 Working solution calibration level 3, for daily calibration .10
7.18 Working solution calibration level 4, for daily calibration .10
7.19 Working solution calibration level 5, for daily calibration. .10
8 Sampling .10
9 Procedure.10
9.1 General .10
9.2 Extraction with KOH .10
9.3 Extractive acetylation .11
9.4 Derivatization of the chlorophenol mixtures and the TCG standards (calibration for
daily use) .11
2
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9.5 Gas chromatography (GC). 11
10 Expression of results . 12
10.1 General . 12
10.2 Calculation of the individual chlorphenols in the test specimen . 12
10.3 Reliability of the procedure . 12
11 Test report . 13
Annex A (informative) Chromatographic test conditions . 14
A.1 Preliminary remarks . 14
A.2 Gas chromatography with mass selective detector (GC-MSD) . 14
Annex B (informative) Procedure characteristics . 16
B.1 General . 16
B.2 Ring test results . 16
B.2.1 Results of the first ring test . 16
B.2.2 Results of the second ring test from one real test specimen and two spikes of the real
test specimen, with 4 laboratories . 17
B.3 Influence of standard solutions . 25
B.4 Influence of internal standards on contents of pentachlorophenol and other
chlorophenols . 31
Annex C (informative) Verification method for free mono- and dichlorophenol . 41
C.1 General . 41
C.2 Procedure . 41
3
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European foreword
This document (prEN 17134-2:2021) 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 17134:2019.
4
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Introduction
In Europe, according to REGULATION (EU) 2019/1021[1] of the European Parliament and of the Council
of 20 June 2019 on persistent organic pollutants 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, 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).
This document specifies a method in which chlorophenols (CP) are acetylated before chromatographic
detection and the amount of detected chlorophenol acetate is quantified by a correction with an internal
standard.
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.
5
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1 Scope
This document specifies a method to determine the content of free pentachlorophenol (PCP), and
tetrachlorophenol- (TeCP), trichlorophenol- (TriCP), dichlorophenol- (DiCP), monochlorophenol-
(MoCP) isomers. The procedure also releases chlorophenols from salts and esters. The method is
applicable to natural and synthetic textiles, including coated fabrics and clothing components (e.g.
buttons, zippers, etc.).
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.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological 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 Abbreviations
The following abbreviations are used in this document for chlorophenols:
CP chlorophenols
MoCP monochlorophenol
DiCP dichlorophenol
TriCP trichlorophenol
TeCP tetrachlorophenol
PCP pentachlorophenol
2-MoCP-d4 2-chlorophenol-d
4
2,3-DiCP-d3 2,3-dichlorophenol-d
3
13
TeCP-13C6 2,3,4,6-tetrachlorophenol- C
6
13
PCP-C13 pentachlorophenol- C
6
TCG tetrachloroguaiacol (= tetrachloro-o-methoxyphenol)
The following abbreviations are used in this document for the designation of textile fibres:
6
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CO cotton
PES polyester
CV viscose
EL elastane
LI linen
PA polyamide
5 Principle
The sample is extracted with a potassium hydroxide solution (KOH solution) for 16 h at 90 ° C.
During subsequent extractive derivatization with n-hexane and acetic acid anhydride, CPs are acetylated
and the chlorinated acetates are analyzed using gas chromatography with a mass-selective detector
13 2
(MSD). The quantitative determination is made by correction with C and H labelled internal standards.
13 13
For pentachlorophenol, the C derivative of PCP is used, for tetrachlorophenols the C derivative of
2,3,4,6-tetrachlorophenol, for tri- and dichlorophenols 2,3-dichlorophenol-d and for
3
monochlorophenols 2-chlorophenol-d . TCG serves as an internal standard for injection control.
4
6 Apparatus
6.1 Gas chromatograph (GC), with mass selective detector (MSD).
6.2 Analytical balance, weighing with an accuracy of 0,1 mg.
6.3 Heating block, sand bath or drying cabinet, suitable for a temperature of 90 °C ± 1 °C in the KOH
solution.
