Rubber compounding ingredients — Organic vulcanizing ...National foreword This British Standard is the UK implementation of ISO 14932:2012. The UK participation in its preparation

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Rubber compounding ingredients — Organic vulcanizing agents — Determination of organic peroxide content

BS ISO 14932:2012

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National foreword

This British Standard is the UK implementation of ISO 14932:2012.

The UK participation in its preparation was entrusted to Technical CommitteePRI/23, Test methods for rubber and non-black compounding ingredients.

A list of organizations represented on this committee can be obtained onrequest to its secretary.

This publication does not purport to include all the necessary provisions of acontract. Users are responsible for its correct application.

© The British Standards Institution 2012

Published by BSI Standards Limited 2012

ISBN 978 0 580 69201 7

ICS 83.040.20

Compliance with a British Standard cannot confer immunity fromlegal obligations.

This British Standard was published under the authority of the StandardsPolicy and Strategy Committee on 29 February 2012.

Amendments issued since publication

Amd. No. Date Text affected

BRITISH STANDARDBS ISO 14932:2012



Rubber compounding ingredients — Organic vulcanizing agents — Determination of organic peroxide contentIngrédients de mélange du caoutchouc — Agents vulcanisants organiques — Détermination de la teneur en peroxyde organique

© ISO 2012

Reference numberISO 14932:2012(E)

First edition2012-01-15

ISO14932

INTERNATIONAL STANDARD

BS ISO 14932:2012



ISO 14932:2012(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2012All 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.

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Published in Switzerland

ii © ISO 2012 – All rights reserved

BS ISO 14932:2012



ISO 14932:2012(E)

© ISO 2012 – All rights reserved iii

Contents Page

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

1 Scope ...................................................................................................................................................................... 11.1 Titration method A for group a) peroxyketals .............................................................................................. 11.2 Titration method B for group b) diacyl peroxides ...................................................................................... 11.3 Titration method C for group c) diaralkyl and alkyl-aralkyl peroxides ................................................. 11.4 Capillary gas-chromatography for dialkyl peroxides ................................................................................ 1

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

3 Terms and definitions ......................................................................................................................................... 2

4 Titration method A ............................................................................................................................................... 24.1 Purpose .................................................................................................................................................................. 24.2 Principle ................................................................................................................................................................. 24.3 General procedure .............................................................................................................................................. 34.4 Expression of results ......................................................................................................................................... 3

5 Titration method B .............................................................................................................................................. 45.1 Purpose .................................................................................................................................................................. 45.2 Principle ................................................................................................................................................................. 45.3 General procedure .............................................................................................................................................. 55.4 Expression of results ......................................................................................................................................... 5

6 Titration method C .............................................................................................................................................. 66.1 Purpose .................................................................................................................................................................. 66.2 Principle ................................................................................................................................................................. 66.3 Reagents ................................................................................................................................................................ 66.4 Apparatus .............................................................................................................................................................. 76.5 Sample pre-treatment ......................................................................................................................................... 76.6 Procedure .............................................................................................................................................................. 76.7 Expression of results ......................................................................................................................................... 8

7 Determination of the assay of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane ....................................... 97.1 Purpose .................................................................................................................................................................. 97.2 Principle ................................................................................................................................................................. 97.3 Reagents ................................................................................................................................................................ 97.4 Apparatus .............................................................................................................................................................. 97.5 Conditions ............................................................................................................................................................. 97.6 Procedure ............................................................................................................................................................107.7 Expression of results ....................................................................................................................................... 11

8 Precision .............................................................................................................................................................. 11

9 Test report ........................................................................................................................................................... 11

Annex A (informative) Method to determine the content of peroxyketal ........................................................... 12

Annex B (normative) Method to determine the content of tert-butyl hydroperoxide ..................................... 16

Annex C (informative) Method to determine the content of diacyl peroxides .................................................. 20

Annex D (normative) Sample preparation for the determination of peroxide in peroxide masterbatches ...23

Annex E (normative) Sample preparation for the determination of alkyl-aralkyl peroxide on polymers . 26

Annex F (informative) Precision ...................................................................................................................................28

Bibliography .....................................................................................................................................................................33



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.

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 14932 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.

ISO 14932:2012(E)

iv © ISO 2012 – All rights reserved

BS ISO 14932:2012



INTERNATIONAL STANDARD ISO 14932:2012(E)

Rubber compounding ingredients — Organic vulcanizing agents — Determination of organic peroxide content

WARNING — Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.

1 Scope

This International Standard specifies four methods for the determination of the content of the following groups of organic peroxides used as rubber vulcanizing agents. There are three titration methods and one using capillary gas-chromatography.

1.1 Titration method A for group a) peroxyketals

— DTBPC: 1,1-Di(tert-butylperoxy)cyclohexane;

— DBPMC: 1,1-Di(tert-butylperoxy)-2-methylcyclohexane;

— DBPTC: 1,1-Di(tert-butylperoxy)-3,3,5-trimethylcylcohexane;

— DBPB: 2,2-Di(tert-butylperoxy)butane;

— BPV: Butyl -4,4-di(tert-butylperoxy)valerate.

1.2 Titration method B for group b) diacyl peroxides

— Dibenzoyl peroxide;

— Di(2,4-dichlorobenzoyl) peroxide;

— Di(4-methylbenzoyl) peroxide.

1.3 Titration method C for group c) diaralkyl and alkyl-aralkyl peroxides

— Di(tert-butylperoxyisopropyl)benzene;

— Dicumyl peroxide;

— tert-Butyl cumyl peroxide.

1.4 Capillary gas-chromatography for dialkyl peroxides

— 2,5-Dimethyl-2,5-di(tert-butylperoxy)hexane.

2 Normative references

The following referenced documents are indispensable for the application 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 385, Laboratory glassware — Burettes

© ISO 2012 – All rights reserved 1

BS ISO 14932:2012


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Rubber compounding ingredients — Organic vulcanizing ...National foreword This British Standard is the UK implementation of ISO 14932:2012. The UK participation in its preparation