Footwear - Critical substances potentially present in footwear and footwear components - Determination of organotin compounds in footwear materials (ISO/TS 16179:2012)

This Technical Specification specifies a test method for determining the presence of organotin compounds. This test method is applicable to all types of footwear materials.

Schuhe - Möglicherweise in Schuhen und Schuhbestandteilen vorhandene kritische Substanzen - Bestimmung zinnorganischer Verbindungen in Schuhwerkstoffen (ISO/TS 16179:2012)

Die vorliegende Technische Spezifikation legt ein Prüfverfahren zur Bestimmung des Vorhandenseins von zinnorganischen Bestandteilen fest. Dieses Prüfverfahren gilt für alle Arten von Schuhwerkstoffen.
ANMERKUNG ISO/TR 16178 legt fest, welche Werkstoffe von dieser Bestimmung erfasst werden.

Chaussures - Substances critiques potentiellement présentes dans les chaussures et les composants de chaussures - Détermination des composés organostanniques dans les matériaux de chaussures (ISO/TS 16179:2012)

L'ISO/TS 16179:2011 sp�cifie une m�thode d'essai permettant de d�terminer la pr�sence de compos�s organostanniques dans les mat�riaux de chaussures. Cette m�thode s'applique � tous les types de mat�riaux de chaussures.

Obutev - Možna prisotnost kritičnih snovi v obutvi ali delih obutve - Ugotavljanje organskih sestavin v materialih obutve (ISO/TS 16179:2012)

Ta tehnična specifikacija določa preskusno metodo za ugotavljanje prisotnosti organskih sestavin. Ta preskusna metoda se uporablja za vse vrste materialov obutve.

General Information

Status
Published
Publication Date
16-Sep-2012
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
28-Aug-2012
Due Date
02-Nov-2012
Completion Date
17-Sep-2012

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Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN ISO/TS 16179:2012
01-oktober-2012
2EXWHY0RåQDSULVRWQRVWNULWLþQLKVQRYLYREXWYLDOLGHOLKREXWYH8JRWDYOMDQMH
RUJDQVNLKVHVWDYLQYPDWHULDOLKREXWYH ,6276
Footwear - Critical substances potentially present in footwear and footwear components -
Determination of organotin compounds in footwear materials (ISO/TS 16179:2012)
Schuhe - Möglicherweise in Schuhen und Schuhbestandteilen vorhandene kritische
Substanzen - Bestimmung zinnorganischer Verbindungen in Schuhwerkstoffen (ISO/TS
16179:2012)
Chaussures - Substances critiques potentiellement présentes dans les chaussures et les
composants de chaussures - Détermination des composés organostanniques dans les
matériaux de chaussures (ISO/TS 16179:2012)
Ta slovenski standard je istoveten z: CEN ISO/TS 16179:2012
ICS:
61.060 Obuvala Footwear
SIST-TS CEN ISO/TS 16179:2012 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN ISO/TS 16179:2012

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SIST-TS CEN ISO/TS 16179:2012


TECHNICAL SPECIFICATION
CEN ISO/TS 16179

SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION
August 2012
ICS 61.060
English Version
Footwear - Critical substances potentially present in footwear
and footwear components - Determination of organotin
compounds in footwear materials (ISO/TS 16179:2012)
Chaussures - Substances critiques potentiellement Schuhe - Möglicherweise in Schuhen und
présentes dans les chaussures et les composants de Schuhbestandteilen vorhandene kritische Substanzen -
chaussures - Détermination des composés Bestimmung zinnorganischer Verbindungen in
organostanniques dans les matériaux de chaussures Schuhwerkstoffen (ISO/TS 16179:2012)
(ISO/TS 16179:2012)
This Technical Specification (CEN/TS) was approved by CEN on 6 August 2012 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TS 16179:2012: E
worldwide for CEN national Members.

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SIST-TS CEN ISO/TS 16179:2012
CEN ISO/TS 16179:2012 (E)
Contents Page
Foreword .3

2

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SIST-TS CEN ISO/TS 16179:2012
CEN ISO/TS 16179:2012 (E)
Foreword
This document (CEN ISO/TS 16179:2012) has been prepared by Technical Committee CEN/TC 309
“Footwear", the secretariat of which is held by AENOR, in collaboration with Technical Committee ISO/TC 216
"Footwear".
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to announce this Technical Specification: 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

3

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SIST-TS CEN ISO/TS 16179:2012

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SIST-TS CEN ISO/TS 16179:2012
TECHNICAL ISO/TS
SPECIFICATION 16179
First edition
2012-08-15
Footwear — Critical substances potentially
present in footwear and footwear
components — Determination of organotin
compounds in footwear materials
Chaussures — Substances critiques potentiellement présentes dans
les chaussures et les composants de chaussures — Détermination des
composés organostanniques dans les matériaux de chaussures
Reference number
ISO/TS 16179:2012(E)
©
ISO 2012

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SIST-TS CEN ISO/TS 16179:2012
ISO/TS 16179:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s
member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved

