Plastics - Differential scanning calorimetry (DSC) - Part 1: General principles (ISO 11357-1:2016)

ISO 11357 specifies several differential scanning calorimetry (DSC) methods for the thermal analysis of
polymers and polymer blends, such as
— thermoplastics (polymers, moulding compounds and other moulding materials, with or without
fillers, fibres or reinforcements),
— thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements), and
— elastomers (with or without fillers, fibres or reinforcements).
ISO 11357 is intended for the observation and measurement of various properties of, and phenomena
associated with, the above-mentioned materials, such as
— physical transitions (glass transition, phase transitions such as melting and crystallization,
polymorphic transitions, etc.),
— chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.),
— the stability to oxidation, and
— the heat capacity.
This part of ISO 11357 specifies a number of general aspects of differential scanning calorimetry, such
as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test
report common to all following parts.
Details on performing specific methods are given in subsequent parts of ISO 11357 (see Foreword).

Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine Grundlagen (ISO 11357-1:2016)

SICHERHEITSHINWEIS — Personen, die dieses Dokument anwenden, sollten mit der üblichen Laborpraxis vertraut sein. Das vorliegende Dokument beabsichtigt nicht, alle mit dessen Anwendung verbundenen Sicherheitsprobleme, soweit sich solche ergeben, anzusprechen. Es liegt in der Verantwortung des Anwenders, entsprechende Arbeits- und Gesundheitsvorkehrungen zu treffen und deren Übereinstimmung mit den Rahmenbedingungen sicherzustellen.
Diese Internationale Norm legt verschiedene Verfahren der Dynamischen Differenz Thermoanalyse (en: differential scanning calorimetry, DSC) zur thermischen Analyse von Polymeren und Polymermischungen fest, wie z. B. von:
   Thermoplasten (Polymeren, Formmassen und Produkten des Formpressens mit oder ohne Füllstoffen, Fasern oder Verstärkungsstoffe);
   Duroplasten (gehärteten oder ungehärteten Materialien mit oder ohne Füllstoffen, Fasern oder Verstärkungsstoffen);
   Elastomeren (mit oder ohne Füllstoffen, Fasern oder Verstärkungsstoffen).
Diese Internationale Norm wird zwecks Beobachtung und quantitativer Erfassung verschiedener Erscheinungen oder Eigenschaften der oben genannten Materialien angewendet, wie z. B.:
   physikalischer Umwandlungen (Glasübergang, Phasenumwandlungen wie Schmelzen oder Kristallisa-tion, polymorphen Umwandlungen usw.);
   chemischer Reaktionen (Polymerisation, Vernetzung und Vulkanisation von Elastomeren und Duro-plasten usw.);
   Oxidationsstabilität; und
   Wärmekapazität.
Dieser Teil von ISO 11357 legt eine Reihe allgemeiner Grundsätze der Dynamischen Differenz Thermo-analyse fest, wie z. B. Kurzbeschreibung des Verfahrens und der Geräte, Probenahme, Kalibrierung sowie allgemeine Aspekte des Verfahrens und des Prüfberichts, die allen darauf folgenden Teilen gemeinsam sind.

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 1: Principes généraux (ISO 11357-1:2016)

ISO 11357-1:2016 spécifie plusieurs méthodes d'analyse calorimétrique différentielle (DSC) pour l'analyse thermique des polymères et des mélanges de polymères tels que
- thermoplastiques (polymères, composants pour moulage et autres produits pour moulage avec ou sans charge(s), fibres ou additifs de renforcement),
- thermodurcissables (matériaux non durcis ou durcis, avec ou sans charge(s), fibres ou additifs de renforcement), et
- élastomères (avec ou sans charge(s), fibres ou additifs de renforcement).
ISO 11357-1:2016 s'applique pour l'observation et le mesurage de différentes propriétés ou phénomènes associés des matériaux susmentionnés tels que
- les transitions physiques (transition vitreuse, transitions de phases telles que la fusion et la cristallisation, les transitions polymorphes, etc.),
- les réactions chimiques (polymérisation, réticulation et durcissement des élastomères et des thermodurcissables, etc.),
- la stabilité à l'oxydation, et
- la capacité thermique.
ISO 11357-1:2016 établit un nombre d'aspects généraux de l'analyse calorimétrique différentielle tels que le principe et l'appareillage, l'échantillonnage, l'étalonnage et les aspects généraux du mode opératoire et du rapport d'essai communs à toutes les parties suivantes.
Les détails relatifs à la réalisation des méthodes spécifiques sont donnés dans les autres parties de l'ISO 11357 (voir l'Avant-propos).

Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 1. del: Splošna načela (ISO 11357-1:2016)

Standard ISO 11357 določa različne metode diferenčne dinamične kalorimetrije (DSC) za toplotno analizo polimerov in mešanic polimerov, kot so:
– plastomeri (polimeri, zmesi za oblikovanje in drug material za oblikovanje, s polnili, vlakni in ojačitvami ali brez njih),
– termoreaktivni materiali (nestrjeni ali strjeni materiali s polnili, vlakni in ojačitvami ali brez njih) in – elastomeri (s polnili, vlakni in ojačitvami ali brez njih).
Standard ISO 11357 je namenjen za opazovanje in merjenje različnih lastnosti (in z njimi povezanih pojavov) zgoraj omenjenih materialov, kot so:
– fizične prehodnosti (prehodnost stekla, prehodna stanja, kot sta topljenje in kristalizacija,
polimorfna prehodnost, itd.),
– kemične reakcije (polimerizacija, prečno povezovanje in strjevanje elastomerov in termoreaktivnih materialov itd.),
– odpornost proti oksidaciji in
– toplotna kapaciteta.
Ta del standarda ISO 11357 določa število splošnih lastnosti diferenčne dinamične kalorimetrije, kot so načelo in aparat, vzorčenje, kalibracija splošnih lastnosti postopka in poročila o preskušanju, skupna vsem naslednjim delom.
Podrobnosti o izvajanju določenih metod so podane v naslednjih delih standarda ISO 11357 (glej predgovor).

General Information

Status
Published
Public Enquiry End Date
04-Jul-2016
Publication Date
07-Nov-2016
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
27-Oct-2016
Due Date
01-Jan-2017
Completion Date
08-Nov-2016

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Standards Content (sample)

SLOVENSKI STANDARD
SIST EN ISO 11357-1:2016
01-december-2016
1DGRPHãþD
SIST EN ISO 11357-1:2010
3ROLPHUQLPDWHULDOL'LIHUHQþQDGLQDPLþQDNDORULPHWULMD '6& GHO6SORãQD
QDþHOD ,62

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

-1:2016)
Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine
Grundlagen (ISO 11357-1:2016)

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 1: Principes généraux

(ISO 11357-1:2016)
Ta slovenski standard je istoveten z: EN ISO 11357-1:2016
ICS:
17.200.10 Toplota. Kalorimetrija Heat. Calorimetry
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 11357-1:2016 en,fr,de

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

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SIST EN ISO 11357-1:2016
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SIST EN ISO 11357-1:2016
EN ISO 11357-1
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2016
EUROPÄISCHE NORM
ICS 83.080.01 Supersedes EN ISO 11357-1:2009
English Version
Plastics - Differential scanning calorimetry (DSC) - Part 1:
General principles (ISO 11357-1:2016)

Plastiques - Analyse calorimétrique différentielle (DSC) Kunststoffe - Dynamische Differenz-Thermoanalyse

- Partie 1: Principes généraux (ISO 11357-1:2016) (DSC) - Teil 1: Allgemeine Grundlagen (ISO 11357-

1:2016)
This European Standard was approved by CEN on 13 August 2016.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11357-1:2016 E

worldwide for CEN national Members.
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SIST EN ISO 11357-1:2016
EN ISO 11357-1:2016 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 11357-1:2016
EN ISO 11357-1:2016 (E)
European foreword

This document (EN ISO 11357-1:2016) has been prepared by Technical Committee ISO/TC 61 “Plastics”

in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by

NBN.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by April 2017, and conflicting national standards shall be

withdrawn at the latest by April 2017.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent

rights.
This document supersedes EN ISO 11357-1:2009.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
Endorsement notice

The text of ISO 11357-1:2016 has been approved by CEN as EN ISO 11357-1:2016 without any

modification.
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SIST EN ISO 11357-1:2016
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SIST EN ISO 11357-1:2016
INTERNATIONAL ISO
STANDARD 11357-1
Third edition
2016-09-15
Plastics — Differential scanning
calorimetry (DSC) —
Part 1:
General principles
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 1: Principes généraux
Reference number
ISO 11357-1:2016(E)
ISO 2016
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland

All rights reserved. Unless otherwise specified, 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 below or ISO’s member body in the country of

the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction ................................................................................................................................................................................................................................vi

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

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

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

4 Basic principles ...................................................................................................................................................................................................... 8

4.1 General ........................................................................................................................................................................................................... 8

4.2 Heat-flux DSC ............................................................................................................................................................................................ 8

4.3 Power-compensation DSC ............................................................................................................................................................. 8

