SIST EN ISO 22744-1:2020
(Main)Textiles and textile products - Determination of organotin compounds - Part 1: Derivatisation method using gas chromatography (ISO 22744-1:2020)
Textiles and textile products - Determination of organotin compounds - Part 1: Derivatisation method using gas chromatography (ISO 22744-1:2020)
This document specifies a test method for determining the presence of organotin compounds. This test
method is applicable to all types of materials of textile products.
NOTE CEN/TR 16741 defines which materials are concerned by this determination.
Textilien und textile Erzeugnisse - Bestimmung von zinnorganischen Verbindungen - Teil 1: Derivatisierung für das gaschromatische Verfahren (ISO 22744-1:2020)
Dieses Dokument legt ein Prüfverfahren zur qualitativen und quantitativen Bestimmung von zinnorganischen Verbindungen fest. Dieses Prüfverfahren ist für alle Arten von Materialien textiler Erzeugnisse anwendbar.
ANMERKUNG CEN/TR 16741 legt fest, auf welche Materialien dieses Verfahren anwendbar ist.
Textiles et produits textiles - Détermination des composés organostanniques - Partie 1: Méthode de dérivation utilisant la chromatographie en phase (ISO 22744-1:2020)
Le présent document spécifie une méthode d'essai pour la qualification et la quantification des composés organostanniques. Cette méthode s'applique à tous les types de matériaux de produits textiles.
NOTE Le CEN/TR 16741 définit à quels matériaux s'applique cette détermination.
Tekstilije in tekstilni izdelki - Določevanje organokositrnih spojin - 1. del: Metoda derivatizacije s plinsko kromatografijo (ISO 22744-1:2020)
General Information
Buy Standard
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 22744-1:2020
01-september-2020
Tekstilije in tekstilni izdelki - Določevanje organokositrnih spojin - 1. del: Metoda
derivatizacije s plinsko kromatografijo (ISO 22744-1:2020)
Textiles and textile products - Determination of organotin compounds - Part 1:
Derivatisation method using gas chromatography (ISO 22744-1:2020)
Textilien und textile Erzeugnisse - Bestimmung von zinnorganischen Verbindungen - Teil
1: Derivatisierung für das gaschromatische Verfahren (ISO 22744-1:2020)
Textiles et produits textiles - Détermination des composés organostanniques - Partie 1:
Méthode de dérivation utilisant la chromatographie en phase (ISO 22744-1:2020)
Ta slovenski standard je istoveten z: EN ISO 22744-1:2020
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 22744-1:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN ISO 22744-1:2020
---------------------- Page: 2 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2020
EUROPÄISCHE NORM
ICS 59.080.01
English Version
Textiles and textile products - Determination of organotin
compounds - Part 1: Derivatisation method using gas
chromatography (ISO 22744-1:2020)
Textiles et produits textiles - Détermination des Textilien und textile Erzeugnisse - Bestimmung von
composés organostanniques - Partie 1: Méthode de zinnorganischen Verbindungen - Teil 1:
dérivation utilisant la chromatographie en phase (ISO Derivatisierung für das gaschromatische Verfahren
22744-1:2020) (ISO 22744-1:2020)
This European Standard was approved by CEN on 24 April 2020.
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, Turkey 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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22744-1:2020 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1:2020 (E)
Contents Page
European foreword . 3
2
---------------------- Page: 4 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1:2020 (E)
European foreword
This document (EN ISO 22744-1:2020) has been prepared by Technical Committee ISO/TC 38
"Textiles" in collaboration with 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 December 2020, and conflicting national standards
shall be withdrawn at the latest by December 2020.
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.
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, 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 the
United Kingdom.
Endorsement notice
The text of ISO 22744-1:2020 has been approved by CEN as EN ISO 22744-1:2020 without any
modification.