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SIST-TS CEN ISO/TS 16179:2012
ISO/TS 16179:2012(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus and materials . 2
6 Preparation of the test piece . 3
7 Procedure . 3
7.1 Preparation of the sodium tetraethylborate solution . 3
7.2 Preparation of standard solutions . 4
7.3 Preparation of the tropolone solution. 5
7.4 Preparation of the buffer solution . 5
7.5 Calibration . 5
7.6 Sample preparation . 6
7.7 Preparation of the blank solution . 6
7.8 Gas chromatography . 6
7.9 Quantification . 7
7.10 Detection limit and quantification limit. 8
8 Test report . 8
Annex A (informative) Suggested gas chromatography-mass spectrometry (GC-MS) conditions for
organotin analysis .10
Annex B (informative) Reliability of the method . 11
Bibliography .12
© ISO 2012 – All rights reserved iii

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SIST-TS CEN ISO/TS 16179:2012
ISO/TS 16179:2012(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
In other circumstances, particularly when there is an urgent market requirement for such documents, a technical
committee may decide to publish other types of document:
— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in
an ISO working group and is accepted for publication if it is approved by more than 50 % of the members
of the parent committee casting a vote;
— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical
committee and is accepted for publication if it is approved by 2/3 of the members of the committee
casting a vote.
An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a further
three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed,
it is reviewed again after a further three years, at which time it must either be transformed into an International
Standard or be withdrawn.
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.
ISO/TS 16179 was prepared by the European Committee for Standardization (CEN) Technical Committee
CEN/TC 309, Footwear, in collaboration with ISO Technical Committee ISO/TC 216, Footwear, in accordance
with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
iv © ISO 2012 – All rights reserved

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SIST-TS CEN ISO/TS 16179:2012
TECHNICAL SPECIFICATION ISO/TS 16179:2012(E)
Footwear — Critical substances potentially present in footwear
and footwear components — Determination of organotin
compounds in footwear materials
1 Scope
This Technical Specification specifies a test method for determining the presence of organotin compounds.
This test method is applicable to all types of footwear materials.
NOTE ISO/TR 16178 defines which materials are concerned by this determination.
2 Normative references
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Principle
The organotin substances are extracted from the footwear material with a methanol-ethanol mixture, in a
medium-strength acidic condition, using tropolone as a complexant agent.
The polar and high-boiling organotin is then converted to the corresponding volatile tetra-alkyl derivative, by
reaction with sodium tetraethylborate, NaB(Et) . Finally, it is detected by a gas chromatograph fitted with a
4
mass selective detector (GC-MS).
Table 1 indicates the list of target compounds which can be analysed with this Technical Specification.
Table 1 — List of target compounds which can be analysed with this Technical Specification
a
Type of compound Compound CAS
n-butyltin trichloride 1118-46-3
Monosubstituted
n-octyltin trichloride 3091-25-6
Di-n-butyltin dichloride 683-18-1
Disubstituted
Di-n-octyltin dichloride 3542-36-7
Tri-n-butyltin chloride 1461-22-9
Trisubstituted Triphenyltin chloride (or fentin chloride) 639-58-7
Tricyclohexyltin chloride 3091-32-5
Tetrasubstituted Tetra-n-butyltin 1461-25-2
a
  Chemical Abstract Service.
4 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
4.1 Water, grade 3 according to ISO 3696.
4.2 Ethanol, GPR grade or industrial methylated spirit (IMS), CAS number: 64-17-5.
4.3 Glacial acetic acid, CAS number: 64-19-7.
© ISO 2012 – All rights reserved 1

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SIST-TS CEN ISO/TS 16179:2012
ISO/TS 16179:2012(E)
4.4 Sodium tetraethylborate, CAS number: 15523-24-7.
4.5 Tetrahydrofuran (THF), stabilized, CAS number: 109-99-9.
4.6 n-heptyltin trichloride, CAS number: 59344-47-7 (internal standard).
4.7 Di-n-heptyltin dichloride, CAS number: 74340-12-8 (internal standard).
4.8 Tri-n-propyltin monochloride, CAS number: 2279-76-7 (internal standard).
4.9 Tetra-n-propyltin, CAS number: 2176-98-9 (internal standard).
4.10 Isooctane, CAS number: 540-84-1.
4.11 Inert gas, e.g. nitrogen, helium or argon.
4.12 Tropolone (2-hydroxy-2,4,6-cycloheptatrien-1-one), of laboratory grade, CAS number: 533-75-5.
4.13 Methanol, of analytical grade, CAS number: 67-56-1.
4.14 Sodium acetate, CAS number: 127-09-3.
4.15 Organotin compounds listed in Table 1.
5 Apparatus and materials
5.1 GC-MS gas chromatograph fitted with a mass selective detector (MS).
5.2 Analytical balance, capable of measuring mass to an accuracy of 0,1 mg.
5.3 Glove bag, box or isolation chamber with built-in gloves that enables work to be carried out in
a totally isolated and controlled environment and has side and front openings and means of sealing the
openings, such as tape.
5.4 Sample tubes of polypropylene, with screw tops and a volume of 50 ml.
5.5 Micropipettes, 10 µl to 500 µl range, with disposable tips.
5.6 Pipette, 1 ml to 10 ml capacity.
5.7 Calibrated pH-meter with a glass combination electrode and range of 0 to 14.
5.8 Volumetric flasks of 10 ml, 25 ml and 100 ml.
5.9 Ultrasonic bath with adjustable temperature.
5.10 Disposable glass Pasteur pipettes.
5.11 Glass beaker.
5.12 Centrifuge.
2 © ISO 2012 – All rights reserved

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SIST-TS CEN ISO/TS 16179:2012
ISO/TS 16179:2012(E)
−1
5.13 Mech
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