Rubber and rubber products — Determination of the composition of vulcanizates and uncured compounds by thermogravimetry — Part 1: Butadiene, ethylene-propylene copolymer and terpolymer, isobutene-isoprene, isoprene and styrene-butadiene rubbers

Caoutchouc et produits à base de caoutchouc — Détermination de la composition des vulcanisats et des mélanges non vulcanisés par thermogravimétrie — Partie 1: Caoutchoucs butadiène, copolymères et terpolymères éthylène-propylène, isobutène-isoprène, isoprène et butadiène-styrène

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Status
Withdrawn
Publication Date
06-Dec-2000
Withdrawal Date
06-Dec-2000
Current Stage
9599 - Withdrawal of International Standard
Start Date
18-Jul-2016
Completion Date
18-Jul-2016
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ISO 9924-1:2000 - Rubber and rubber products -- Determination of the composition of vulcanizates and uncured compounds by thermogravimetry
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INTERNATIONAL ISO
STANDARD 9924-1
Second edition
2000-12-01
Rubber and rubber products —
Determination of the composition of
vulcanizates and uncured compounds by
thermogravimetry —
Part 1:
Butadiene, ethylene-propylene copolymer
and terpolymer, isobutene-isoprene,
isoprene and styrene-butadiene rubbers
Caoutchouc et produits à base de caoutchouc — Détermination de la
composition des vulcanisats et des mélanges non vulcanisés par
thermogravimétrie —
Partie 1: Caoutchoucs butadiène, copolymères et terpolymères éthylène-
propylène, isobutène-isoprène, isoprène et butadiène-styrène
Reference number
ISO 9924-1:2000(E)
ISO 2000
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ISO 9924-1:2000(E)
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ii © ISO 2000 – All rights reserved
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ISO 9924-1:2000(E)
Contents Page

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

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

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

3 Principle..........................................................................................................................................................2

4 Reagents.........................................................................................................................................................2

5 Apparatus .......................................................................................................................................................2

6 Thermogravimetric analyser checks ...........................................................................................................3

7 Procedure .......................................................................................................................................................4

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

9 Precision.........................................................................................................................................................7

10 Test report ......................................................................................................................................................8

© ISO 2000 – All rights reserved iii
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ISO 9924-1:2000(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 3.

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 part of ISO 9924 may be the subject of patent

rights. ISO shall not be held responsible for identifying any or all such patent rights.

International Standard ISO 9924-1 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products,

Subcommittee SC 2, Testing and analyses.

This second edition cancels and replaces the first edition (ISO 9924-1:1993), which has been technically revised.

ISO 9924 consists of the following parts, under the general title Rubber and rubber products — Determination of

the composition of vulcanizates and uncured compounds by thermogravimetry:

� Part 1: Butadiene, ethylene-propylene copolymer and terpolymer, isobutene-isoprene, isoprene and styrene-

butadiene rubbers
� Part 2: Acrylonitrile-butadiene and halobutyl rubbers
iv © ISO 2000 – All rights reserved
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INTERNATIONAL STANDARD ISO 9924-1:2000(E)
Rubber and rubber products — Determination of the composition
of vulcanizates and uncured compounds by thermogravimetry —
Part 1:
Butadiene, ethylene-propylene copolymer and terpolymer,
isobutene-isoprene, isoprene and styrene-butadiene rubbers

WARNING — Persons using this part of ISO 9924 should be familiar with normal laboratory practice. This

part of ISO 9924 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

1.1 This part of ISO 9924 specifies a thermogravimetric method for the determination of the total organic content,

carbon black content and ash in vulcanizates and uncured compounds. The loss in mass at 300 °Cis an

approximate guide to the volatile-matter content of the compound.

1.2 The method is suitable for the analysis of rubber compounds and vulcanizates containing the following

rubbers occurring alone or as mixtures:
a) polyisoprene of natural or synthetic origin;
b) polybutadiene;
c) styrene-butadiene copolymers;
d) isobutylene-isoprene copolymers;
e) ethylene-propylene copolymers and related terpolymers.

NOTE The field of application of the method may be extended to the analysis of compounds containing rubbers different

from those given in this subclause, provided that the applicability of the method is tested beforehand using known compounds

or vulcanizates having a similar composition. Other compounds are covered in ISO 9924-2.

1.3 The method is not suitable for rubbers containing polymers which form a carbonaceous residue during

pyrolysis, such as many chlorine- or nitrogen-containing rubbers.

1.4 The method is also not suitable for materials containing additives which cause the formation of

carbonaceous residues during pyrolysis, such as cobalt and lead salts or phenolic resins.

