Plastics - Differential scanning calorimetry (DSC) - Part 7: Determination of crystallization kinetics (ISO/DIS 11357-7:2021)

Kunststoffe - Dynamische Differenzkalorimetrie (DSC) - Teil 7: Bestimmung der Kristallisationskinetik (ISO/DIS 11357-7:2021)

Dieses Dokument legt zwei Verfahren (das isotherme und nicht-isotherme Verfahren) für die Untersuchung der Kristallisationskinetik teilkristalliner Polymere mittels Dynamischer Differenz-Thermoanalyse (DSC) (Dynamischer Differenzkalorimetrie) fest.
Es ist ausschließlich auf geschmolzene Polymere anwendbar.
ANMERKUNG Diese Verfahren sind nicht geeignet, wenn sich die Molekularstruktur des Polymers während der Prüfung verändert.

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 7: Détermination de la cinétique de cristallisation (ISO/DIS 11357-7:2021)

Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 7. del: Ugotavljanje kristalizacijske kinetike (ISO/DIS 11357-7:2021)

General Information

Status
Not Published
Public Enquiry End Date
31-May-2021
Current Stage
5020 - Formal vote (FV) (Adopted Project)
Start Date
08-Dec-2021
Due Date
26-Jan-2022

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SLOVENSKI STANDARD
oSIST prEN ISO 11357-7:2021
01-maj-2021
Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 7. del:
Ugotavljanje kristalizacijske kinetike (ISO/DIS 11357-7:2021)

Plastics - Differential scanning calorimetry (DSC) - Part 7: Determination of crystallization

kinetics (ISO/DIS 11357-7:2021)
Kunststoffe - Dynamische Differenzkalorimetrie (DSC) - Teil 7: Bestimmung der
Kristallisationskinetik (ISO/DIS 11357-7:2021)

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 7: Détermination de la

cinétique de cristallisation (ISO/DIS 11357-7:2021)
Ta slovenski standard je istoveten z: prEN ISO 11357-7
ICS:
17.200.10 Toplota. Kalorimetrija Heat. Calorimetry
83.080.01 Polimerni materiali na Plastics in general
splošno
oSIST prEN ISO 11357-7:2021 en,fr,de

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

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oSIST prEN ISO 11357-7:2021
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oSIST prEN ISO 11357-7:2021
DRAFT INTERNATIONAL STANDARD
ISO/DIS 11357-7
ISO/TC 61/SC 5 Secretariat: DIN
Voting begins on: Voting terminates on:
2021-03-15 2021-06-07
Plastics — Differential scanning calorimetry (DSC) —
Part 7:
Determination of crystallization kinetics
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 7: Détermination de la cinétique de cristallisation
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
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BE CONSIDERED IN THE LIGHT OF THEIR
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WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 11357-7:2021(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 2021
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oSIST prEN ISO 11357-7:2021
ISO/DIS 11357-7:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

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ii © ISO 2021 – All rights reserved
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oSIST prEN ISO 11357-7:2021
ISO/DIS 11357-7:2021(E)
Contents Page

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

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

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

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

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

5 Apparatus and materials.............................................................................................................................................................................. 2

6 Test specimens........................................................................................................................................................................................................ 2

7 Test conditions and specimen conditioning ............................................................................................................................ 2

8 Calibration .................................................................................................................................................................................................................. 2

8.1 Calibration in heating mode ........................................................................................................................................................ 2

8.2 Symmetry of temperature scale ............................................................................................................................................... 2

9 Procedure..................................................................................................................................................................................................................... 2

9.1 General ........................................................................................................................................................................................................... 2

9.2 Loading the test specimen into the crucible .................................................................................................................. 3

9.3 Insertion of the crucibles into the instrument ............................................................................................................ 3

9.4 Melting of the polymer ..................................................................................................................................................................... 3

9.5 Isothermal crystallisation.............................................................................................................................................................. 3

9.6 Non-isothermal crystallisation ................................................................................................................................................. 5

10 Expression of results ........................................................................................................................................................................................ 5

10.1 General ........................................................................................................................................................................................................... 5

10.2 Methods of determination of crystallisation kinetics ............................................................................................ 5

10.2.1 Isothermal crystallisation ........................................................................................................................................ 5

10.2.2 Non-isothermal crystallisation ............................................................................................................................ 7

11 Precision ....................................................................................................................................................................................................................... 8

12 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Equations for crystallisation kinetics of polymers ..................................................................9

Bibliography .............................................................................................................................................................................................................................11

© ISO 2021 – All rights reserved iii
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oSIST prEN ISO 11357-7:2021
ISO/DIS 11357-7:2021(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 on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO's adherence to the WTO principles in the Technical

Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.

The committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical-

chemical properties.

This third edition cancels and replaces the second edition (ISO 11357-7:2015), which has been

technically revised with the following main changes:

a) an indication of suitable substances for checking the symmetry of the temperature scale has

been added;

b) the procedure of determination of the start temperature of isothermal crystallisation has been

corrected;

c) an approach for the dependence of the rate constant of the Nakamura equation on temperature has

been added.

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 and glass transition step height

— Part 3: Determination of temperature and enthalpy of melting and crystallisation

— Part 4: Determination of specific heat capacity

— Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction

and degree of conversion

— Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature

(dynamic OIT)
— Part 7: Determination of crystallisation kinetics
iv © ISO 2021 – All rights reserved
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oSIST prEN ISO 11357-7:2021
DRAFT INTERNATIONAL STANDARD ISO/DIS 11357-7:2021(E)
Plastics — Differential scanning calorimetry (DSC) —
Part 7:
Determination of crystallization kinetics
1 Scope

This document specifies two methods (isothermal and non-isothermal) for studying the crystallisation

kinetics of partially crystalline polymers using differential scanning calorimetry (DSC).

It is only applicable to molten polymers.

NOTE These methods are not suitable if the molecular structure of the polymer is modified during the test.

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 472, Plastics — Vocabulary

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

ISO 11357-3, Plastics — Differential scanning calorimetry (DSC) — Part 3: Determination of temperature

and enthalpy of melting and crystallization
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472, ISO 11357-1, ISO 11357-3,

and the following 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/
3.1
crystallisation kinetics

description of the rate of crystallisation of a material taking into account the effects of variables such as

time, temperature, pressure, stress, and molecular structure

Note 1 to entry: These factors and also any additives, fillers, or contaminants can modify the crystallinity of the

polymer at the end of crystallisation.
3.2
relative crystallinity

ratio between the crystallinity at a particular point in time or a particular temperature and the

crystallinity at the end of crystallisation

Note 1 to entry: The relative crystallinity can be expressed either as a ratio or as a percentage if multiplied by 100.

© ISO 2021 – All rights reserved 1
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oSIST prEN ISO 11357-7:2021
ISO/DIS 11357-7:2021(E)

Note 2 to entry: In DSC, the relative crystallinity can be determined as the ratio between the partial area of the

crystallisation peak, at each time or each temperature, and the total area of the peak.

4 Principle
The principle is specified in ISO 11357-1.
5 Apparatus and materials
5.1 Differential scanning calorimeter, according to ISO 11357-1.
5.2 Crucibles, according to ISO 11357-1.

It can be necessary to verify that the material used for the crucibles does not modify the crystallisation

kinetics of the polymer.
5.3 Balance, according to ISO 11357-1.
5.4 Heating mode calibration materials, according to ISO 11357-1.
5.5 Substances for checking the symmetry of the temperature scale
Suitable substances shall be selected showing low and defined
...

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