3
---------------------- Page: 5 ----------------------
SIST EN ISO 22744-1:2020
---------------------- Page: 6 ----------------------
SIST EN ISO 22744-1:2020
INTERNATIONAL ISO
STANDARD 22744-1
First edition
2020-05
Textiles and textile products —
Determination of organotin
compounds —
Part 1:
Derivatisation method using gas
chromatography
Textiles et produits textiles — Détermination des composés
organostanniques —
Partie 1: Méthode de dérivation utilisant la chromatographie en
phase gazeuse
Reference number
ISO 22744-1:2020(E)
©
ISO 2020
---------------------- Page: 7 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus and materials. 3
7 Preparation of the test piece . 3
8 Procedure. 4
8.1 General . 4
8.2 Preparation of the sodium tetraethylborate solution. 4
8.3 Preparation of standard solutions . 4
8.3.1 General. 4
8.3.2 Internal standards — Stock solution (100 mg/l of organotin cation) . 5
8.3.3 Internal standards — Working solution (10 mg/l of organotin cation) . 5
8.3.4 Target compounds — Stock solution (1 000 mg/l of organotin cation) . 6
8.3.5 Target compounds — Working solution (10 mg/l of organotin cation) . 6
8.4 Preparation of the tropolone solution . 6
8.5 Preparation of the buffer solution . 6
8.6 Preparation of the calibration solutions . 6
8.7 Sample preparation . 7
8.8 Preparation of the blank solution . 7
8.9 Gas chromatography . 7
9 Expression of results . 8
10 Test report .10
Annex A (informative) Suggested gas chromatography-mass spectrometry (GC-MS)
conditions for organotin analysis .11
Annex B (informative) Reliability of the method .12
Bibliography .13
© ISO 2020 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/
iso/ foreword .html.
This document was prepared by the European Committee for Standardization (CEN) Technical
Committee CEN/TC 248, Textiles and textile products, in collaboration with ISO Technical Committee
ISO/TC 38, Textiles, in accordance with the Agreement on technical cooperation between ISO and CEN
(Vienna Agreement).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 22744-1:2020
INTERNATIONAL STANDARD ISO 22744-1:2020(E)
Textiles and textile products — Determination of organotin
compounds —
Part 1:
Derivatisation method using gas chromatography
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.
1 Scope
This document specifies a test method for the qualification and quantification of organotin compounds.
This test method is applicable to all types of materials of textile products.
NOTE CEN/TR 16741 defines which materials are applicable to this determination.
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
ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use
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 http:// www .electropedia .org/
4 Principle
The organotin substances are extracted from the material of a textile product with a methanol-ethanol
mixture using tropolone as a complexing agent.
The polar and high-boiling organotin is then converted to the corresponding volatile alkyl derivative,
by reaction with sodium tetraethylborate, NaB(Et) . Finally, it is detected and quantified by using a gas
4
chromatograph fitted with a mass selective detector (GC-MS).
Table 1 indicates the list of target compounds which can be analysed with this document.
This document is also applicable for further organotin substances provided that the method is validated
with the additional compounds.
© ISO 2020 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Table 1 — List of target compounds that can be analysed and internal standards
Type of
a
Compound CAS number
compound
Internal standard: n-Heptyltin trichloride 59344–47–7
Methyltin trichloride 993–16–8
Monosubstituted n-Butyltin trichloride 1118–46–3
n-Octyltin trichloride 3091–25–6
Phenyltin trichloride 1124–19–2
Internal standard: Di-n-heptyltin dichloride 74340–12–8
Dimethyltin dichloride 753–73–1
Di-n-propyltin dichloride 867–36–7
Disubstituted
Di-n-butyltin dichloride 683–18–1
Di-n-octyltin dichloride 3542–36–7
Diphenyltin dichloride 1135–99–5
Internal standard: Tri-n-pentyltin chloride 3342–67–4
Trimethyltin chloride 1066–45–1
Tri-n-propyltin chloride 2279–76–7
b
Trisubstituted Tri-n-butyltin chloride 1461–22–9
Tri-n-octyltin chloride 2587–76–0
Triphenyltin chloride (or fentin chloride) 639–58–7
Tricyclohexyltin chloride 3091–32–5
Internal standard: Tetra-n-propyltin 2176–98–9
Tetrasubstituted Tetra-n-ethyltin 597–64–8
Tetra-n-butyltin 1461–25–2
a
Chemical Abstract Service.
b
If bis(tri-n-butyltin)oxide (TBTO), CAS number 56–35–9, is present, it is detected as tri-
n-butyltin.
