SIST EN 17137:2019
(Main)Textiles - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes
Textiles - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes
This standard specifies a method of analysis for determining the content of chlorobenzenes and chlorotoluenes in textile products and components such as upper fabric, interlining, lining, zippers, buttons, labels, threads and applications. The method applies to a mass fraction of 0.1 mg/kg to 10 mg/kg per single isomer. Both higher and lower concentrations can be determined if the weight of the sample
is selected accordingly or if appropriate dilutions are made in the course of analysis.
Textilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzol und Chlortoluol
Dieses Dokument legt ein Analysenverfahren zur Bestimmung des Gehaltes an Chlorbenzolen und Chlortoluolen in textilen Erzeugnissen fest, hergestellt aus Komponenten wie z. B. Oberstoff, Einlagen, Futter, Reißverschlüssen aus Kunststoff, Knöpfen aus Kunststoff, Etiketten, Garnen und Applikationen.
Das Verfahren gilt für einen Massenanteil von 0,1 mg/kg bis 10 mg/kg je Einzelisomer. Höhere und niedrigere Konzentrationen können bestimmt werden, wenn die Einwaage der Probe entsprechend gewählt wird bzw. im Analysengang entsprechende Verdünnungen vorgenommen werden.
Textiles - Détermination de la teneur de composés à base de chlorobenzènes et chlorotoluènes
Le présent document spécifie une méthode d’analyse pour déterminer la teneur en chlorobenzènes et chlorotoluènes des produits textiles constitués de composants tels qu’une matière extérieure, une entredoublure, une doublure, des fermetures à glissière en plastique, des boutons en plastique, des étiquettes, des fils et des appliqués.
La méthode s’applique à une fraction massique de 0,1 mg/kg à 10 mg/kg par isomère unique. Des concentrations plus élevées et plus faibles peuvent être déterminées si la masse de l’échantillon est sélectionnée en conséquence ou si des dilutions appropriées sont réalisées au cours de l’analyse.
Tekstilije - Določevanje spojin na osnovi klorobenzenov in klorotoluenov
Ta standard določa metodo za analizo, s katero se določi vsebnost klorobenzenov in klorotoluenov v tekstilnih izdelkih ter sestavnih delih, kot so zgornja tkanina, vmesna podloga, podloga, gumbi, oznake, niti in njihove kombinacije. Metoda se uporablja za masni delež od 0,1 mg/kg do 10 mg/kg na posamezni izomer. Določiti je mogoče višje in nižje koncentracije, če je teža vzorca ustrezno izbrana ali če so med analizo pripravljene ustrezne raztopine.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.ROXHQRYTextilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzol und ChlortoluolTextiles - Détermination de la teneur de composés à base de chlorobenzènes et chlorotoluènesTextiles - Determination of the content of compounds based on chlorobenzenes and chlorotoluenes59.080.01Tekstilije na splošnoTextiles in generalICS:Ta slovenski standard je istoveten z:EN 17137:2018SIST EN 17137:2019en,fr,de01-januar-2019SIST EN 17137:2019SLOVENSKI
STANDARD
SIST EN 17137:2019
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17137
November
t r s z ICS
w {ä r z rä r s English Version
Textiles æ Determination of the content of compounds based on chlorobenzenes and chlorotoluenes Textiles æ Détermination de la teneur de composés à base de chlorobenzènes et chlorotoluènes
Textilien æ Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzol und Chlortoluol This European Standard was approved by CEN on
u September
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels
9
t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s y s u yã t r s z ESIST EN 17137:2019
EN 17137:2018 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions . 4 4 Principle . 4 5 Apparatus . 4 6 Reagents . 5 7 Procedure. 6 7.1 Sampling and test specimen preparation. 6 7.2 Extraction . 6 7.3 Filtration . 6 7.4 Gas chromatographic determination . 6 7.5 Calibration . 6 7.6 Calculation and expression of the results . 7 8 Reliability of the method . 7 9 Test report . 7 Annex A (informative)
Chromatographic analyses . 8 A.1 Capillary gas chromatography/mass selective detector (GC-MS) . 8 Annex B (informative)
Reliability of the method . 11 B.1 General . 11 B.2 Accuracy . 11 B.3 Detection Limit (LOD) and Quantification Limit (LOQ) . 12 B.4 Repeatability . 13 B.5 Reproducibility . 14 B.6 Robustness. 15 B.7 Selectivity . 16 B.8 Extraction Efficiency . 17 Bibliography . 18
SIST EN 17137:2019
EN 17137:2018 (E) 3 European foreword This document (EN 17137:2018) 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 2019 and conflicting national standards shall be withdrawn at the latest by May 2019. 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 is based on DIN 54 232, which was created by the Working Committee NA 062-05-12 AA “Textiles chemical test methods and fibre separation” of the Standard Committee Testing (NMP) in the DIN Deutsches Institut for Standardization. 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, Former Yugoslav Republic of 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. SIST EN 17137:2019