5 Apparatus and materials.............................................................................................................................................................................. 9

6 Specimen ....................................................................................................................................................................................................................10

7 Test conditions and specimen conditioning .........................................................................................................................11

7.1 Test conditions .....................................................................................................................................................................................11

7.2 Conditioning of specimens ........................................................................................................................................................11

8 Calibration ...............................................................................................................................................................................................................11

8.1 General ........................................................................................................................................................................................................11

8.2 Calibration materials ......................................................................................................................................................................12

8.3 Temperature calibration ..............................................................................................................................................................12

8.3.1 General...................................................................................................................................................................................12

8.3.2 Procedure ............................................................................................................................................................................12

8.3.3 Accuracy of calibration ............................................................................................................................................13

8.4 Heat calibration ...................................................................................................................................................................................13

8.4.1 General...................................................................................................................................................................................13

8.4.2 Procedure ............................................................................................................................................................................14

8.4.3 Accuracy of calibration ............................................................................................................................................14

8.5 Heat flow rate calibration ...........................................................................................................................................................15

8.5.1 General...................................................................................................................................................................................15

8.5.2 Procedure ............................................................................................................................................................................15

9 Procedure..................................................................................................................................................................................................................17

9.1 Setting up the apparatus..............................................................................................................................................................17

9.1.1 Switching on .....................................................................................................................................................................17

9.1.2 Purge gas .................. .................................................... ........................................................................................................17

9.1.3 Experimental conditions ........................................................................................................................................17

9.1.4 Baseline determination ...........................................................................................................................................17

9.2 Loading the specimen into the crucible .........................................................................................................................17

9.2.1 General...................................................................................................................................................................................17

9.2.2 Selection of crucibles ................................................................................................................................................18

9.2.3 Weighing the specimen crucible......................................................................................................................18

9.2.4 Loading the specimen ........................................................................................................................................... ....18

9.2.5 Determination of the mass of the specimen..........................................................................................18

9.3 Insertion of crucibles into the instrument ...................................................................................................................18

9.4 Performing measurements ........................................................................................................................................................18

9.4.1 General...................................................................................................................................................................................18

9.4.2 Scanning mode ...............................................................................................................................................................18

9.4.3 Isothermal mode ...........................................................................................................................................................19

9.5 Post-run checks ...................................................................................................................................................................................20

9.5.1 Check for loss in mass ..............................................................................................................................................20

9.5.2 Inspection of specimens .........................................................................................................................................20

9.5.3 Checking of crucibles and crucible holder ..............................................................................................20

10 Test report ................................................................................................................................................................................................................20

© ISO 2016 – All rights reserved iii
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
[12]

Annex A (normative) Extended, high-precision, temperature calibration .......................................................22

Annex B (normative) Extended, high-precision, heat calibration ......................................................................................24

Annex C (informative) Recommended calibration materials ..................................................................................................26

Annex D (informative) Interaction of calibration materials with different crucible materials ...........29

Annex E (informative) General recommendations .............................................................................................................................31

Bibliography .............................................................................................................................................................................................................................33

iv © ISO 2016 – All rights reserved
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(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 11357-1:2009), 3.7.2 of which has been

technically revised.

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 crystallization kinetics
© ISO 2016 – All rights reserved v
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
Introduction

ISO 11357 describes thermoanalytical DSC test methods which can be used for quality assurance

purposes, for routine checks of raw materials and finished products or for the determination of

comparable data needed for data sheets or databases. The procedures given in ISO 11357 apply as long

as product standards or standards describing special atmospheres for conditioning of specimens do

not specify otherwise.
vi © ISO 2016 – All rights reserved
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SIST EN ISO 11357-1:2016
INTERNATIONAL STANDARD ISO 11357-1:2016(E)
Plastics — Differential scanning calorimetry (DSC) —
Part 1:
General principles

SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory

practice, if applicable. This document does not purport to address all of the safety concerns, if

any, associated with its use. It is the responsibility of the user to establish appropriate safety

and health practices and to ensure compliance with any regulatory requirements.
1 Scope

ISO 11357 specifies several differential scanning calorimetry (DSC) methods for the thermal analysis of

polymers and polymer blends, such as

— thermoplastics (polymers, moulding compounds and other moulding materials, with or without

fillers, fibres or reinforcements),

— thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements), and

— elastomers (with or without fillers, fibres or reinforcements).

ISO 11357 is intended for the observation and measurement of various properties of, and phenomena

associated with, the above-mentioned materials, such as

— physical transitions (glass transition, phase transitions such as melting and crystallization,

polymorphic transitions, etc.),

— chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.),

— the stability to oxidation, and
— the heat capacity.

