Textiles -- Determination of certain flame retardants

ISO/TR 17881-3:2018 describes a method for determining short-chain chlorinated paraffins (C10-C13) (SCCPs) in textiles using carbon skeleton reaction gas chromatography with a flame ionization detector (GC-FID). ISO/TR 17881-3:2018 is applicable to all kinds of textile products.

Textiles -- Détermination de certains retardateurs de flamme

General Information

Status
Published
Publication Date
15-Mar-2018
Current Stage
6060 - International Standard published
Start Date
22-Feb-2018
Completion Date
16-Mar-2018
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ISO/TR 17881-3:2018 - Textiles -- Determination of certain flame retardants
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TECHNICAL ISO/TR
REPORT 17881-3
First edition
2018-03
Textiles — Determination of certain
flame retardants —
Part 3:
Chlorinated paraffin flame retardants
Textiles — Détermination de certains retardateurs de flamme —
Partie 3: Retardateurs de flamme à base de paraffines chlorées
Reference number
ISO/TR 17881-3:2018(E)
ISO 2018
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ISO/TR 17881-3:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018

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.
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Email: copyright@iso.org
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Published in Switzerland
ii © ISO 2018 – All rights reserved
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ISO/TR 17881-3:2018(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Procedure..................................................................................................................................................................................................................... 3

7.1 Preparation of standard solutions ......................................................................................................................................... 3

7.1.1 Stock standard solutions ........................................................................................................................................... 3

7.1.2 Working solutions ........................................................................................................................................................... 3

7.2 Specimen extraction ........................................................................................................................................................................... 3

7.2.1 Ultrasonic wave extraction ...................................................................................................................................... 3

7.2.2 Purification ........................................................................................................................................................................... 3

7.3 Pretesting by GC-ECD ........................................................................................................................................................................ 4

7.4 Determination by GC-FID ............................................................................................................................................................... 4

8 Calculation .................................................................................................................................................................................................................. 4

8.1 Pretesting result obtained by GC-ECD ................................................................................................................................ 4

8.2 Quantity of SCCPs obtained by GC-FID ............................................................................................................................... 4

9 Detection limit ........................................................................................................................................................................................................ 5

10 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Test parameters for GC-ECD ............................................................................................................................. 7

Annex B (informative) Test parameters for GC-FID ...........................................................................................................................11

© ISO 2018 – All rights reserved iii
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ISO/TR 17881-3:2018(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 on 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 the following

URL: www .iso .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 38, Textiles.
A list of all parts in the ISO 17881 series can be found on the ISO website.
iv © ISO 2018 – All rights reserved
---------------------- Page: 4 ----------------------
TECHNICAL REPORT ISO/TR 17881-3:2018(E)
Textiles — Determination of certain flame retardants —
Part 3:
Chlorinated paraffin flame retardants

WARNING — The use of this document can involve hazardous substances and/or procedures.

It refers only to technical suitability and does not purport to address all of the health and

safety risks 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 it is assumed that the execution of its provisions is entrusted

to appropriately qualified and experienced people.
1 Scope

This document describes a method for determining short-chain chlorinated paraffins (C -C ) (SCCPs)

10 13

in textiles using carbon skeleton reaction gas chromatography with a flame ionization detector (GC-FID).

It is applicable to all kinds of textile products.
2 Normative references
There are no normative references in this document.
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:

— IEC Electropedia: available at https:// www .electropedia .org/
— ISO Online browsing platform: available at https:// www .iso .org/ obp
4 Principle

SCCPs are extracted from textile specimens by an ultrasonic generator with n-hexane/acetone. SCCPs

are pretested by gas chromatography with an electron capture detector (GC-ECD) and then quantified

by GC-FID using an external standard method. SCCPs are dechlorinated by reacting with hydrogen

to generate straight-chain alkane (C -C ) under the action of a PdCl catalyst. GC-FID is used to

10 13 2

determine the quantity of straight-chain alkane following an external standard method, and then the

quantity of SCCPs is calculated.
5 Reagents

Unless otherwise specified, only reagents of recognized analytical grade are used.

5.1 Short-chain chlorinated paraffins (SCCPs) (C -C , 51,5 % Cl), 100 µg/ml in cyclohexane.

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5.2 Short chain chlorinated paraffins (SCCPs) (C -C , 55,5 % Cl), 100 µg/ml in cyclohexane.

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5.3 Short-chain chlorinated paraffins (SCCPs) (C -C , 63 % Cl), 100 µg/ml in cyclohexane.

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© ISO 2018 – All rights reserved 1
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ISO/TR 17881-3:2018(E)
5.4 Straight-chain alkane (C -C ), purity > 99,5 %.
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5.5 n-hexane/acetone, 1:1 (volume fraction).
5.6 Diethyl ether.
5.7 Acetic acid solution, 5 % (volume fraction).
5.8 Ammonia, 25 % (mass fraction).
5.9 Mixture of n-hexane/diethyl ether, 90/10 (volume fraction).
5.10 Cyclopentane.
5.11 Cyclohexane.
5.12 Calcium carbonate (CaCO ).
5.13 Palladium chloride (PdCl ) catalyst.

After dissolving 0,08 g of PdCl in 10 ml of 5 % acetic acid (5.7), the solution is transferred to the watch

glass filled with 19 g of glass beads (6.11). The watch glass is placed into a boiling water bath, and

the solution is constantly stir
...

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