5 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1 Water, grade 3 according to ISO 3696.
5.2 Ethanol, technical grade or industrial methylated spirit (IMS), CAS number: 64-17-5.
5.3 Glacial acetic acid, CAS number: 64-19-7.
5.4 Sodium tetraethylborate, CAS number: 15523-24-7.
5.5 Tetrahydrofuran (THF), stabilized, CAS number: 109-99-9.
5.6 n-Heptyltin trichloride, CAS number: 59344-47-7 (internal standard).
5.7 Di-n-heptyltin dichloride, CAS number: 74340-12-8 (internal standard).
5.8 Tri-n-pentyltin chloride, CAS number: 3342-67-4 (internal standard).
2 © ISO 2020 – All rights reserved
---------------------- Pag
...
SLOVENSKI STANDARD
SIST EN ISO 22744-1:2020
01-september-2020
Tekstilije in tekstilni izdelki - Določevanje organokositrnih spojin - 1. del: Metoda
derivatizacije s plinsko kromatografijo (ISO 22744-1:2020)
Textiles and textile products - Determination of organotin compounds - Part 1:
Derivatisation method using gas chromatography (ISO 22744-1:2020)
Textilien und textile Erzeugnisse - Bestimmung von zinnorganischen Verbindungen - Teil
1: Derivatisierung für das gaschromatische Verfahren (ISO 22744-1:2020)
Textiles et produits textiles - Détermination des composés organostanniques - Partie 1:
Méthode de dérivation utilisant la chromatographie en phase (ISO 22744-1:2020)
Ta slovenski standard je istoveten z: EN ISO 22744-1:2020
ICS:
59.060.01 Tekstilna vlakna na splošno Textile fibres in general
SIST EN ISO 22744-1:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN ISO 22744-1:2020
---------------------- Page: 2 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2020
EUROPÄISCHE NORM
ICS 59.080.01
English Version
Textiles and textile products - Determination of organotin
compounds - Part 1: Derivatisation method using gas
chromatography (ISO 22744-1:2020)
Textiles et produits textiles - Détermination des Textilien und textile Erzeugnisse - Bestimmung von
composés organostanniques - Partie 1: Méthode de zinnorganischen Verbindungen - Teil 1:
dérivation utilisant la chromatographie en phase (ISO Derivatisierung für das gaschromatische Verfahren
22744-1:2020) (ISO 22744-1:2020)
This European Standard was approved by CEN on 24 April 2020.
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, Turkey 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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22744-1:2020 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1:2020 (E)
Contents Page
European foreword . 3
2
---------------------- Page: 4 ----------------------
SIST EN ISO 22744-1:2020
EN ISO 22744-1:2020 (E)
European foreword
This document (EN ISO 22744-1:2020) has been prepared by Technical Committee ISO/TC 38
"Textiles" in collaboration with 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 December 2020, and conflicting national standards
shall be withdrawn at the latest by December 2020.
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.
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, 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 the
United Kingdom.
Endorsement notice
The text of ISO 22744-1:2020 has been approved by CEN as EN ISO 22744-1:2020 without any
modification.
