SIST EN ISO 11358:1999

Plastics - Thermogravimetry (TG) of polymers - General principles (ISO 11358:1997)

Kunststoffe - Thermogravimetrie (TG) von Polymeren - Allgemeine Grundlagen (ISO 11358:1997)

1.1 Diese Internationale Norm legt allgemeine Bedingungen für die thermogravimetrische Analyse von Polymeren fest. 1.2 Diese Internationale Norm ist anwendbar auf flüssige und feste Stoffe. Die festen Stoffe können als Pellets, Granulat oder Pulver vorliegen. Mit dem Verfahren können auch auf eine geeignete Probengröße reduzierte Fertigteile untersucht werden.

Plastiques - Thermogravimétrie (TG) des polymeres - Principes généraux (ISO 11358:1997)

1.1 La présente Norme internationale prescrit les conditions générales d'analyse des polymères au moyen des techniques de thermogravimétrie. 1.2 Elles est applicable aux corps liquides et aux solides, ces derniers se présentant sous forme de granulés, de grains ou de poudre. Cette méthode d'analyse est également applicable aux objets façonnés sur lesquels on prélève une éprouvette de dimensions appropriées. 1.3 La thermogravimétrie peut être utilisée pour déterminer la température initiale et la vitesse de décomposition des polymères et pour mesurer simultanément les quantités de substances volatiles, d'additifs et/ou de charges qu'ils contiennent. 1.4 Les mesurages thermogravimétriques peuvent être réalisés selon un mode dynamique (variation de masse en fonction de la température ou du temps, dans des conditions prédéfinies) ou un mode isotherme (variation de masse en fonction du temps, à température constante).

Polimerni materiali – Termogravimetrija polimerov – Splošna načela (ISO 11358:1997)

General Information

• Status: Withdrawn
• Publication Date: 30-Apr-1999
• Withdrawal Date: 13-Aug-2014
• ICS: 83.080.01 - Plastics in general
• Technical Committee: IPMA - Polimer materials and products
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 13-Aug-2014
• Due Date: 05-Sep-2014
• Completion Date: 14-Aug-2014
• Ref Project: EN ISO 11358:1997 - Plastics - Thermogravimetry (TG) of polymers - General principles (ISO 11358:1997)

Relations

• Replaced By: SIST EN ISO 11358-1:2014 - Plastics - Thermogravimetry (TG) of polymers - Part 1: General principles (ISO 11358-1:2014)
• Effective Date: 01-Oct-2014

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 11358:1999
01-maj-1999
3ROLPHUQLPDWHULDOL±7HUPRJUDYLPHWULMDSROLPHURY±6SORãQDQDþHOD,62

Plastics - Thermogravimetry (TG) of polymers - General principles (ISO 11358:1997)
Kunststoffe - Thermogravimetrie (TG) von Polymeren - Allgemeine Grundlagen (ISO
11358:1997)
Plastiques - Thermogravimétrie (TG) des polymeres - Principes généraux (ISO
11358:1997)
Ta slovenski standard je istoveten z: EN ISO 11358:1997
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 11358:1999 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 11358:1999

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SIST EN ISO 11358:1999

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SIST EN ISO 11358:1999

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SIST EN ISO 11358:1999
INTERNATIONAL
IS0
STANDARD
11358
First edition
1997-04- 15
Plastics - Thermogravimetry (TG) of
polymers - General principles
Plastiques - Thermogravim&rie (TG) des polymkes -
Principes g&&aux
Reference number
IS0 11358:1997(E)

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SIST EN ISO 11358:1999
IS0 11358:1997(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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.
International Standard IS0 11358 was prepared by Technical Committee
ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properfies.
Annex A of this International Standard is for information only.
0 IS0 1997
All 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 the publisher.
International Organization for Standardization
Case postale 56 l CH-1211 Geneve 20 l Switzerland
Internet central @ iso.ch
x.400
c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii

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SIST EN ISO 11358:1999
INTERNATIONAL STANDARD @ IS0 IS0 11358:1997(E)
Plastics - Thermogravimetry (TG) of polymers -
General principles
1 Scope
1.1 This International Standard specifies the general conditions for the analysis of polymers using
thermogravimetric techniques.
1.2 It is applicable to liquids or solids. Solid materials may be in the form of pellets, granules or powders.
Fabricated shapes reduced to appropriate specimen size may also be analysed by this method.
1.3 Thermogravimetry can be used to determine the temperature(s) and rate(s) of decomposition of polymers, and
to measure at the same time the amounts of volatile matter, additives and/or fillers they contain.
1.4 The thermogravimetric measurements may be carried out in a dynamic mode (mass change versus
) or an isothermal mode (mass change versus time at constant
temperature or time under programmed conditions
temperature).
2 Normative reference
The following standard contains provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the edition indicated was valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent edition of the standard indicated below. Members of IEC and IS0 maintain
registers of currently valid International Standards.
- Standard atmospheres for conditioning and testing.
IS0 291 :-‘I, Plastics
3 Definitions
For the purposes of this International Standard, the following definitions apply:
3.1 thermogravimetry (TG): A technique in which the mass of a test specimen is measured as a function of
temperature or time, while the test specimen is subjected to a controlled temperature programme.
3.2 dynamic mass-change determination: A technique for obtaining a record of the variation of the mass of a
test specimen with temperature T which is changing at a programmed rate.
3.3 isothermal mass-change determination: A technique for obtaining a record of the variation of the mass of a
test specimen with time t at constant temperature T.
1) To be published. (Revision of IS0 291:1977)