This part of ISO 11357 specifies a number of general aspects of differential scanning calorimetry, such

as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test

report common to all following parts.

Details on performing specific methods are given in subsequent parts of ISO 11357 (see Foreword).

2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. 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 80000-5, Quantities and units — Part 5: Thermodynamics
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472 and ISO 80000-5 and the

following apply.
© ISO 2016 – All rights reserved 1
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
3.1
differential scanning calorimetry
DSC

technique in which the difference between the rate of flow of heat into a specimen crucible containing

the specimen and that into a reference crucible (3.3) is derived as a function of temperature and/or time

while the specimen and reference are subjected to the same controlled temperature programme in a

specified atmosphere using a symmetrical measurement system

Note 1 to entry: It is common practice to record, for each measurement run, a curve in which temperature or time

is plotted as the abscissa and heat flow rate (3.4) difference as the ordinate. The endothermic and/or exothermic

direction is indicated on the DSC curve.

Note 2 to entry: According to the principles of thermodynamics, energy absorbed by a system is considered

positive while energy released is negative. This approach implies that the endothermic direction points upwards

in the ordinate and the exothermic direction downwards (see Figures 1 and 2). It also has the advantage that the

direction of thermal effects in plots of heat flow rate (3.4) and specific heat is consistent.

3.2
calibration material

material for which one or more of the thermal properties are sufficiently homogeneous and

well established to be used for the calibration of a DSC instrument or for the assessment of a

measurement method
3.3
reference crucible
crucible used on the reference side of the symmetrical crucible holder assembly
Note 1 to entry: Normally, the reference crucible is empty.

Note 2 to entry: In special cases, such as the measurement of highly filled or reinforced polymers or specimens

having a heat capacity comparable to that of the crucible, a suitable material can be used inside the reference

crucible. This reference material should be thermally inactive over the temperature and time range of interest

and its heat capacity should be similar to that of the specimen. In the case of filled or reinforced products, the

pure filler or reinforcement can be used, for example.
3.4
heat flow rate
quantity of heat transferred per unit time (dQ/dt)
Note 1 to entry: It is expressed in watts (W) or milliwatts (mW).

Note 2 to entry: The total quantity of heat transferred, Q, corresponds to the time integral of the heat flow rate:

Q =∫ dt
3.5
change in heat

quantity of heat absorbed (endothermic, ΔQ positive) or released (exothermic, ΔQ negative) within a

specified time, t, or temperature, T, range by a specimen undergoing a chemical or physical change

and/or a temperature change:
ΔQ = dt
60 dQ
ΔQ = dT
β dt
2 © ISO 2016 – All rights reserved
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
where

ΔQ is expressed in joules (J) or as a specific quantity, Δq, expressed in joules per amount of material

−1 −1
in grams (J⋅g ) or joules per amount of material in moles (J⋅mol );

β is the constant heating or cooling rate, dT/dt, expressed in kelvins per minute (K⋅min ).

Note 1 to entry: If measurements are made at constant pressure, ΔQ corresponds to the change in enthalpy, ΔH.

3.6
specific heat capacity at constant pressure

quantity of heat necessary to raise the temperature of unit mass of material by 1 K at constant pressure:

 
1dQ
c =×
 
m dT
 
 
160 dQ
c =× ×
 
m β dt
 
where

dQ is the quantity of heat, expressed in joules (J), necessary to raise the temperature of an amount

of material of mass m, expressed in grams (g), by dT kelvins at constant pressure;

β is the heating rate, expressed in kelvins per minute (K⋅min );
−1 −1
c is expressed in joules per gram per kelvin (J⋅g ⋅K ).
−1 −1

Note 1 to entry: c may also be expressed in joules per mole per kelvin (J⋅mol ⋅K ) when the amount of material,

m, is expressed in moles.

Note 2 to entry: When analysing polymers, ensure that the measured specific heat capacity does not include any

heat change due to a chemical reaction or a physical transition.
3.7
baseline
part of the recorded curve in which no reactions or transitions take place

Note 1 to entry: This can be an isothermal baseline when the temperature is maintained constant or a dynamic

baseline when the temperature is changed in accordance with a controlled temperature programme.