3
---------------------- Page: 5 ----------------------
SIST EN ISO 22744-1:2020
---------------------- Page: 6 ----------------------
SIST EN ISO 22744-1:2020
INTERNATIONAL ISO
STANDARD 22744-1
First edition
2020-05
Textiles and textile products —
Determination of organotin
compounds —
Part 1:
Derivatisation method using gas
chromatography
Textiles et produits textiles — Détermination des composés
organostanniques —
Partie 1: Méthode de dérivation utilisant la chromatographie en
phase gazeuse
Reference number
ISO 22744-1:2020(E)
©
ISO 2020
---------------------- Page: 7 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus and materials. 3
7 Preparation of the test piece . 3
8 Procedure. 4
8.1 General . 4
8.2 Preparation of the sodium tetraethylborate solution. 4
8.3 Preparation of standard solutions . 4
8.3.1 General. 4
8.3.2 Internal standards — Stock solution (100 mg/l of organotin cation) . 5
8.3.3 Internal standards — Working solution (10 mg/l of organotin cation) . 5
8.3.4 Target compounds — Stock solution (1 000 mg/l of organotin cation) . 6
8.3.5 Target compounds — Working solution (10 mg/l of organotin cation) . 6
8.4 Preparation of the tropolone solution . 6
8.5 Preparation of the buffer solution . 6
8.6 Preparation of the calibration solutions . 6
8.7 Sample preparation . 7
8.8 Preparation of the blank solution . 7
8.9 Gas chromatography . 7
9 Expression of results . 8
10 Test report .10
Annex A (informative) Suggested gas chromatography-mass spectrometry (GC-MS)
conditions for organotin analysis .11
Annex B (informative) Reliability of the method .12
Bibliography .13
© ISO 2020 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/
iso/ foreword .html.
This document was prepared by the European Committee for Standardization (CEN) Technical
Committee CEN/TC 248, Textiles and textile products, in collaboration with ISO Technical Committee
ISO/TC 38, Textiles, in accordance with the Agreement on technical cooperation between ISO and CEN
(Vienna Agreement).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 22744-1:2020
INTERNATIONAL STANDARD ISO 22744-1:2020(E)
Textiles and textile products — Determination of organotin
compounds —
Part 1:
Derivatisation method using gas chromatography
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.
1 Scope
This document specifies a test method for the qualification and quantification of organotin compounds.
This test method is applicable to all types of materials of textile products.
NOTE CEN/TR 16741 defines which materials are applicable to this determination.
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
ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use
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 http:// www .electropedia .org/
4 Principle
The organotin substances are extracted from the material of a textile product with a methanol-ethanol
mixture using tropolone as a complexing agent.
The polar and high-boiling organotin is then converted to the corresponding volatile alkyl derivative,
by reaction with sodium tetraethylborate, NaB(Et) . Finally, it is detected and quantified by using a gas
4
chromatograph fitted with a mass selective detector (GC-MS).
Table 1 indicates the list of target compounds which can be analysed with this document.
This document is also applicable for further organotin substances provided that the method is validated
with the additional compounds.
© ISO 2020 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 22744-1:2020
ISO 22744-1:2020(E)
Table 1 — List of target compounds that can be analysed and internal standards
Type of
a
Compound CAS number
compound
Internal standard: n-Heptyltin trichloride 59344–47–7
Methyltin trichloride 993–16–8
Monosubstituted n-Butyltin trichloride 1118–46–3
n-Octyltin trichloride 3091–25–6
Phenyltin trichloride 1124–19–2
Internal standard: Di-n-heptyltin dichloride 74340–12–8
Dimethyltin dichloride 753–73–1
Di-n-propyltin dichloride 867–36–7
Disubstituted
Di-n-butyltin dichloride 683–18–1
Di-n-octyltin dichloride 3542–36–7
Diphenyltin dichloride 1135–99–5
Internal standard: Tri-n-pentyltin chloride 3342–67–4
Trimethyltin chloride 1066–45–1
Tri-n-propyltin chloride 2279–76–7
b
Trisubstituted Tri-n-butyltin chloride 1461–22–9
Tri-n-octyltin chloride 2587–76–0
Triphenyltin chloride (or fentin chloride) 639–58–7
Tricyclohexyltin chloride 3091–32–5
Internal standard: Tetra-n-propyltin 2176–98–9
Tetrasubstituted Tetra-n-ethyltin 597–64–8
Tetra-n-butyltin 1461–25–2
a
Chemical Abstract Service.
b
If bis(tri-n-butyltin)oxide (TBTO), CAS number 56–35–9, is present, it is detected as tri-
n-butyltin.
5 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1 Water, grade 3 according to ISO 3696.