EN 17137:2018 (E) 4 1 Scope This document specifies a method of analysis for determining the content of chlorobenzenes and chlorotoluenes in textile products made of components such as outer fabric, interlining, lining, plastic slide fasteners, plastic buttons, labels, threads and appliques. The method applies to a mass fraction of 0,1 mg/kg to 10 mg/kg per single isomer. Both higher and lower concentrations can be determined if the mass of the sample is selected accordingly or if appropriate dilutions are made during the analysis. 2 Normative references There are no normative references in this document. 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses: — IEC Electropedia: available at http://www.electropedia.org/ — ISO Online browsing platform: available at http://www.iso.org/obp 3.1 component individual part (one material) of the textile product sample 3.2 composite test specimen test specimen composed from various sub-test specimens of components 4 Principle The cut test specimen is extracted via ultrasonication in a closed vessel using dichloromethane. Interfering particles and fibres are removed by filtering through membrane filters. Without additional purification, the extract is analysed to determine the content of chlorobenzenes and chlorotoluenes by GC-MS with selected ion mode, using an internal standard for quantification. 5 Apparatus 5.1 Standard laboratory equipment. 5.2 Glass vials with tight closure. NOTE Vial volumes of 40 ml to 100 ml have been found suitable. 5.3 Ultrasonic bath for extraction. 5.4 Analytical balance, resolution of at least 0,000 1 g. 5.5 Syringes with Luer Lock, 2 ml, with disposable syringe filters, made of polytetrafluoroethylene (PTFE) membrane. NOTE Pore size of 0,45 µm has been found suitable. 5.6 Gas chromatograph with mass selective detector (MSD). SIST EN 17137:2019
EN 17137:2018 (E) 5 6 Reagents 6.1 Dichloromethane for residue analysis (analytical grade). 6.2 Reference substances Reference substances are listed in Table 1. Table 1 — Reference substances Substance CAS-Number a 2-Chlorotoluene 95–49–8 3-Chlorotoluene 108–41–8 4-Chlorotoluene 106–43–4 2,3-Dichlorotoluene 32768–54–0 2,4-Dichlorotoluene 95–73–8 2,5-Dichlorotoluene 19398–61–9 2,6-Dichlorotoluene 118–69–4 3,4-Dichlorotoluene 95–75–0 2,3,6-Trichlorotoluene 2077–46–5 2,4,5-Trichlorotoluene 6639–30–1 Pentachlorotoluene 877–11–2 1,2-Dichlorobenzene 95–50–1 1,3-Dichlorobenzene 541–73–1 1,4-Dichlorobenzene 106–46–7 1,2,3-Trichlorobenzene 87–61–6 1,2,4-Trichlorobenzene 120–82–1 1,3,5-Trichlorobenzene 108–70–3 1,2,3,4-Tetrachlorobenzene 634–66–2 1,2,3,5-Tetrachlorobenzene 634–90–2 1,2,4,5-Tetrachlorobenzene 95–94–3 Pentachlorobenzene 608–93–5 Hexachlorobenzene 118–74–1 2,4,5,6-Tetrachloro-m-Xylene (internal standard) 877–09–8
a Chemical Abstracts Service Number SIST EN 17137:2019
EN 17137:2018 (E) 6 7 Procedure 7.1 Sampling and test specimen preparation The test specimen is usually a composite test specimen of sub-test specimens of different components. Attention has to be paid to take equivalent masses of the different selected components. For multicoloured and differently coloured products all available colours shall be selected and be tested. Up to four colours may be tested together. In order to gather four colours, the following rules shall be applied. The rules have been listed in order of preference: — select the four colours from the same part of the textile article; — if the four colours do not come from the same part of the textile article, select these four colours from textile parts made of the same type of textile fibre. Each colour shall have approximately the same mass in order to obtain the total mass of 2 g. If the rules cannot be applied (e.g. due to a complex printed pattern, plastic buttons), the sampling description of the selected test specimens shall be reported. The test specimens are cut into pieces (approx. 5 mm wide) and stored in sealed glass vials until further processing. 7.2 Extraction (2,0 ± 0,1) g of the cut test specimen are weighed in a vial, and overlaid with 20 ml dichloromethane. After adding 200 µl internal standard solution (e.g. at concentration of 10 µg/ml), the test specimen is extracted for (30 ± 1) min in an ultrasonic bath (starting at laboratory ambient temperature). 7.3 Filtration 1 ml of the extract is taken with a disposable syringe and cleaned of interfering particles and fibres with the help of membrane filters. After filtration, the extract is transferred into a vial. 7.4 Gas chromatographic determination The substances of the extract are separated on a capillary column, and analysed using a mass-selective detector in selected ion mode (SIM). Examples of instrumental parameters are shown in Annex A. 7.5 Calibration Individual stock solutions are prepared for calibration of the reference substances (e.g. 10 mg to 10 ml
= 1 mg/ml). Then a mixed standard is prepared (e.g. 1 ml of each stock solution to 100
= 10 µg/ml). This mixed calibration standard is used to prepare calibration solutions of various concentrations (e.g. 10, 50, 100, 200, 400, 600, 800, 1 000 ng/ml). Finally 1 ml of each individual calibration solution is mixed with 10 µI of the internal standard solution (e.g. at concentration of 10µg/ml) and analysed. SIST EN 17137:2019
EN 17137:2018 (E) 7 7.6 Calculation and expression of the results The concentrations of chlorobenzenes or chlorotoluenes arise as a mass fraction in µg/ml of the following formula: ββ=sampleISTDsampleISTDF×Fm (1) where Fsample is the measured value of the analyte (area value); FISTD is t
...