Note 2 to entry: The baselines defined in 3.7.1 to 3.7.3 refer to the quasi-stationary range only, i.e. when the

instrument is operating under stable conditions shortly after starting and shortly before ending the DSC run (see

Figure 1).
© ISO 2016 – All rights reserved 3
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
Key
dQ/dt heat flow rate 4 virtual baseline
T temperature 5 instrument baseline
t time 6 quasi-stationary range
1 dQ/dt vs t (or T) 7 isothermal start baseline
2 T vs t 8 isothermal end baseline
3 specimen baselines Endothermic direction.
Figure 1 — Schematic drawing showing baselines
3.7.1
instrument baseline

curve obtained using only empty crucibles of identical mass and material in the specimen and reference

positions of the DSC cell

Note 1 to entry: The instrument baseline is required for heat capacity measurements.

3.7.2
specimen baseline

DSC curve obtained outside any reaction or transition zone(s) while the instrument is loaded with both

the specimen in the specimen crucible and the reference crucible (3.3)

Note 1 to entry: In this part of the curve, the difference in heat flow rate (3.4) between the specimen crucible and

the reference crucible (3.3) depends solely on the heat capacity of the specimen and the instrument baseline (3.7.1).

Note 2 to entry: The specimen baseline reflects the temperature dependence of the heat capacity of the specimen.

Note 3 to entry: For heat capacity determinations, a dynamic DSC curve is required and, in addition, the

instrument baseline (3.7.1) and the isothermal start and end baselines (see Figure 1).

4 © ISO 2016 – All rights reserved
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SIST EN ISO 11357-1:2016
ISO 11357-1:2016(E)
3.7.3
virtual baseline

imaginary line drawn through a reaction and/or transition zone assuming the heat of reaction and/or

transition to be zero

Note 1 to entry: Assuming the change in heat capacity with temperature to be linear, the virtual baseline is

drawn by interpolating or extrapolating the specimen baseline in a straight line. It is normally indicated on the

DSC curve for convenience (see Figures 1 and 2).

Note 2 to entry: The virtual baseline drawn from peak onset, T , to peak end, T , (the peak baseline) allows the

i f

determination of the peak area from which the heat of transition can be obtained. If there is no significant change

in heat capacity during the transition or reaction, the baseline can be drawn simply by connecting the peak onset

and peak end by a straight line. If significant heat capacity changes occur, a sigmoidal baseline can be drawn.

Note 3 to entry: Extrapolated and interpolated virtual baselines will not necessarily coincide with each other

(see Figure 2).
3.8
step
abrupt positive or negative change in the height of a
...

SLOVENSKI STANDARD
kSIST FprEN ISO 11357-1:2016
01-junij-2016
GHO6SORãQD3ROLPHUQLPDWHULDOL'LIHUHQþQDGLQDPLþQDNDORULPHWULMD '6& 
QDþHOD ,62)',6

Plastics - Differential scanning calorimetry (DSC) - Part 1: General principles (ISO/FDIS

11357-1:2016)
Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine
Grundlagen (ISO/FDIS 11357-1:2016)

Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 1: Principes généraux

(ISO/FDIS 11357-1:2016)
Ta slovenski standard je istoveten z: FprEN ISO 11357-1
ICS:
17.200.10 Toplota. Kalorimetrija Heat. Calorimetry
83.080.01 Polimerni materiali na Plastics in general
splošno
kSIST FprEN ISO 11357-1:2016 en,fr,de

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

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kSIST FprEN ISO 11357-1:2016
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kSIST FprEN ISO 11357-1:2016
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 11357-1
ISO/TC 61/SC 5
Plastics — Differential scanning
Secretariat: DIN
calorimetry (DSC) —
Voting begins on:
2016-05-12
Part 1:
Voting terminates on:
General principles
2016-08-04
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 1: Principes généraux
Please see the administrative notes on page ii
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 SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 11357-1:2016(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN-
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2016
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
ISO/CEN PARALLEL PROCESSING

This final draft has been developed within the International Organization for Standardization (ISO), and pro-

cessed under the ISO-lead mode of collaboration as defined in the Vienna Agreement. The final draft was

established on the basis of comments received during a parallel enquiry on the draft.

This final draft is hereby submitted to the ISO member bodies and to the CEN member bodies for a parallel

two-month approval vote in ISO and formal vote in CEN.
Positive votes shall not be accompanied by comments.
Negative votes shall be accompanied by the relevant technical reasons.
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland

All rights reserved. Unless otherwise specified, 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 below or ISO’s member body in the country of

the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction ................................................................................................................................................................................................................................vi

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

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

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

4 Basic principles ...................................................................................................................................................................................................... 8

4.1 General ........................................................................................................................................................................................................... 8

4.2 Heat-flux DSC ............................................................................................................................................................................................ 8

4.3 Power-compensation DSC ............................................................................................................................................................. 9