6.4 Gas-tight glass vials, for example headspace vials, (20 ml) .
6.5 GC vials, about 2 ml.
6.6 Pasteur pipettes, graduated pipettes, suitable autopipettes
6.7 Vortex shaker
−1
6.8 Horizontal shaker, capable of at least 200 min
7 Reagents
7.1 General
Unless otherwise stated, chemicals of analytical grade shall be used.
7.2 Chlorophenol mixture Stock solution
A mixture of chlorophenols which, at a concentration of 50 μg/ml in a suitable solvent (for example
7
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Acetonitrile) contains the following isomers:
2-chlorophenol CAS number: 95-57-8
3-chlorophenol CAS number: 108-43-0
4-chlorophenol CAS number: 106-48-9
2,3-dichlorophenol CAS number: 576-24-9
2,4-dichlorophenol CAS number: 120-83-2
2,5-dichlorophenol CAS number: 583-78-8
2,6-dichlorophenol CAS number: 87-65-0
3,4-dichlorophenol CAS number: 95-77-2
3,5-dichlorophenol CAS number: 591-35-5
2,3,4-trichlorophenol CAS number: 15950-66-0
2,3,5-trichlorophenol CAS number: 933-78-8
2,3,6-trichlorophenol CAS number: 933-75-5
2,4,5-trichlorophenol CAS number: 95-95-4
2,4,6-trichlorophenol CAS number: 88-06-2
3,4,5-trichlorophenol CAS number 609-19-8
2,3,4,5-tetrachlorophenol CAS number 4901-51-3
2,3,4,6-tetrachlorophenol CAS number: 58-90-2
2,3,5,6-tetrachlorphenol CAS number: 935-95-5
pentachlorophenol CAS number: 87-86-5
NOTE This mixture of chlorophenols is available from laboratory chemical suppliers.
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7.3 Tetrachloroguaiacol (tetrachloro-o-methoxyphenol) CAS number: 2539-17-5
7.4 Isotope labelled internal standards
2-chlorophenol-d CAS number: 93951-73-6
4
2,3-dichlorophenol-d CAS number: 93951-74-7
3
13
2,3,4,6-tetrachlorophenol- C CAS number:1246820-81-4
6
13
pentachlorophenol- C CAS number: 85380-74-1
6
Instead of the isotope-labelled derivatives of tetra-, di- and monochlorophenol mentioned, other isotope-
labelled analogues of the same chlorination levels, e.g. 4-chlorophenol-d , may also be used as internal
4
standards.
7.5 n-Hexane, for residue analysis.
7.6 Potassium hydroxide solution (KOH), aqueous solution (1 mol/l).
Weigh 56,1 g KOH into a 1 l volumetric flask and dissolve with 100 ml water (7.12) (caution: heat
generation!). After cooling, fill up to 1 l with water (7.12).
7.7 Tetrachloroguiacol (TCG) solution, at a concentration of 1 μg/ml in acetonitrile
(internal standard for injection control)
Dissolve 10 mg TCG in 100 ml acetonitrile (7.14). Take 1,0 ml from this stock solution and dilute to 100 ml
with acetonitrile (7.14).
7.8 Stock solution isotope-labelled internal standards in KOH solution, each 0,1 mg/ml
Dissolve 10 mg of each isotope-labelled internal standard (7.4) in 100 ml KOH solution (7.6).
7.9 Extraction solution (containing isotope-labelled internal standards)
1,0 ml stock solution isotope-labelled internal standards (7.8) is filled up with KOH solution (7.6) in a 1 l
volumetric flask, the concentration of each of the isotope-labelled internal standards (7.4) is 0,1 µg/ml .
The concentration of isotope-labelled internal standards shall be adapted to the respective calibration
range of the chlorophenols (see solutions 7.15 to 7.19). If a more sensitive measuring instrument is used
and the calibration is lowered, then the concentration of isotope-labelled internal standards in the KOH
solution should also be reduced.