SLOVENSKI STANDARD
oSIST prEN 17137:2017
01-julij-2017
7HNVWLOLMH'RORþHYDQMHVSRMLQQDRVQRYLNORUREHQ]HQRYLQNORURWROXHQRY
Textiles - Determination of the content of compounds based on chlorobenzenes and
chlorotoluenes
Textilien - Bestimmung des Gehaltes von Verbindungen auf der Basis von Chlorbenzol
und Chlortoluol
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
oSIST prEN 17137:2017 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 17137:2017
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oSIST prEN 17137:2017
DRAFT
EUROPEAN STANDARD
prEN 17137
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2017
ICS 59.080.01
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, Former Yugoslav Republic of 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 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: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17137:2017 E
worldwide for CEN national Members.
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Apparatus . 4
6 Reagents . 5
7 Procedure. 5
7.1 Sampling and test specimen preparation. 5
7.2 Extraction . 6
7.3 Filtration . 6
7.4 Gas chromatographic determination . 6
7.5 Calibration . 6
7.6 Calculation and expression of the results . 6
8 Reliability of the method . 7
9 Test report . 7
Annex A (informative) Chromatographic analyses . 8
A.1 Capillary gas chromatography/mass selective detector (GC-MS) . 8
Annex B (informative) Reliability of the method. 11
B.1 General . 11
B.2 Accuracy . 11
B.3 Detection Limit (LOD) and Quantification Limit (LOQ) . 12
B.4 Repeatability . 14
B.5 Reproducibility . 15
B.6 Robustness. 16
B.7 Selectivity . 17
B.8 Extraction Efficiency . 18
Bibliography . 19
2
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
European foreword
This document (prEN 17137:2017) 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 Enquiry.
This document is based on DIN 54 232, which was created by the Working Committee NA 062-05-12 AA
“Textiles chemical test methods and fibre separation” of the Standard Committee Testing (NMP) in the
DIN Deutsches Institut for Standardization.
3
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
1 Scope
This European Standard specifies a method of analysis for determining the content of chlorobenzenes
and chlorotoluenes in textile products made of components such as outer fabric, interlining, lining,
plastic slide fasteners, plastic buttons, labels, threads and appliques.
The method applies to a mass fraction of 0,1 mg/kg to 10 mg/kg per single isomer. Both higher and
lower concentrations can be determined if the mass of the sample is selected accordingly or if
appropriate dilutions are made during the analysis.
2 Normative references
Not applicable.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
component
individual part (one material) of the textile product sample
3.2
composite test specimen
test specimen composed from various sub-test specimens of components
4 Principle
The cut test specimen is extracted via ultrasonication in a closed vessel using dichloromethane.
Interfering particles and fibres are removed by filtering through membrane filters. Without additional
purification, the extract is analysed to determine the content of chlorobenzenes and chlorotoluenes by
GC-MS with selected ion mode, using an internal standard for quantification.
5 Apparatus
5.1 Standard laboratory equipment
5.2 Glass vials with tight closure
NOTE Vial volumes of 40 ml to 100 ml have been found suitable.
5.3 Ultrasonic bath for extraction
5.4 Analytical balance, resolution of at least 0,000 1 g
5.5 Syringes with Luer Lock, 2 ml, with disposable syringe filters, made of polytetrafluoroethylene
(PTFE) membrane
NOTE Pore size of 0,45 µm has been found suitable.