5 Apparatus and materials...........................................................................................................................................................................10

6 Specimen ....................................................................................................................................................................................................................11

7 Test conditions and specimen conditioning .........................................................................................................................12

7.1 Test conditions .....................................................................................................................................................................................12

7.2 Conditioning of specimens ........................................................................................................................................................12

8 Calibration ...............................................................................................................................................................................................................12

8.1 General ........................................................................................................................................................................................................12

8.2 Calibration materials ......................................................................................................................................................................13

8.3 Temperature calibration ..............................................................................................................................................................13

8.3.1 General...................................................................................................................................................................................13

8.3.2 Procedure ............................................................................................................................................................................13

8.3.3 Accuracy of calibration ............................................................................................................................................14

8.4 Heat calibration ...................................................................................................................................................................................14

8.4.1 General...................................................................................................................................................................................14

8.4.2 Procedure ............................................................................................................................................................................15

8.4.3 Accuracy of calibration ............................................................................................................................................15

8.5 Heat flow rate calibration ...........................................................................................................................................................16

8.5.1 General...................................................................................................................................................................................16

8.5.2 Procedure ............................................................................................................................................................................16

9 Procedure..................................................................................................................................................................................................................18

9.1 Setting up the apparatus..............................................................................................................................................................18

9.1.1 Switching on .....................................................................................................................................................................18

9.1.2 Purge gas .................. .................................................... ........................................................................................................18

9.1.3 Experimental conditions ........................................................................................................................................18

9.1.4 Baseline determination ...........................................................................................................................................18

9.2 Loading the specimen into the crucible .........................................................................................................................18

9.2.1 General...................................................................................................................................................................................18

9.2.2 Selection of crucibles ................................................................................................................................................19

9.2.3 Weighing the specimen crucible......................................................................................................................19

9.2.4 Loading the specimen ........................................................................................................................................... ....19

9.2.5 Determination of the mass of the specimen..........................................................................................19

9.3 Insertion of crucibles into the instrument ...................................................................................................................19

9.4 Performing measurements ........................................................................................................................................................19

9.4.1 General...................................................................................................................................................................................19

9.4.2 Scanning mode ...............................................................................................................................................................19

9.4.3 Isothermal mode ...........................................................................................................................................................20

9.5 Post-run checks ...................................................................................................................................................................................21

9.5.1 Check for loss in mass ..............................................................................................................................................21

9.5.2 Inspection of specimens .........................................................................................................................................21

9.5.3 Checking of crucibles and crucible holder ..............................................................................................21

10 Test report ................................................................................................................................................................................................................21

© ISO 2016 – All rights reserved iii
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
[12]

Annex A (normative) Extended, high-precision, temperature calibration .......................................................23

Annex B (normative) Extended, high-precision, heat calibration ......................................................................................25

Annex C (informative) Recommended calibration materials ..................................................................................................27

Annex D (informative) Interaction of calibration materials with different crucible materials ...........30

Annex E (informative) General recommendations .............................................................................................................................32

Bibliography .............................................................................................................................................................................................................................34

iv © ISO 2016 – All rights reserved
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(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 11357-1:2009), 3.7.2 of which has been

technically revised.

ISO 11357 Plastics — Differential scanning calorimetry (DSC) consists of the following parts.

— 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 crystallization kinetics
© ISO 2016 – All rights reserved v
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
Introduction

This International Standard describes thermoanalytical DSC test methods which can be used for

quality assurance purposes, for routine checks of raw materials and finished products or for the

determination of comparable data needed for data sheets or databases. The procedures given in this

International Standard apply as long as product standards or standards describing special atmospheres

for conditioning of specimens do not specify otherwise.
vi © ISO 2016 – All rights reserved
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kSIST FprEN ISO 11357-1:2016
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 11357-1:2016(E)
Plastics — Differential scanning calorimetry (DSC) —
Part 1:
General principles
1 Scope

SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory

practice, if applicable. This document does not purport to address all of the safety concerns, if

any, associated with its use. It is the responsibility of the user to establish appropriate safety

and health practices and to ensure compliance with any regulatory requirements.

This International Standard specifies several differential scanning calorimetry (DSC) methods for the

thermal analysis of polymers and polymer blends, such as

— thermoplastics (polymers, moulding compounds and other moulding materials, with or without

fillers, fibres or reinforcements),

— thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements), and

— elastomers (with or without fillers, fibres or reinforcements).

This International Standard is intended for the observation and measurement of various properties of,

and phenomena associated with, the above-mentioned materials, such as

— physical transitions (glass transition, phase transitions such as melting and crystallization,

polymorphic transitions, etc.),

— chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.),

— the stability to oxidation, and
— the heat capacity.