5.2 Ethanol, technical grade or industrial methylated spirit (IMS), CAS number: 64-17-5.
5.3 Glacial acetic acid, CAS number: 64-19-7.
5.4 Sodium tetraethylborate, CAS number: 15523-24-7.
5.5 Tetrahydrofuran (THF), stabilized, CAS number: 109-99-9.
5.6 n-Heptyltin trichloride, CAS number: 59344-47-7 (internal standard).
5.7 Di-n-heptyltin dichloride, CAS number: 74340-12-8 (internal standard).
5.8 Tri-n-pentyltin chloride, CAS number: 3342-67-4 (internal standard).
2 © ISO 2020 – All rights reserved
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SIST
...
SLOVENSKI STANDARD
oSIST prEN ISO 22744-1:2018
01-oktober-2018
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VHVWDYLQDKPDWHULDORYWHNVWLOQLKL]GHONRY8JRWDYOMDQMHRUJDQVNLKVHVWDYLQGHO
0HWRGD]XSRUDERSOLQVNHNURPDWRJUDILMH ,62',6
Textiles and textile product - Critical substances potentially present in components of
textile product materials - Determination of organotin compounds - Part 1: Method using
gas chromatography (ISO/DIS 22744-1:2018)
Textilien und textile Erzeugnisse - Kritische Stoffe, die potentiell in Bestandteilen von
Materialien textiler Erzeugnisse vorhanden sind - Bestimmung von zinnorganischen
Verbindungen - Teil 1: Gaschromatographisches Verfahren (ISO/DIS 22744-1:2018)
Textiles et produits textiles - Substances critiques potentiellement présentes dans les
composants de matériaux de produits textiles - Détermination des composés
organostanniques - Partie 1: Méthode utilisant la chromatographie en phase gazeuse
(ISO/DIS 22744-1:2018)
Ta slovenski standard je istoveten z: prEN ISO 22744-1
ICS:
59.060.01 Tekstilna vlakna na splošno Textile fibres in general
oSIST prEN ISO 22744-1:2018 de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 22744-1:2018
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oSIST prEN ISO 22744-1:2018
ENTWURF
EUROPÄISCHE NORM
prEN ISO 22744-1
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2018
ICS 59.080.01
Deutsche Fassung
Textilien und textile Erzeugnisse - Kritische Stoffe, die
potentiell in Bestandteilen von Materialien textiler
Erzeugnisse vorhanden sind - Bestimmung von
zinnorganischen Verbindungen - Teil 1:
Gaschromatographisches Verfahren (ISO/DIS 22744-1:2018)
Textiles and textile product - Critical substances Textiles et produits textiles - Substances critiques
potentially present in components of textile product potentiellement présentes dans les composants de
materials - Determination of organotin compounds - matériaux de produits textiles - Détermination des
Part 1: Method using gas chromatography (ISO/DIS composés organostanniques - Partie 1: Méthode
22744-1:2018) utilisant la chromatographie en phase gazeuse (ISO/DIS
22744-1:2018)
Dieser Europäische Norm-Entwurf wird den CEN-Mitgliedern zur parallelen Umfrage vorgelegt. Er wurde vom Technischen
Komitee CEN/TC 248 erstellt.
Wenn aus diesem Norm-Entwurf eine Europäische Norm wird, sind die CEN-Mitglieder gehalten, die CEN-Geschäftsordnung zu
erfüllen, in der die Bedingungen festgelegt sind, unter denen dieser Europäischen Norm ohne jede Änderung der Status einer
nationalen Norm zu geben ist.
Dieser Europäische Norm-Entwurf wurde von CEN in drei offiziellen Fassungen (Deutsch, Englisch, Französisch) erstellt. Eine
Fassung in einer anderen Sprache, die von einem CEN-Mitglied in eigener Verantwortung durch Übersetzung in seine
Landessprache gemacht und dem CEN-CENELEC-Management-Zentrum mitgeteilt worden ist, hat den gleichen Status wie die
offiziellen Fassungen.