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SIST EN ISO 11358:1999
@ IS0
IS0 11358: 1997(E)
3.4 TG curve: A curve drawn in thermogravimetry by plotting the mass of a test specimen as the ordinate (y-axis)
and the temperature T, or time t, as the abscissa (x-axis).
3.5 differential scanning calorimetry (DSC): A technique in which the difference in heat flux (power) into a test
specimen and a reference specimen is measured as a function of temperature and/or time while the test specimen
and the reference specimen are subjected to a controlled temperature programme.
3.6 differential thermal analysis (DTA): A technique in which the difference in temperature between a test
specimen and a reference specimen is measured as a function of temperature and/or time while the test specimen
and the reference specimen are subjected to a controlled temperature programme.
3.7 Curie temperature: The temperature at which a ferromagnetic material passes from the ferromagnetic state
to the paramagnetic state or vice versa.
3.8 sample: A small part or portion of a bulk material or batch of products intended to be representative of the
whole.
3.9 test specimen: A complete product or single piece taken from a sample and used to carry out a test. In the
case of bulk materials such as pellets, powders and granules: a portion taken from a sample and used to carry out a
test.
4 Principle
4.1 A test specimen is heated at a constant rate with a controlled temperature programme, and the change in
mass is measured as a function of temperature. Alternatively, the specimen is kept at a given constant temperature
and the change in mass is measured as a function of time over a given period.
In general, the reactions which cause the mass of a test specimen to change are decomposition or oxidation
reactions or the volatilization of a component. The change in mass is recorded as a TG curve.
4.2 The change in mass of a material as a function of temperature and the extent of this change are indicators of
the thermal stability of the material. TG data can therefore be used to evaluate the relative thermal stability of
polymers of the same generic family and polymer-polymer or polymer-additive interactions, using measurements
made under the same test conditions.
4.3 TG data may be used for process control, process development and material evaluation. Long-term thermal
stability is a complex function of service and environmental conditions. TG data alone will not describe the long-term
thermal stability of a polymer.
5 Apparatus
instruments suitab lie for the rmog ravimetric measurements are available. The basic
A number of co mmercial
apparatus compo nents con sist of the fol owing:
5.1 Thermobalance, of the null or deflection type. Where the mass of the test specimen is less than 50 mg, the
thermobalance shall be capable of measuring the mass with an accuracy of + 0,020 mg. The thermobalance shall
be constructed so that gas flows around the test specimen and permits heat transfer to it at a constant rate.
5.2 Furnace, with a housing of low thermal mass to allow rapid or slow heating and cooling (generally at least
50 “C/min) over a temperature range of ambient to about 1 000 “C.
5.3 Temperature sensor, capable of measuring the temperature of the test specimen. It shall be located as close
as possible to the test specimen.
2

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SIST EN ISO 11358:1999
0 IS0 IS0 11358: 1997(E)
5.4 Temperature programmer, capable of providing a linear rate of scanning over a predetermined temperature
range.
5.5 Recording device, capable of recording the specimen mass and temperature and/or time in a way that the
relation between mass loss and temperature or time is illustrated. An X-Y recorder is suitable for this purpose.
5.6 Specimen holder, of shape and dimensions sufficient for a mass of at least 5 mg and made of a material
capable of withstanding the maximum temperature to be used.
5.7 Purge gas: dry air or oxygen (oxidizing conditions) or a suitable inert gas with an oxygen content of
0,001 % (V/V) or less (non-oxidizing conditions). In either case, the water content of the purge gas shall be less than
0,001 % (m/m).
5.8 Flowmeter, capable of measuring gas-flow rates of 50 mI/min to 150 mI/min.
5.9 Balance, capable of measuring the initial mass of the specimen with an accuracy of 0,Ol mg.
6 Test specimen preparation
Test specimens may be liquids or solids. The latter may be in the form of powders, pellets, granules or cut pieces.
For finished products, the test specimen shall be in the form normally found in use.
6.1 Test specimens from finished products
Cut the test specimen to an appropriate size for the specimen holder. Microtomes or razor blades are suitable for
this purpose.
Test specimen size and shape will generally be dependent on the sample holder. Surface area will affect the overall
NOTE -
results. For instance, in comparing a test specimen of large surface area with a test specimen of smaller surface area, both
having the same mass, the smaller surface area test specimen normally changes at a slower rate.
6.2 Test specimen conditioning
Unless otherwise specified, test specimens shall be conditioned, prior to measurement, at 23 “C + 2 “C and
(50 + 5) % relative humidity in accordance with IS0 291, or by any other method specified by agreement between
the interested parties.
6.3 Test specimen mass
The mass of the test specimen shall be greater than 10 mg unless only smaller quantities of material are available.
7 Calibration
7.1 Mass calibration
Without any gas flow through the thermobalance (to prevent any disturbance through buoyancy and/or convection
effects), calibrate the thermobalance as follows, using calibrated weights in the range 10 mg to 100 mg:
Zero the thermobalance. Place the calibration weight on the thermobalance and measure the corresponding mass
change. If necessary, adjust the thermobalance so that the measured mass is equal to the mass of the calibration
weight.

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SIST EN ISO 11358:1999
@ IS0
IS0 11358: 1997(E)
7.2 Temperature calibration
Position the temperature sensor, usually a thermocouple, to provide the most accurate reading of the test specimen
temperature. This position may differ for each instrument.
Carry out the temperature calibration using the same atmosphere, rate of gas flow and heating rate as will be used
in the actual determination (see clause 8).
If the thermobalance is used alone, use the fol
...