This part of ISO 11357 specifies a number of general aspects of differential scanning calorimetry, such

as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test

report common to all following parts.

Details on performing specific methods are given in subsequent parts of ISO 11357 (see Foreword).

2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. 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 80000-5, Quantities and units — Part 5: Thermodynamics
3 Terms a nd definiti ons

For the purposes of this document, the terms and definitions given in ISO 472 and ISO 80000-5 and the

following apply.
© ISO 2016 – All rights reserved 1
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
3.1
differential scanning calorimetry
DSC

technique in which the difference between the rate of flow of heat into a specimen crucible containing

the specimen and that into a reference crucible (3.3) is derived as a function of temperature and/or

time while the specimen and reference are subjected to the same controlled temperature programme

in a specified atmosphere using a symmetrical measurement system

Note 1 to entry: It is common practice to record, for each measurement run, a curve in which temperature or time

is plotted as the abscissa and heat flow rate (3.4) difference as the ordinate. The endothermic and/or exothermic

direction is indicated on the DSC curve.

Note 2 to entry: According to the principles of thermodynamics, energy absorbed by a system is considered

positive while energy released is negative. This approach implies that the endothermic direction points upwards

in the ordinate and the exothermic direction downwards (see Figures 1 and 2). It also has the advantage that the

direction of thermal effects in plots of heat flow rate (3.4) and specific heat is consistent.

3.2
calibration material

material for which one or more of the thermal properties are sufficiently homogeneous and

well established to be used for the calibration of a DSC instrument or for the assessment of a

measurement method
3.3
reference crucible
crucible used on the reference side of the symmetrical crucible holder assembly
Note 1 to entry: Normally, the reference crucible is empty.

Note 2 to entry: In special cases, such as the measurement of highly filled or reinforced polymers or specimens

having a heat capacity comparable to that of the crucible, a suitable material can be used inside the reference

crucible. This reference material should be thermally inactive over the temperature and time range of interest

and its heat capacity should be similar to that of the specimen. In the case of filled or reinforced products, the

pure filler or reinforcement can be used, for example.
3.4
he at f low r at e
quantity of heat transferred per unit time (dQ/dt)
Note 1 to entry: It is expressed in watts (W) or milliwatts (mW).

Note 2 to entry: The total quantity of heat transferred, Q, corresponds to the time integral of the heat flow rate:

Q =∫ dt
3.5
change in heat

quantity of heat absorbed (endothermic, ΔQ positive) or released (exothermic, ΔQ negative) within a

specified time, t, or temperature, T, range by a specimen undergoing a chemical or physical change

and/or a temperature change:
ΔQ = dt
60 dQ
ΔQ = dT
β dt
2 © ISO 2016 – All rights reserved
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
where

ΔQ is expressed in joules (J) or as a specific quantity, Δq, expressed in joules per amount of material

−1 −1
in grams (J⋅g ) or joules per amount of material in moles (J⋅mol );

β is the constant heating or cooling rate, dT/dt, expressed in kelvins per minute (K⋅min ).

Note 1 to entry: If measurements are made at constant pressure, ΔQ corresponds to the change in enthalpy, ΔH.

3.6
s p e c i f ic he at c ap ac it y at c on s t a nt pr e s s u r e

quantity of heat necessary to raise the temperature of unit mass of material by 1 K at constant pressure:

 
1dQ
c =×
 
m dT
 
 
160 dQ
c =× ×
 
m β dt
 
where

dQ is the quantity of heat, expressed in joules (J), necessary to raise the temperature of an amount

of material of mass m, expressed in grams (g), by dT kelvins at constant pressure;

β is the heating rate, expressed in kelvins per minute (K⋅min );
−1 −1
c is expressed in joules per gram per kelvin (J⋅g ⋅K ).
−1 −1

Note 1 to entry: c may also be expressed in joules per mole per kelvin (J⋅mol ⋅K ) when the amount of material,

m, is expressed in moles.

Note 2 to entry: When analysing polymers, ensure that the measured specific heat capacity does not include any

heat change due to a chemical reaction or a physical transition.
3.7
baseline
part of the recorded curve in which no reactions or transitions take place

Note 1 to entry: This can be an isothermal baseline when the temperature is maintained constant or a dynamic

baseline when the temperature is changed in accordance with a controlled temperature programme.