5.6 Gas chromatograph with mass selective detector (MSD)
4
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
6 Reagents
6.1 Dichloromethane for residue analysis (analytical grade)
6.2 Reference substances
Reference substances are listed in Table 1.
Table 1 — Reference substances
a
Substance CAS-Number
2-Chlorotoluene 95–49–8
3-Chlorotoluene 108–41–8
4-Chlorotoluene 106–43–4
2,3-Dichlorotoluene 32768–54–0
2,4-Dichlorotoluene 95–73–8
2,5-Dichlorotoluene 19398–61–9
2,6-Dichlorotoluene 118–69–4
3,4-Dichlorotoluene 95–75–0
2,3,6-Trichlorotoluene 2077–46–5
2,4,5-Trichlorotoluene 6639–30–1
Pentachlorotoluene 877–11–2
1,2-Dichlorobenzene 95–50–1
1,3-Dichlorobenzene 541–73–1
1,4-Dichlorobenzene 106–46–7
1,2,3-Trichlorobenzene 87–61–6
1,2,4-Trichlorobenzene 120–82–1
1,3,5-Trichlorobenzene 108–70–3
1,2,3,4-Tetrachlorobenzene 634–66–2
1,2,3,5-Tetrachlorobenzene 634–90–2
1,2,4,5-Tetrachlorobenzene 95–94–3
Pentachlorobenzene 608–93–5
Hexachlorobenzene 118–74–1
2,4,5,6-Tetrachloro-m-Xylene (internal standard) 877–09–8
a
Chemical Abstracts Service Number
7 Procedure
7.1 Sampling and test specimen preparation
The test specimen is usually a composite test specimen of sub-test specimens of different components.
Attention has to be paid to take equivalent masses of the different selected components. For
multicoloured and differently coloured products all available colours shall be selected and be tested.
Up to four colours may be tested together.
In order to gather four colours, the following rules shall be applied. The rules have been listed in order
of preference:
5
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
— Select the four colours from the same part of the textile article;
— If the four colours do not come from the same part of the textile article, select these four colours from
textile parts from textile parts made of the same type of textile fibre;
Each colour shall have approximately the same mass in order to obtain the total mass of 2 g.
If the rules cannot be applied (e.g. due to a complex printed pattern, plastic buttons), the sampling
description of the selected test specimens shall be reported.
The test specimens are cut into pieces (approx. 5 mm wide) and stored in sealed glass vials until further
processing.
7.2 Extraction
(2,0 ± 0,1) g of the cut test specimen are weighed in a vial, and overlaid with 20 ml dichloromethane.
After adding 200 µl internal standard solution, the test specimen is extracted for (30 ± 1) min in an
ultrasonic bath (starting at laboratory ambient temperature).
7.3 Filtration
1 ml of the extract is taken with a disposable syringe and cleaned of interfering particles and fibres with
the help of membrane filters. After filtration, the extract is transferred into a vial.
7.4 Gas chromatographic determination
The substances of the extract are separated on a capillary column, and analysed using a mass-selective
detector in selected ion mode (SIM).
Examples of instrumental parameters are shown in Annex A.
7.5 Calibration
Individual stock solutions are prepared for calibration of the reference substances (e.g. 10 mg to 10 ml
of dichloromethane, mass concentration β = 1 mg/ml). Then a mixed standard is prepared (e.g. 1 ml of
each stock solution to 100 ml of dichloromethane, mass concentration β = 10 µg/ml). This mixed
calibration standard is used to prepare calibration solutions of various concentrations (e.g. 10, 50, 100,
200, 400, 600, 800, 1 000 ng/ml). Finally 1 ml of each individual calibration solution is mixed with 10 µI
of the internal standard solution (e.g. at concentration of 10µg/ml) and analysed.
7.6 Calculation and expression of the results
The concentrations of chlorobenzenes or chlorotoluenes arise as a mass fraction in µg/ml of the
following equation:
F β
sample sample
=m× (1)
F β
ISTD ISTD
where
F is the measured value of the analyte (area value);
sample
F is the measured value of the internal standard (area value);
ISTD
β is the mass concentration of the analyte in the extract (µg/ml);
sample
β is the mass concentration of the internal standard in the extract (µg/ml);
ISTD
m is the slope of the calibration;
6
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oSIST prEN 17137:2017
prEN 17137:2017 (E)
The concentrations of the analytes are calculated as mass fraction w in mg/kg using the following
equation:
β ×V
( )
sample
(2)
w=
E
where
w is the mass fraction (mg/kg);
V is the extraction volume (ml);
E is the initial mass (g).
8 Reliability of the method
For the reliability of the method, see Annex B.
9 Test report
The test
...
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