Plastics - Differential scanning calorimetry (DSC) - Part 8: Determination of thermal conductivity (ISO/FDIS 11357-8:2020)

See title

Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 8: Bestimmung der Wärmeleitfähigkeit (ISO/FDIS 11357-8:2020)

Dieses Dokument legt ein Verfahren zur Bestimmung der Wärmeleitfähigkeit von festen ungefüllten und gefüllten oder faserverstärkten Kunststoffen und Verbundstoffen durch die Dynamische Differenz-Thermoanalyse (DSC) fest.
Es ist anwendbar für Werkstoffe mit Wärmeleitfähigkeiten bis zu 1 W/(m ⋅ K).

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 8: Détermination de la conductivité thermique (ISO/FDIS 11357-8:2020)

Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 8. del: Ugotavljanje toplotne prevodnosti (ISO/FDIS 11357-8:2020)

General Information

Status
Not Published
Technical Committee
Drafting Committee
Current Stage
6055 - CEN Ratification completed (DOR) - Publishing
Due Date
25-Jan-2021
Completion Date
25-Jan-2021

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SLOVENSKI STANDARD
oSIST prEN ISO 11357-8:2020
01-marec-2020
Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 8. del:
Ugotavljanje toplotne prevodnosti (ISO/DIS 11357-8:2019)

Plastics - Differential scanning calorimetry (DSC) - Part 8: Determination of thermal

conductivity (ISO/DIS 11357-8:2019)
Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 8: Bestimmung der
Wärmeleitfähigkeit (ISO/DIS 11357-8:2019)

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 8: Détermination de la

conductivité thermique (ISO/DIS 11357-8:2019)
Ta slovenski standard je istoveten z: prEN ISO 11357-8
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
oSIST prEN ISO 11357-8:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN ISO 11357-8:2020
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oSIST prEN ISO 11357-8:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 11357-8
ISO/TC 61/SC 5 Secretariat: DIN
Voting begins on: Voting terminates on:
2019-12-31 2020-03-24
Plastics — Differential scanning calorimetry —
Part 8:
Determination of thermal conductivity
ICS: 83.080.01
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
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STANDARDS MAY ON OCCASION HAVE TO
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WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 11357-8:2019(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. ISO 2019
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oSIST prEN ISO 11357-8:2020
ISO/DIS 11357-8:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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

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ii © ISO 2019 – All rights reserved
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oSIST prEN ISO 11357-8:2020
ISO/DIS 11357-8:2019(E)
Contents Page

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

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 1

5 Apparatus and substances.......................................................................................................................................................................... 2

5.1 DSC instrument ....................................................................................................................................................................................... 2

5.2 Crucibles ....................................................................................................................................................................................................... 2

5.3 Melting substance ................................................................................................................................................................................. 2

5.4 Protective lacquer................................................................................................................................................................................. 3

5.5 Length measuring device ............................................................................................................................................................... 3

6 Specimens .................................................................................................................................................................................................................... 3

6.1 Geometry ...................................................................................................................................................................................................... 3

6.2 Number and sampling ...................................................................................................................................................................... 3

7 Conditioning .............................................................................................................................................................................................................. 3

8 Calibration .................................................................................................................................................................................................................. 4

9 Measurement procedure .............................................................................................................................................................................. 4

9.1 Preparation of crucibles .................................................................................................................................................................. 4

9.2 Use of thermal contact substances ........................................................................................................................................ 4

9.3 Measurement of melting substance ...................................................................................................................................... 4

9.3.1 Placing of crucibles in sample holder ............................................................................................................ 4

9.3.2 Distribution of melting substance on crucible ground ................................................................... 4

9.3.3 Measurement of the slope of the melting curve without test specimen .......................... 5

9.3.4 Insertion of test specimen ....................................................................................................................................... 5

9.3.5 Measurement of the slope of the melting curve with test specimen .................................. 5

9.4 E valuation of the slope of the peaks of the melting substance ...................................................................... 5

10 Calculation of thermal conductivity ................................................................................................................................................. 7

11 Service life of crucibles upon using gallium as melting substance ..................................................................7

12 Precision and bias ............................................................................................................................................................................................... 7

13 Test report ................................................................................................................................................................................................................... 7

Annex A (informative) Interlaboratory determination of thermal conductivity measured by

means of DSC ............................................................................................................................................................................................................ 9

Bibliography .............................................................................................................................................................................................................................15

© ISO 2019 – All rights reserved iii
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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 5, Physical-

chemical properties.
A list of all parts in the ISO 11357 series can be found on the ISO website.

