Plastics — Determination of bound acrylonitrile content in the continuous phase of acrylonitrile-butadiene-styrene (ABS) by Dumas combustion method

This document specifies a method for the determination of bound acrylonitrile content in the continuous phase of acrylonitrile-butadiene-styrene (ABS) copolymer using Dumas combustion method. This document is applicable to ABS resin with a mass fraction of bound acrylonitrile content in continuous phase between 5 % and 50 %.

Plastiques — Détermination de la teneur en acrylonitrile lié dans la phase continue d'acrylonitrile-butadiène-styrène (ABS) par la méthode de combustion Dumas

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Status
Published
Publication Date
16-Nov-2022
Current Stage
6060 - International Standard published
Due Date
07-Jan-2023
Completion Date
17-Nov-2022
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ISO 24048:2022 - Plastics — Determination of bound acrylonitrile content in the continuous phase of acrylonitrile-butadiene-styrene (ABS) by Dumas combustion method Released:17. 11. 2022
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INTERNATIONAL ISO
STANDARD 24048
First edition
2022-11
Plastics — Determination of bound
acrylonitrile content in the continuous
phase of acrylonitrile-butadiene-
styrene (ABS) by Dumas combustion
method
Plastiques — Détermination de la teneur en acrylonitrile lié dans
la phase continue d'acrylonitrile-butadiène-styrène (ABS) par la
méthode de combustion Dumas
Reference number
ISO 24048:2022(E)
© ISO 2022
---------------------- Page: 1 ----------------------
ISO 24048:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
© ISO 2022 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 24048:2022(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 Sampling and preparation of the specimen ............................................................................................................................ 3

7.1 Preparation of cold methanol and settlement of centrifuge .......................................................................... 3

7.2 Sample dispersion ............................................................................................................................................................................... 3

7.3 Centrifuge separation....................................................................................................................................................................... 3

7.4 Precipitation of continuous phase ........................................................................................................................................ 3

7.5 Centrifuge and work-up .................................................................................................................................................................. 3

8 Procedure ....................................................................................................................................................................................................................4

8.1 Calibration .................................................................................................................................................................................................. 4

8.1.1 General ........................................................................................................................................................................................ 4

8.1.2 Instrument set up .............................................................................................................................................................. 4

8.1.3 Setting up calibration curve..................................................................................................................................... 4

8.2 Measurement ........................................................................................................................................................................................... 5

8.3 Calculation .................................................................................................................................................................................................. 5

9 Precision ....................................................................................................................................................................................................................... 6

9.1 General ........................................................................................................................................................................................................... 6

9.2 Repeatability, r........................................................................................................................................................................................ 6

9.3 Reproducibility, R ................................................................................................................................................................................. 6

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

Annex A (informative) Summary of precision data ............................................................................................................................. 7

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

iii
© ISO 2022 – All rights reserved
---------------------- Page: 3 ----------------------
ISO 24048:2022(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 Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9,

Thermoplastic materials.

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.
© ISO 2022 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 24048:2022(E)
Plastics — Determination of bound acrylonitrile content
in the continuous phase of acrylonitrile-butadiene-styrene
(ABS) by Dumas combustion method
1 Scope

This document specifies a method for the determination of bound acrylonitrile content in the continuous

phase of acrylonitrile-butadiene-styrene (ABS) copolymer using Dumas combustion method. This

document is applicable to ABS resin with a mass fraction of bound acrylonitrile content in continuous

phase between 5 % and 50 %.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes the 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 472, Plastics — Vocabulary
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472 apply.

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 https:// www .electropedia .org/
4 Principle

The ABS samples are dispersed in acetone. The dissolved continuous phase is separated from the

dispersed elastomeric phase using a high-speed centrifuge. The separated supernatant is precipitated

by methanol and then washed by n-hexane. The nitrogen content of the precipitate is determined

through Dumas combustion method and the content of acrylonitrile in the continuous phase is

calculated.
5 Reagents
5.1 Reference materials:
Combustible organic compounds with known nitrogen content, purity ≥ 99,99 %.

EXAMPLE Acetanilide, ethylenediaminetetraacetic acid (EDTA), aspartic acid, atropine, etc.

5.2 Oxygen gas, purity ≥ 99,99 % or in accordance with the analyser manufacturer’s instruction.

5.3 Carrier gas, helium, argon or carbon dioxide, purity ≥ 99,995 % or in accordance with the

analyser manufacturer’s instruction.
5.4 Acetone, volume fraction ≥ 99,8 %.
© ISO 2022 – All rights reserved
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ISO 24048:2022(E)
5.5 Methanol, volume fraction ≥ 99,8 %.
5.6 N-hexane, volume fraction ≥ 95 %.
6 Apparatus
6.1 Automatic analyser
The automatic analyser consists of the following components:

a) a combustion unit, capable of complete combustion of the sample in an atmosphere of high-purity

oxygen;

b) an oxygen feeder, capable of feeding enough high purity oxygen for complete combustion;

c) a reduction unit, capable of fully converting liberated nitrogenous compounds to nitrogen gas;

d) an absorber (or another type of separator) of by-products, capable of separating nitrogen from

other combustion products;

NOTE 1 When helium or argon is used as the carrier gas, this unit normally separates nitrogen from

carbon dioxide and water; when carbon dioxide is used as the carrier gas, this unit normally separates

nitrogen from water.
e) a thermal conductivity detector (TCD), capable of detecting nitrogen formed;

f) a microprocessor, capable of calibrating the apparatus with a reference material and of converting

the detector response into the mass of nitrogen in the sam
...

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