CEN-Mitglieder sind die nationalen Normungsinstitute von Belgien, Bulgarien, Dänemark, Deutschland, der ehemaligen
jugoslawischen Republik Mazedonien, Estland, Finnland, Frankreich, Griechenland, Irland, Island, Italien, Kroatien, Lettland,
Litauen, Luxemburg, Malta, den Niederlanden, Norwegen, Österreich, Polen, Portugal, Rumänien, Schweden, der Schweiz,
Serbien, der Slowakei, Slowenien, Spanien, der Tschechischen Republik, der Türkei, Ungarn, dem Vereinigten Königreich und
Zypern.
Die Empfänger dieses Norm-Entwurfs werden gebeten, mit ihren Kommentaren jegliche relevante Patentrechte, die sie kennen,
mitzuteilen und unterstützende Dokumentationen zur Verfügung zu stellen.
Warnvermerk : Dieses Schriftstück hat noch nicht den Status einer Europäischen Norm. Es wird zur Prüfung und Stellungnahme
vorgelegt. Es kann sich noch ohne Ankündigung ändern und darf nicht als Europäischen Norm in Bezug genommen werden.
EUROPÄISCHES KOMITEE FÜR NORMUNG
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
CEN-CENELEC Management-Zentrum: Rue de la Science 23, B-1040 Brüssel
© 2018 CEN Alle Rechte der Verwertung, gleich in welcher Form und in welchem Ref. Nr. prEN ISO 22744-1:2018 D
Verfahren, sind weltweit den nationalen Mitgliedern von CEN
vorbehalten.
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oSIST prEN ISO 22744-1:2018
prEN ISO 22744-1:2018 (D)
Inhalt
Seite
Europäisches Vorwort . 3
Vorwort . 4
1 Anwendungsbereich . 5
2 Normative Verweisungen . 5
3 Kurzbeschreibung . 5
4 Reagenzien . 6
5 Geräte und Materialien . 6
6 Herstellen des Prüfstücks . 7
7 Durchführung . 7
7.1 Herstellung der Natriumtetraethylboratlösung . 7
7.2 Herstellung der Standardlösungen . 7
7.2.1 Allgemeines . 7
7.2.2 Interne Standard-Stammlösung (1 000 mg/l des zinnorganischen Kations) . 9
7.2.3 Interne Standard-Arbeitslösung (10 mg/l des zinnorganischen Kations) . 9
7.2.4 Zielverbindung-Stammlösung (1 000 mg/l des zinnorganischen Kations) . 9
7.2.5 Zielverbindung-Arbeitslösung (10 mg/l des zinnorganischen Kations) . 9
7.3 Herstellung der NaDDC-Lösung . 9
7.4 Herstellung der Pufferlösung . 9
7.5 Kalibrierung . 10
7.6 Probenherstellung . 10
7.7 Herstellung der Blindlösung . 11
7.8 Gaschromatographie . 11
7.9 Quantifizierung . 12
7.10 Nachweisgrenze und Bestimmungsgrenze . 13
8 Prüfbericht . 13
(informativ) Für die Analyse zinnorganischer Verbindungen mittels
Gaschromatographie–Massenspektrometrie (GC-MS) empfohlene Bedingungen . 14
Literaturhinweise . 15
2
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oSIST prEN ISO 22744-1:2018
prEN ISO 22744-1:2018 (D)
Europäisches Vorwort
Dieses Dokument (prEN ISO 22744-1:2018) wurde vom Technischen Komitee ISO/TC 38 „Textiles“ in
Zusammenarbeit mit dem Technischen Komitee CEN/TC 248 „Textilien und textile Erzeugnisse“ erarbeitet,
dessen Sekretariat von BSI gehalten wird.
Dieses Dokument ist derzeit zur parallelen Umfrage vorgelegt.
Dieses Dokument wurde an ISO/TS 16179 angelehnt, das vom Europäischen Komitee für Normung (CEN)
und dessen Technischem Komitee CEN/TC 309 „Schuhe“ in Zusammenarbeit mit dem Technischen Komitee
ISO/TC 216 „Footwear“ in Übereinstimmung mit der Vereinbarung zur technischen Zusammenarbeit
zwischen ISO und CEN (Wiener Vereinbarung) erarbeitet wurde. Die Anlehnung erfolgte auf der Grundlage
der Erweiterung des Anwendungsbereiches auf textile Erzeugnisse.