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 2019 – All rights reserved
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Introduction

The advantage of using DSC for measuring the thermal conductivity of plastics is that with the same

instrument also the specific heat capacity can be obtained. This enables the determination of the

thermal diffusivity by dividing the thermal conductivity by the density and specific heat capacity.

In addition, DSC instruments are widely-used and available in almost all test institutes and labs. Hence,

measurements of thermal conductivity can be done without need for procurement of an additional

instrument.
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oSIST prEN ISO 11357-8:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 11357-8:2019(E)
Plastics — Differential scanning calorimetry —
Part 8:
Determination of thermal conductivity
1 Scope

This document establishes a method for determination of the thermal conductivity of solid unfilled and

filled or fibre reinforced plastics and composites by means of Differential Scanning Calorimetry (DSC).

It is applicable for materials with thermal conductivities of up to 1 W/(m⋅K).
2 Normative references

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

constitutes 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 291, Plastics — Standard atmospheres for conditioning and testing
ISO 472, Plastics — Vocabulary

ISO 6344-1, Coated abrasives — Grain size analysis — Part 1: Grain size distribution test

ISO 11357-1, Plastics — Differential scanning calorimetry (DSC) — Part 1: General principles

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472 and ISO 11357-1 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 http:// www .electropedia .org/
4 Principle

For the determination of thermal conductivity, the usual placement of the specimen in the sample holder

position is modified according to a procedure proposed in the literature.[1],[2] Additional details on

scientific background, deduction of results and performance of measurements can be found in[3] and [4].

As usual, an empty crucible is placed in the reference position of the sample holder assembly. The test

specimen is placed directly onto the sensor of the sample position and a crucible containing a substance

of known melting temperature is put on top of the specimen (see Figure 1). The thermal conductivity is

measured at a temperature slightly above the melting point of this substance in the small temperature

range in which the slope of the melting peak with test specimen is determined (see 9.2, Figure 2)..

Upon heating, a temperature gradient is created in the specimen. The temperature of the top of

the specimen remains constant at the melting temperature T of the melting substance while the

temperature of the bottom side of the specimen corresponds to the temperature of the sample side

sensor. The differential heat flow between sample and reference sensor is measured by the DSC

instrument.
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ISO/DIS 11357-8:2019(E)

From the temperature difference between top and bottom of the sample (T - T ), the sample height h

m p

and the heat flow rate difference Q between sample and the reference sensor, the thermal conductivity

of the specimen is determined.
Key
h height of specimen
heat flow rate difference between sample and reference position
S sensor of sample position
S sensor of reference position

T melting temperature of known substance and temperature of top of specimen, respectively

T temperature of sample position and bottom side of specimen, respectively
T temperature of reference position
Figure 1 — Schematic layout of measurement
5 Apparatus and substances
5.1 DSC instrument

A DSC instrument in accordance with specifications given in ISO 11357-1 shall be used.

Only original raw data shall be used without any further data processing.

NOTE According to currently available results the method has been verified with heat-flux type DSC

instruments only. However, it is expected that power-compensated DSC instruments are suitable, too.

5.2 Crucibles

Aluminium crucibles shall be used fitting the DSC instrument. Both, open or ventilated closed crucibles

are suitable. Upon using sealed crucibles suitable precautions shall be taken to prevent excessive inside

pressure.
Care shall be taken to avoid deformation of the plane crucible bottom.
NOTE Uneven crucible bottoms may result in too low thermal conductivity values.
5.3 Melting substance

Certified melting substances or melting substances having a purity of 99,9999 % or better shall be used.

The melting temperature determines the temperature of measurement of the thermal conductivity.

Melting temperatures of specimens to be measured shall be above those of the melting substances to be

used. In case of doubt, this shall be ensured by performing suitable preliminary tests.

NOTE Metals such as gallium or indium have been found suitable.
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5.4 Protective lacquer
If metals that can react with the crucible material are used as melting subst
...

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