7.10 Potassium carbonate (K CO ), aqueous solution (0,1 mol/l).
2 3
Weigh 13,82 g K CO into a 1 l volumetric flask, dissolve with water (7.12) and fill up to 1 l.
2 3
9
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7.11 Acetic anhydride (C4H6O3), for analysis.
7.12 Water, grade 3, according to ISO 3696.
7.13 Acetone
7.14 Acetonitrile
7.15 Working solution calibration level 1, for daily calibration
30 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 10 ml volumetric
flask; the concentration of chlorophenols is 0,15 μg/ml.
7.16 Working solution calibration level 2, for daily calibration
400 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 10 ml volumetric
flask; the concentration of chlorophenols is 2,0 μg/ml.
7.17 Working solution calibration level 3, for daily calibration
800 μl stock solution chlorophenol mixture (7.2) are filled up with acetonitrile (7.14) in a 10 ml
volumetric flask; the concentration of chlorophenols is 4 μg/ml.
7.18 Working solution calibration level 4, for daily calibration
600 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 2 ml volumetric
flask; the concentration of chlorophenols is 15 μg/ml.
7.19 Working solution calibration level 5, for daily calibration.
1 000 μl stock solution chlorophenol mixture (7.2) is filled up with acetonitrile (7.14) in a 2 ml volumetric
flask; the concentration of chlorophenols is 25 μg/ml.
The concentrations of the calibration solutions (7.15 to 7.19) are examples and should be adjusted
according to the specified limit values and the linearity of the device.
8 Sampling
From the material to be examined, a representative test specimen shall be taken and cut into pieces of
about 0,5 cm × 0,5 cm.
9 Procedure
9.1 General
If it is only required to test for free mono- and dichlorophenols, the procedure described in Annex C shall
be applied.
9.2 Extraction with KOH
Place approximately 1 g (minimum sample weight 0,2 g) of the cut test specimen (to the nearest 0,01 g)
in the reaction vessel (6.4). Add 10 ml extraction solution (7.9). After closing, the vessel is transferred to
a heating apparatus (6.3) and left for 16 h ± 15 min at (90 ± 1) °C. The temperature in the reaction vessel
is checked with extraction solution. If the test specimen to be examined is too voluminous to be
10
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completely covered with KOH solution for the period of extraction, the test specimen shall be weighed
down with glass balls or a comparable inert object to ensure complete wetting, or a suitable larger
amount of extraction solution shall be added (take into account the different specimen weight to liquor
ratio in the calculation).
NOTE Deviations from the specified extraction time and temperature can lead to significant deviations in the
result.
9.3 Extractive acetylation
After extraction, the test specimen shall be cooled down to room temperature and shaken vigorously
(1 min vortex shaker (6.7) or 10 min horizontal shaker (6.8)). Transfer 4 ml of the KOH extraction
solution into a new reaction vessel (6.4) and add 6 ml potassium carbonate solution (7.10), 2 ml n-hexane
(7.5), 250 μl TCG solution (7.7) and 1 ml acetic acid anhydride (7.11).
−1
After closing the vessel, shake it for 30 min at a shaking rate of at least 200 min on a horizontal shaker
(6.8). An efficient mixing of the phases shall be ensured.
After shaking, centrifugation may improve phase separation. The vessel is then opened carefully (caution:
overpressure!). Transfer an aliquot (for example 1 ml) from the upper phase to a GC vial (6.5) for analysis.
Take 4 ml of extraction solution and add 2 ml of n-hexane to reliably detect a value of 0,05 mg/kg
chlorophenols. For device configurations that allow lower limits of detection, the volume of extraction
solution used for acetylation may be reduced or the amount of n-hexane added may be increased. The
same volumes shall be used for calibration and test specimens. A validation with the changed conditions
shall be executed.
By reducing the weight of the test specimen higher limit values can be covered.