Note 2 to entry: The baselines defined in 3.7.1 to 3.7.3 refer to the quasi-stationary range only, i.e. when the

instrument is operating under stable conditions shortly after starting and shortly before ending the DSC run (see

Figure 1).
© ISO 2016 – All rights reserved 3
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
Key
dQ/dt heat flow rate 4 virtual baseline
T temperature 5 instrument baseline
t time 6 quasi-stationary range
1 dQ/dt vs t (or T) 7 isothermal start baseline
2 T vs t 8 isothermal end baseline
3 specimen baselines
Endothermic direction.
Figure 1 — Schematic drawing showing baselines
3.7.1
instrument baseline

curve obtained using only empty crucibles of identical mass and material in the specimen and reference

positions of the DSC cell

Note 1 to entry: The instrument baseline is required for heat capacity measurements.

3.7.2
specimen baseline

DSC curve obtained outside any reaction or transition zone(s) while the instrument is loaded with both

the specimen in the specimen crucible and the reference crucible (3.3)

Note 1 to entry: In this part of the curve, the difference in heat flow rate (3.4) between the specimen crucible

and the reference crucible (3.3) depends solely on the heat capacity of the specimen and the instrument baseline

(3.7.1).

Note 2 to entry: The specimen baseline reflects the temperature dependence of the heat capacity of the specimen.

Note 3 to entry: For heat capacity determinations, a dynamic DSC curve is required and, in addition, the

instrument baseline (3.7.1) and the isothermal start and end baselines (see Figure 1).

4 © ISO 2016 – All rights reserved
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
3.7.3
virtual baseline

imaginary line drawn through a reaction and/or transition zone assuming the heat of reaction and/or

transition to be zero

Note 1 to entry: Assuming the change in heat capacity with temperature to be linear, the virtual baseline is

drawn by interpolating or extrapolating the specimen baseline in a straight line. It is normally indicated on the

DSC curve for convenience (see Figures 1 and 2).

Note 2 to entry: The virtual baseline drawn from peak onset, T , to peak end, T , (the peak baseline) allows the

i f

determination of the peak area from which the heat of transition can be obtained. If there is no significant change

in heat capacity during the transition or reaction, the baseline can be drawn simply by connecting the peak onset

and peak end by a straight line. If significant heat capacity changes occur, a sigmoidal baseline can be drawn.

Note 3 to entry: Extrapolated and interpolated virtual baselines will not necessarily coincide with each other

(see Figure 2).
3.8
step

abrupt positive or negative change in the height of a DSC curve, taking place over a limited

temperature range

Note 1 to entry: A step in the DSC curve can be caused by, for example, a glass transition (see Figure 2).

3.8.1
step height

difference between the heights of the extrapolated baselines before and after a step, measured at the

time or temperature corresponding to the point on the DSC curve which is equidistant between the two

baselines
3.9
peak

part of the DSC curve which departs from the specimen baseline (3.7.2), reaches a maximum or

minimum, and subsequently returns to the specimen baseline (3.7.2)

Note 1 to entry: A peak in the DSC curve may indicate a chemical reaction or a first-order transition. The initial

departure of the peak from the virtual baseline (3.7.3) corresponds to the start of the reaction or transition.

3.9.1
endothermic peak

peak in which the rate of flow of heat into the specimen crucible is greater than that into the reference

crucible (3.3)
Note 1 to entry: This corresponds to a transition which absorbs heat.
3.9.2
exothermic peak

peak in which the rate of flow of heat into the specimen crucible is less than that into the reference

crucible (3.3)
Note 1 to entry: This corresponds to a transition which releases heat.
3.9.3
peak area
area enclosed by a peak and the interpolated virtual baseline (3.7.3)
© ISO 2016 – All rights reserved 5
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kSIST FprEN ISO 11357-1:2016
ISO/FDIS 11357-1:2016(E)
3.9.4
peak height

greatest distance in the ordinate direction between the interpolated virtual baseline (3.7.3) and the

DSC curve during a peak

Note 1 to entry: The peak height, which is expressed in watts (W) or watts per gram (W/g), is not necessarily

proportional to the mass of the specimen.
3.9.5
peak width
distance between the onset and end temperatures or times of a peak
3.10
characteristic temperatures, T, and times, t
values for temperature and time obtained from the DSC curve
Note 1 to entry: See Figure 2.

Note 2 to entry: For all types of DSC instrument, a distinction needs to be made between two different categories

of temperature:
— the temperature at the reference position;
— the temperature at the specimen position.

The reference position temperature is the one preferred for plotting thermograms. If the specimen position

temperature is used, then this information will need to be included in the test report.

Note 3 to entry: Characteristic temperatures are expressed in degrees Celsius (°C), relative temperatures and

tempera
...

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