1.5 The method is not suitable for compounds containing mineral fillers, such as carbonates or hydrated

aluminium oxides, which decompose in the temperature range from 25 °Cto650 °C, unless suitable corrections

based on prior knowledge of filler behaviour can be made.

1.6 The method is not suitable for the determination of the total polymer content of compounds or vulcanizates

containing non-rubber organic ingredients that cannot be completely removed by solvent extraction carried out in

accordance with ISO 1407.
© ISO 2000 – All rights reserved 1
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ISO 9924-1:2000(E)
2 Normative references

The following normative documents contain provisions which, through reference in this text, constitute provisions of

this part of ISO 9924. For dated references, subsequent amendments to, or revisions of, any of these publications

do not apply. However, parties to agreements based on this part of ISO 9924 are encouraged to investigate the

possibility of applying the most recent editions of the normative documents indicated below. For undated

references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain

registers of currently valid International Standards.
ISO 1407:1992, Rubber — Determination of solvent extract.

ISO/TR 9272:1986, Rubber and rubber products — Determination of precision for test method standards.

3Principle

3.1 A weighed test portion is heated, following a pre-set programme, from 70 °Cto300 °C in a stream of

nitrogen and is maintained at 300 °C for 10 min. The loss in mass indicates approximately the total content of non-

rubber organic matter volatile at 300 °C. In general, this value is not equivalent to the value of the solvent extract.

3.2 The oven temperature is then raised to 550 °C, still in a stream of nitrogen, and maintained at 550 °Cfor

15 min. The organic matter which was undistilled at 300 °C and the polymer distill off, and the loss in mass

between 70 °C and 550 °C represents the total organic-matter content.

NOTE The total rubber content is calculated by subtracting the value of the solvent extract, determined in accordance with

ISO 1407, from the total organic content, provided that all non-rubber ingredients can be extracted.

3.3 The oven temperature is raised from 550 °Cto650 °C in a stream of nitrogen, then the gas is changed from

nitrogen to air or oxygen, or a mixture of air or oxygen, and the temperature is maintained at 650 °C for 15 min or

until no further loss in mass is observed. The carbon black is burnt off, and the loss in mass in the oxidizing

atmosphere at 650 °C thus represents the carbon black content. A balanced flow of gas is maintained throughout

the changeover to avoid buoyancy effects.
3.4 The mass of the residue at 650 °C represents the ash.
4 Reagents
4.1 Dry nitrogen, with an oxygen content of less than 10 mg/kg (ppm).
4.2 Dry air or oxygen.
5 Apparatus
5.1 Thermogravimetric analyser.

There are many types of analyser commercially available. All should be suitable for use with this part of ISO 9924,

but their suitability should be checked using the procedure in clause 6. Calibrate and operate the thermogravimetric

analyser in accordance with the manufacturer’s instructions.
The basic components of an analyser are as follows:
5.1.1 Thermogravimetric balance.
5.1.2 Electrically heated, thermo-regulated oven.
5.1.3 Temperature programmer, for the oven.
2 © ISO 2000 – All rights reserved
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ISO 9924-1:2000(E)

5.1.4 Switching device, allowing a stream of nitrogen or a stream of air or oxygen (or a mixture of nitrogen and

air or oxygen) to flow through the oven at a predetermined and constant flow rate.

5.1.5 X/Y recorder, for recording the temperature/mass plot. Alternatively, temperature/time and mass/time plots

may be recorded simultaneously using a two-pen Y/T recorder.

5.1.6 Auxiliary equipment for producing differential curves (useful but not mandatory for this part of

ISO 9924).
5.2 Analytical balance, capable of weighing to 0,1 mg.
6 Thermogravimetric analyser checks
6.1 Measurement of purge time t

6.1.1 Place a test portion of carbon black or black-filled rubber, as specified in the manufacturer’s instructions, in

the thermobalance sample pan and heat to 650 °C in a stream of nitrogen, at the maximum rate allowed by the

temperature programmer.

6.1.2 Maintaining the temperature at 650 °C, introduce air or oxygen and allow the test portion to combust fully.

6.1.3 When there is no further mass change, switch off the oven heater and allow the oven to cool to room

temperature, maintaining the air or oxygen flow. At this point, the oven will have been thoroughly purged with air or

oxygen. The following operations are designed to determine the time t required to completely restore the inert

atmosphere of nitrogen.

6.1.4 With the oven at 25 °C� 5 °C, introduce a fresh test portion of carbon black, of mass as specified in the

manufacturer’s instructions, into the balance pan and close the apparatus.

6.1.5 Record the time t , switch over to nitrogen gas flow, and set the oven temperature to increase to 650 °Cat

as fast a rate as practicable and then remain constant.
6.1.6 Observe the thermogravimetric analyser mass trace and,
...

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