ISO 11357-7:2002

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

This part of ISO 11357 specifies two methods, isothermal and non-isothermal, for studying the crystallization kinetics of partially crystalline polymers using differential scanning calorimetry (DSC). It is only applicable to melted polymers. NOTE These methods are not suitable if the molecular structure of the polymer is modified during the test.

Plastiques — Analyse calorimétrique différentielle (DSC) — Partie 7: Détermination de la cinétique de cristallisation

L'ISO 11357-7:2002 spécifie deux méthodes, isotherme et non isotherme, permettant d'étudier la cinétique de cristallisation de polymères semi-cristallins en utilisant l'analyse calorimétrique différentielle (DSC). Elle s'applique uniquement aux polymères fondus.

General Information

• Status: Withdrawn
• Publication Date: 05-Jun-2002
• Withdrawal Date: 05-Jun-2002
• ICS: 83.080.01 - Plastics in general
• Technical Committee: ISO/TC 61/SC 5 - Physical-chemical properties
• Drafting Committee: ISO/TC 61/SC 5/WG 8 - Thermal analysis
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 10-Aug-2015

Relations

• Revised: ISO 11357-7:2015 - Plastics — Differential scanning calorimetry (DSC) — Part 7: Determination of crystallization kinetics
• Effective Date: 10-Mar-2012

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 11357-7
First edition
2002-05-01
Plastics — Differential scanning calorimetry
(DSC) —
Part 7:
Determination of crystallization kinetics
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 7: Détermination de la cinétique de cristallisation

Reference number
ISO 11357-7:2002(E)
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ISO 2002

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ISO 11357-7:2002(E)
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ISO 11357-7:2002(E)
Contents Page
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 . 3
8 Calibration . 3
9 Procedure . 3
10 Expression of results . 5
11 Precision . 7
12 Test report . 7
Annex
A Equations for crystallization kinetics of polymers. 8
Bibliography. 10
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ISO 11357-7:2002(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 11357 may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 11357-7 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 characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of
conversion
— Part 6: Determination of oxidation induction time
— Part 7: Determination of crystallization kinetics
— Part 8: Determination of amount of absorbed water
Annex A of this part of ISO 11357 is for information only.
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INTERNATIONAL STANDARD ISO 11357-7:2002(E)
Plastics — Differential scanning calorimetry (DSC) —
Part 7:
Determination of crystallization kinetics
1 Scope
This part of ISO 11357 specifies two methods, isothermal and non-isothermal, for studying the crystallization kinetics
of partially crystalline polymers using differential scanning calorimetry (DSC).
It is only applicable to melted polymers.
NOTE These methods are not suitable if the molecular structure of the polymer is modified during the test.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this part of ISO 11357. 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 11357 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 472, Plastics — Vocabulary
ISO 11357-1:1997, 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 part of ISO11357, the terms and definitions given in ISO472, ISO11357-1 and
ISO 11357-3 and the following apply.
3.1
crystallization kinetics
description of the rate of crystallization of a material taking into account the effects of variables such as time,
temperature, pressure, stress and molecular structure
NOTE These factors and also any additives, fillers or contaminants can modify the crystallinity of the polymer at the end of
crystallization.
3.2
relative crystallinity
α
the ratio between the crystallinity at a particular point in time or a particular temperature and the crystallinity at the
end of crystallization
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ISO 11357-7:2002(E)
NOTE 1 The relative crystallinity is given by the ratio of the partial enthalpy of crystallization, at each time or each temperature,
and the total enthalpy of crystallization ∆H :
c
α =∆H /∆H
t orT t orT c
where
α and ∆H are the relative crystallinity and the enthalpy of crystallization at a given time in the isothermal mode;
t t
α and ∆H are the relative crystallinity and the enthalpy of crystallization at a given temperature in the non-isothermal
T T
mode.
NOTE 2 In DSC, the relative crystallinity can be determined as the ratio between the partial area of the crystallization peak, at
each time or each temperature, and the total area of the peak.
4Principle
See ISO 11357-1:1997, clause 4.
5 Apparatus and materials
5.1 Differential scanning calorimeter
Use a differential scanning calorimeter meeting the following requirements:
◦
a) capable of generating constant heating and cooling rates, preferably at least 40 C/min;
◦
b) capable of maintaining the test temperature constant to within ± 0,1C6 for at least 0min;
c) to h) see ISO 11357-1:1997, subclause 5.1, items c) to h).
5.2 Crucibles
See ISO 11357-1:1997, subclause 5.2.
It may be necessary to verify that the metal of these crucibles does not modify the crystallization kinetics of the
polymer.
5.3 Balance
See ISO 11357-1:1997, subclause 5.3.
5.4 Calibration materials
See ISO 11357-1:1997, annex A.
5.5 Purge gas
The gas used shall be a dry inert gas of analytical grade in order to avoid oxidation and hydrolytic degradation.
6 Test specimens
See ISO 11357-1:1997, clause 6.
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ISO 11357-7:2002(E)
7 Test conditions and specimen conditioning
See ISO 11357-1:1997, clause 7.
8 Calibration
See ISO 11357-1:1997, clause 8.
Temperature calibration shall be carried out in the heating mode only. The temperature correction terms in the
isothermal or cooling mode are determined by linear extrapolation of values measured at different heating rates.
The linearity of the temperature scale in the heating and cooling modes shall be checked using materials which do
not supercool. The use of the liquid-liquid transition of liquid crystals or the use of 4,4'-azoxyanisole is recommended.
9 Procedure
...