Anerkennungsnotiz
Der Text von ISO/DIS 22744-1:2018 wurde von CEN als prEN ISO 22744-1:2018 ohne irgendeine
Abänderung genehmigt.
3
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oSIST prEN ISO 22744-1:2018
prEN ISO 22744-1:2018 (D)
Vorwort
ISO (die Internationale Organisation für Normung) ist eine weltweite Vereinigung nationaler
Normungsorganisationen (ISO-Mitgliedsorganisationen). Die Erstellung von Internationalen Normen wird
üblicherweise von Technischen Komitees von ISO durchgeführt. Jede Mitgliedsorganisation, die Interesse an
einem Thema hat, für welches ein Technisches Komitee gegründet wurde, hat das Recht, in diesem Komitee
vertreten zu sein. Internationale staatliche und nichtstaatliche Organisationen, die in engem Kontakt mit ISO
stehen, nehmen ebenfalls an der Arbeit teil. ISO arbeitet bei allen elektrotechnischen Themen eng mit der
Internationalen Elektrotechnischen Kommission (IEC) zusammen.
Die Verfahren, die bei der Entwicklung dieses Dokuments angewendet wurden und die für die weitere Pflege
vorgesehen sind, werden in den ISO/IEC-Direktiven, Teil 1 beschrieben. Es sollten insbesondere die
unterschiedlichen Annahmekriterien für die verschiedenen ISO-Dokumentenarten beachtet werden. Dieses
Dokument wurde in Übereinstimmung mit den Gestaltungsregeln der ISO/IEC-Direktiven, Teil 2 erarbeitet
(siehe www.iso.org/directives).
Es wird auf die Möglichkeit hingewiesen, dass einige Elemente dieses Dokuments Patentrechte berühren
können. ISO ist nicht dafür verantwortlich, einige oder alle diesbezüglichen Patentrechte zu identifizieren.
Details zu allen während der Entwicklung des Dokuments identifizierten Patentrechten finden sich in der
Einleitung und/oder in der ISO-Liste der erhaltenen Patenterklärungen (siehe www.iso.org/patents).
Jeder in diesem Dokument verwendete Handelsname dient nur zur Unterrichtung der Anwender und
bedeutet keine Anerkennung.
Eine Erläuterung zum freiwilligen Charakter von Normen, der Bedeutung ISO-spezifischer Begriffe und
Ausdrücke in Bezug auf Konformitätsbewertungen sowie Informationen darüber, wie ISO die Grundsätze der
Welthandelsorganisation (WTO) hinsichtlich technischer Handelshemmnisse (TBT) berücksichtigt, enthält
der folgende Link: www.iso.org/iso/foreword.html.
Dieses Dokument wurde vom Technischen Komitee ISO/TC 261, Footwear erarbeitet.
4
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oSIST prEN ISO 22744-1:2018
prEN ISO 22744-1:2018 (D)
1 Anwendungsbereich
Dieses Dokument legt ein Prüfverfahren zur Bestimmung des Vorhandenseins von zinnorganischen
Bestandteilen fest. Dieses Prüfverfahren gilt für alle Arten von Materialien textiler Erzeugnisse.
ANMERKUNG CEN/TR 16741 legt fest, auf welche Werkstoffe diese Bestimmung anzuwenden ist.
2 Normative Verweisungen
Die folgenden Dokumente, die in diesem Dokument teilweise oder als Ganzes zitiert werden, sind für die
Anwendung dieses Dokuments erforderlich. Bei datierten Verweisungen gilt nur die in Bezug genommene
Ausgabe. Bei undatierten Verweisungen gilt die letzte Ausgabe des in Bezug genommenen Dokuments
(einschließlich aller Änderungen).
ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use
EN ISO 3696:1995, Wasser für analytische Zwecke — Spezifikation und Prüfverfahren (ISO 3696:1987)
3 Kurzbeschreibung
Die zinnorganischen Substanzen werden aus dem Material eines textilen Erzeugnisses mit einem Methanol-
Ethanol-Gemisch mittlerer Säurestärke mit Natriumdiethyldithiocarbamat (NaDDC) als Komplexbildner
extrahiert.
