Plastiques -- Analyse calorimétrique différentielle (DSC)

General Information

Status
Published
Current Stage
4020 - DIS ballot initiated: 5 months
Start Date
26-Jul-2001
Ref Project

Buy Standard

Draft
ISO/DIS 11357-4.3 - Plastics -- Differential scanning calorimetry (DSC)
English language
10 pages
world standards week 25% off
Preview
world standards week 25% off
Preview

Standards Content (sample)

DRAFT INTERNATIONAL STANDARD ISO/DIS 11357-4.3
ISO/TC 61/SC 5 Secretariat: SNV
Voting begins on Voting terminates on
2001-08-02 2001-10-02

INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION

Plastics — Differential scanning calorimetry (DSC) —
Part 4:
Determination of specific heat capacity
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 4: Détermination de la capacité thermique massique
ICS 83.080.01

In accordance with the provisions of Council Resolution 15/1993 this document is circulated

in the English language only.

Conformément aux dispositions de la Résolution du Conseil 15/1993, ce document est

distribué en version anglaise seulement.

To expedite distribution, this document is circulated as received from the committee

secretariat. ISO Central Secretariat work of editing and text composition will be undertaken at

publication stage.

Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du

secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au

Secrétariat central de l'ISO au stade de publication.

THIS DOCUMENT IS A DRAFT CIRCULATED 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 BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT

INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO WHICH

REFERENCE MAY BE MADE IN NATIONAL REGULATIONS.
© International Organization for Standardization, 2001
---------------------- Page: 1 ----------------------
ISO/DIS 11357-4.3
Copyright notice

This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted

under the applicable laws of the user’s country, neither this ISO draft nor any extract from it may be

reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic,

photocopying, recording or otherwise, without prior written permission being secured.

Requests for permission to reproduce should be addressed to ISO at the address below or ISO’s member

body in the country of the requester.
Copyright Manager
ISO Central Secretariat
1 rue de Varembé
1211 Geneva 20 Switzerland
tel. + 41 22 749 0111
fax + 41 22 734 1079
internet: iso@iso.ch
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
---------------------- Page: 2 ----------------------
ISO/DIS 11357-4.3
Contents

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

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

3 Definitions ......................................................................................................................................................1

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

5 Apparatus .......................................................................................................................................................3

6 Test specimen................................................................................................................................................3

7 Testing conditions and conditioning of the test specimen.......................................................................4

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

9 Determination of specific heat capacities...................................................................................................7

10 Report .............................................................................................................................................................7

Annex A (informative) An approximate expression of specific heat capacity of pure α-alumina [3~5]...........8

Bibliography..............................................................................................................................................................10

© ISO 2001 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/DIS 11357-4.3
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.

International Standard ISO 11357-4 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee

SC 5, Physical-chemical properties.

ISO 11357 consists of the following parts, under the general title Plastics - Differential scanning calorimetry (DSC):

 Part 1: General principles
 Part 2: Determination of glass transition temperature

 Part 3: Determination of temperature and enthalpy of melting and crystallization

 Part 4: Determination of specific heat capacity

 Part 5: Determination of polymerization temperatures and/or times and polymerization kinetics

 Part 6: Determination of oxidation induction time
 Part 7: Determination of crystallization kinetics
Annex A is for information only.
iv © ISO 2001 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/DIS 11357-4.3
Introduction

A list of standards related to this part of ISO 11357 is given in the bibliography.

© ISO 2001 – All rights reserved v
---------------------- Page: 5 ----------------------
DRAFT INTERNATIONAL STANDARD ISO/DIS 11357-4.3
Plastics — Differential scanning calorimetry (DSC) – Part 4:
Determination of specific heat capacity
1 Scope

This International Standard specifies the method for determining of specific heat capacity of plastics by differential

scanning calorimetry.
2 Normative references

The following standards contain the provisions which, through reference in this text, constitute provisions of this

International Standard. At the time of publication, the editions indicated were 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 standards indicated below. Members of IEC and ISO maintain

registers of currently valid International standards.
ISO 472:1999, Plastics – Vocabulary.

ISO11357-1, Plastics-Differential Scanning Calorimetry (DSC) - Part 1: General principles.

ISO31-0, General Principles.
3 Definitions

For the purposes of this International Standard, the terms and definitions given in ISO 11357-1 and the following

apply.
3.1
Calibration material
materials whose specific heat capacity values have been established are used

NOTE Usually, α-alumina (such as synthetic sapphire ) of 99.9% or higher purity is used as a calibration material.

3.2
Specific heat capacity (at constant pressure)

The quantity of heat necessary to raise the temperature of unit mass of material by 1 K at constant pressure. It is

indicated by c , and the following equation is obtained:
. .
-1 -1
cp = m Cp = m (dQ / dT)p (1)

where m is the mass of the material, C is the heat capacity and dQ is the heat quantity necessary to raise the

temperature of the material by dT. Subscript p indicates an isobaric process. c is expressed in kilojoules per

. . . .
-1 -1 -1 -1
kilogram per K (kJ kg K ) or in joule per gram per K (J g K ).

This equation is valid in a temperature range where a material shows no first order phase transition.

(dQ / dT) = (dt / dT ) (dQ / dt)
-1 .
= (heating rate) (heat flow rate) (2)
© ISO 2001 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/DIS 11357-4.3
4 Principle

Each measurement consists of three test at the same scanning rate runs as follow (figure 1) (Annex A[1,2]):

(1) blank run (set of empty pans in DSC holders)
(2) calibration run (calibration material and empty pan)
(3) specimen run (specimen and empty pan).

Based on the DSC principle (ISO 11357-1) and the definition of the specific heat capacity as described in 3.2, the

following relations are obtained, where P is dQ / dt , specimen is a part of sample for measurement and the

superscrips of sp and cal represent specimen and calibration:
sp sp
m c ∝ P - P (3)
p specimen run blank run
cal cal
m c ∝ P - P (4)
p calibration run blank run
Where P shows the DSC signal, when P , P and P are measured, c can be
run specimen run calibration run blank run p
cal cal sp
calculated using equation (6), since c , m and m are known values
sp sp
m c P - P
p specimen run blank run
= (5)
cal
cal
m c P - P
p calibration run blank run
cal
m (P - P )
specimen run blan k run
sp cal
c = c (6)
p p
m (P - P )
calibration run blank run

NOTE Certain types of DSC can be calibrated using electrical calibration (Joule effect). In this case, it is not needed to

refer to a calibration run.
2 © ISO 2001 – All rights reserved
---------------------- Page: 7 ----------------------
ISO/DIS 11357-4.3

Figure 1 — Typical DSC curve on specific heat capacity measurement after baseline adjuststment

I ; isothermal baseline at T , II ; isothermal baseline at T
b f
5 Apparatus
5.1 DSC apparatus
See ISO 11357-1, clause 5.1
5.2 Pan
(See ISO 11357-1, clause 5.2)

NOTE 1 Pans for the test specimen and the reference should be of the same shape, material and the mass should be

equal.

NOTE 2 The same blank run and calibration run can be used for several measurements, if the instrument is sufficiently

stable and the mass difference between calibration material pan and empty pan is corrected. An adequate correction can be

obtained by adding the term c (T) β ∆m to the heat flow rate signal of the sample, where c is specific heat capacity of

p pan p p
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.