9.4 Derivatization of the chlorophenol mixtures and the TCG standards (calibration for
daily use)
100 μl of each chlorophenol working solution (7.15 to 7.19), 4 ml extraction solution (7.9), 6 ml
potassium carbonate solution (7.10), 2 ml n-hexane (7.5), 250 μl TCG solution (7.7) and 1 ml of acetic
acid anhydride (7.11) shall be added into a separate reaction vessel (6.4). After closing the vessel, shake
−1
it for 30 min at a shaking rate of at least 200 min on a horizontal shaker (6.8). The vessel is centrifuged
after shaking and then carefully opened (caution: overpressure!). Transfer an aliquot (for example 1 ml)
from the upper phase from each reaction vessel to a GC vial (6.5) for analysis. Depending on the device, a
basic calibration is carried out for detection and determination and for the linear working area.
9.5 Gas chromatography (GC)
Various types of gas chromatographic equipment may be used. The chromatography conditions specified
in Annex A are an example of parameters that have been successfully applied in the analysis.
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10 Expression of results
10.1 General
The quantitative determination is made using multi-point calibration with at least three points.
The calibration curve is constructed by plotting the area units against the known standard concentrations
13
and correcting for the isotope-labelled internal standards. Pentachlorophenol- C is used as an internal
6
13
standard for pentachlorophenol, 2,3,4,6-tetrachlorophenol- C for tetrachlorophenols, 2,3-
6
dichlorophenol-d for tri- und dichlorophenols and 2-chlorophenol-d for monochlorophenols. From the
3 4
calibration curve, the concentration of chlorophenol, in μg/ml (ρ ), is interpolated.
s
If the recovery of the isotope-labelled internal standards due to matrix effects is lower than the specified
recovery of the laboratory's quality guideline, other valid methods, such as addition procedures, may be
used to determine the quantitative result. In exceptional cases, at the discretion of the person responsible
for the laboratory, a value may also be calculated against TCG. However, if possible, the calculation against
isotope-labelled chlorophenols should always be preferred. For materials with very low recoveries of the
isotope-labelled internal standards, 5 ml n-hexane (7.5), 625 μl TCG solution (7.7) and 2,5 ml acetic
anhydride (7.11) may be added to the total extraction solution containing the specimen in the same vessel
and then proceed as described above. For the following instrumental analysis according to 9.5 and
Annex A, the n-hexane phase obtained here is significantly more matrix-loaded than the phase according
to 9.3, but empirically the recoveries of the isotope-labelled internal standards improve.
Values calculated via TCG shall be reported separately in the test report.
10.2 Calculation of the individual chlorphenols in the test specimen
The content of chlorophenol is calculated as a mass portion w, in mg/kg, of the test specimen according
to equation (1):
𝜌𝜌 ×𝑉𝑉 ×𝑉𝑉
s KOH n-hexane
𝑤𝑤= (1)
𝐴𝐴 ×𝑚𝑚
KOH E
where
w the concentration of chlorophenol found, in mg/kg;
ρ the interpolated chlorophenol concentration, in μg/ml measured solution;
s
V the volume of the KOH extraction solution according to 9.2, in ml (here 10 ml);
KOH
A aliquot of the KOH extraction solution according to 9.2, in ml (here 4 ml);
KOH
V the volume of the added amount of n-hexane, in ml (here 2 ml);
n-hexane
m the mass of the test specimen, in g.
E
10.3 Reliability of the procedure
For the reliability (precision) of the procedure, see Annex B.
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11 Test report
The test report shall include at least the following information:
a) reference to this document, i.e. EN 17134-2:202X;
b) kind, origin and designation of the sample;
c) the result for each CP, in mg/kg, rounded to a maximum of 2 significant figures with a maximum of 2
decimal points;
d) any deviations from the given procedure;
e) an indication whether values were calculated via TCG and, if so, which;
f) date of analysis.
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Annex A
(informative)
Chromatographic test conditions
A.1 Preliminary remarks
Due to possible differences in the instrumental equipment (6.1) of the laboratories, no general
requirements for gas chromatographic analyses can be made. The following chromatographic conditions
are an example of the parameters that have been successfully applied in this method.
A.2 Gas chromatography with mass
...
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