Die zinnorganische Verbindung, eine polare Verbindung mit hohem Siedepunkt, wird dann durch Reaktion
mit Natriumtetraethylborat, NaB(Et) , in das entsprechende flüchtige Tetraalkylderivat umgewandelt.
4
Abschließend erfolgt ein gaschromatographischer Nachweis mit einem massenselektiven Detektor (GC-MS).
In Tabelle 1 sind die Zielverbindungen angegeben, die nach diesem Dokument analysiert werden können.
Tabelle 1 — Aufzählung von Zielverbindungen, die analysiert werden können
a
Art der Verbindung Verbindung CAS
n-Butylzinntrichlorid 1118-46-3
Monosubstituiert
n-Octylzinntrichlorid 3091-25-6
Di-n-butylzinndichlorid 683-18-1
Disubstituiert
Di-n-octylzinndichlorid 3542-36-7
b
Tri-n-butylzinnchlorid 1461-22-9
Trisubstituiert Triphenylzinnchlorid (oder Fentinchlorid) 639-58-7
Tricyclohexylzinnchlorid 3091-32-5
Tetrasubstitutiert Tetra-n-butylzinn 1461-25-2
a
Chemical Abstract Service.
b
Wenn Bis(tri-n-butylzinn)oxid (TBTO), CAS-Nr. 56-35-9, vorhanden ist, wird es als Tri-n-butylzinn nachgewiesen.
5
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oSIST prEN ISO 22744-1:2018
prEN ISO 22744-1:2018 (D)
4 Reagenzien
Sofern nicht anders festgelegt, werden ausschließlich Reagenzien mit einer anerkannter analytischen
Reinheit verwendet.
4.1 Wasser, Qualität 3 nach EN ISO 3696.
4.2 Ethanol, GPR-rein oder denaturierter Industriealkohol (IMS), CAS-Nummer: 64-17-5.
4.3 Eisessig, CAS-Nummer: 64-19-7.
4.4 Natriumtetraethylborat, CAS-Nummer: 15523-24-7.
4.5 Tetrahydrofuran (THF), stabilisiert, CAS-Nummer: 109-99-9.
4.6 n-Heptylzinntrichlorid, CAS-Nummer: 59344-47-7 (interner Standard).
4.7 Di-n-heptylzinndichlorid, CAS-Nummer: 74340-12-8 (interner Standard).
4.8 Tri-n-propylzinnmonochlorid, CAS-Nummer: 2279-76-7 (interner Standard).
4.9 Tetra-n-propylzinn, CAS-Nummer: 2176-98-9 (interner Standard).
4.10 Isooctan, CAS-Nummer: 540-84-1.
4.11 Inertgas, z. B. Stickstoff, Helium oder Argon.
4.12 Natriumdiethyldithiocarbamat (NaDDC), CAS-Nummer: 148-18-5.
4.13 Methanol, analysenrein, CAS-Nummer: 67-56-.
4.14 Natriumacetat, CAS-Nummer: 127-09-3.
4.15 Zinnorganische Verbindungen, wie in Tabelle 1 aufgeführt.
5 Geräte und Materialien
Es müssen die üblichen Laborgeräte und Laborgeräte aus Glas nach ISO 4787 und die folgenden verwendet
werden.
5.1 GC-MS, Gaschromatograph, mit massenselektivem Detektor (MS).
5.2 Analysenwaage, zum Messen der Masse mit einer Fehlergrenze von 0,1 mg.
5.3 Glasgefäß, mit Schraubverschluss und einem Volumen von 50 ml.
5.4 Mikropipetten, 10 µl bis 500 µl Bereich, mit Einwegspitzen.
5.5 Pipette, Volumen 1 ml bis 10 ml.
5.6 Kalibriertes pH-Messgerät, mit einer Glas-Elektrode und einem Messbereich von 0 bis 14.
5.7 Ultraschallbad, mit einstellbarer Temperatur, geeignet für den Betrieb bei etwa 60 °C.
5
...
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