Plastics -- Epoxy resins -- Determination of degree of crosslinking of crosslinked epoxy resins by differential scanning calorimetry (DSC)

This document specifies a method whereby the heat of reaction generated during epoxy resin crosslinking is measured by differential scanning calorimetry (DSC). The degree of crosslinking is determined based on this result. This method is applicable to epoxy resin systems with a moderate or slow crosslinking-reaction speed. It might not be applicable to systems with a fast crosslinking-reaction speed at ambient temperature.

Plastiques -- Résines époxydes -- Détermination du degré de réticulation des résines époxydes réticulées par analyse calorimétrique différentielle (DSC)

General Information

Status
Published
Publication Date
18-Jul-2018
Current Stage
6060 - International Standard published
Start Date
07-Jun-2018
Completion Date
19-Jul-2018
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ISO 14322:2018 - Plastics -- Epoxy resins -- Determination of degree of crosslinking of crosslinked epoxy resins by differential scanning calorimetry (DSC)
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INTERNATIONAL ISO
STANDARD 14322
Second edition
2018-07
Plastics — Epoxy resins —
Determination of degree of
crosslinking of crosslinked epoxy
resins by differential scanning
calorimetry (DSC)
Plastiques — Résines époxydes — Détermination du degré
de réticulation des résines époxydes réticulées par analyse
calorimétrique différentielle (DSC)
Reference number
ISO 14322:2018(E)
ISO 2018
---------------------- Page: 1 ----------------------
ISO 14322:2018(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.
ISO copyright office
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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 2018 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 14322:2018(E)
Contents Page

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

Introduction ..................................................................................................................................................................................................................................v

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

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

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

4 Principle ........................................................................................................................................................................................................................ 2

5 Materials ....................................................................................................................................................................................................................... 3

6 Apparatus ..................................................................................................................................................................................................................... 3

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

7.1 Calibration .................................................................................................................................................................................................. 3

7.2 Preliminary test ...................................................................................................................................................................................... 4

7.2.1 General...................................................................................................................................................................................... 4

7.2.2 Procedure for preliminary test ............................................................................................................................ 4

7.3 DSC measurement on the crosslinked resin under investigation ............................................................... 4

8 Expression of results ........................................................................................................................................................................................ 5

9 Precision ....................................................................................................................................................................................................................... 5

9.1 General ........................................................................................................................................................................................................... 5

9.2 Materials and crosslinking conditions ................................................................................................................................ 5

9.3 Precision of the method .................................................................................................................................................................. 5

10 Test report ................................................................................................................................................................................................................... 6

Annex A (informative) Example of a procedure used for the preliminary test, with typical

operating conditions ........................................................................................................................................................................................ 7

Bibliography ................................................................................................................................................................................................................................ 8

© ISO 2018 – All rights reserved iii
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ISO 14322:2018(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 61, Plastics, Subcommittee SC 12,

Thermosetting materials.

This second edition cancels and replaces the first edition (ISO 14322:2012), of which it constitutes a

minor revision.
The changes compared to the previous edition are as follows:
— the title has been updated (DSC has been added at the end);
— Clause 2 has been updated;
— the subclauses under 7.2 have been renumbered;
— editorial changes have been applied.

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 2018 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 14322:2018(E)
Introduction

It is possible to determine the degree of crosslinking of a crosslinked epoxy resin by observing changes

in its mechanical, electrical or thermal properties.

However, such an approach is inadequate in cases in which the test sample is to be evaluated as is or

is to be examined under various crosslinking conditions. This document provides a method whereby

the degree of crosslinking is determined without the need for complicated procedures for preparing,

conditioning or configuring the test sample. The degree of crosslinking is determined by comparing the

heat of the crosslinking reaction for the test sample with that of a reference sample, using a differential

scanning calorimeter.

The advantages of this method are that sample preparation is simple and measurements can be made

with very small amounts of sample. For these reasons, this document is useful for investigations of,

and in establishing conditions for, crosslinking reactions. It can also be used for production and quality

control.

Finally, since epoxy resin systems are highly diverse, the applicability of this document to each resin

system needs be established. A technique to test the applicability to an epoxy resin system is included

in this document.
© ISO 2018 – All rights reserved v
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INTERNATIONAL STANDARD ISO 14322:2018(E)
Plastics — Epoxy resins — Determination of degree of
crosslinking of crosslinked epoxy resins by differential
scanning calorimetry (DSC)

SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory

practice, if applicable. This document does not purport to address all of the safety concerns, if

any, associated with its use. It is the responsibility of the user to establish appropriate safety

and health practices and to determine the applicability of any other restrictions.

1 Scope

This document specifies a method whereby the heat of reaction generated during epoxy resin

crosslinking is measured by differential scanning calorimetry (DSC). The degree of crosslinking is

determined based on this result.

This method is applicable to epoxy resin systems with a moderate or slow crosslinking-reac

...

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