EN ISO 11357-1:1997

SLOVENSKI STANDARD
SIST EN ISO 11357-1:1999
01-maj-1999
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Plastics - Differential scanning calorimetry (DSC) - Part 1: General principles (ISO 11357
-1:1997)
Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine
Grundlagen (ISO 11357-1:1997)
Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 1: Principes généraux
(ISO 11357-1:1997)
Ta slovenski standard je istoveten z: EN ISO 11357-1:1997
ICS:
17.200.10 Toplota. Kalorimetrija Heat. Calorimetry
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 11357-1:1999 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
ISO
INTERNATIONAL
113574
STANDARD
First editisn
1997-04-15
Plastics - Differential scanning
calorimetry (DSC) -
Part 1:
General principles
- Analyse calorimetrique diff&entielle (DSC) -
Plastiques
Partie 1: Principes gh&aux
Reference number
ISO 11357-1:1997(E)

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
ISO 11357-1: 1997(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. Esch 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.
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 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 PIastics -
Differential scanning calorimetry (DSC):
- Par? 1: General principles
Part 2: Determination of glass transition tempera ture
- Parf 3: Determination of temperature and enthalpy of melting and
crys ta Iliza tion
Part 4: Determination of specific heat capacity
- Part 5: Determination of polymerization tempera tures and/or times
and polymeriza tion kinetics
Part 6: Determination of Oxidation induction time
- Part 7: Determination of crystallization kinetics
Annexes A, B and C of this part of ISO 11357 are for information only.
0 ISO 1997
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopying and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case postale 56 l CH-121 1 Geneve 20 l Switzerland
Internet central@ iso.ch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
ISO 113574 : 1997(E)
INTERNATIONAL STANDARD @ ISO
- Differential scanning calorimetry (DSC) -
Plastics
Part 1:
General principles
WARNING - The use of this International Standard may involve hazardous materials, operations and
equipment. This Standard does not Purpott to address all of the safety Problems associated with its use. lt
is the responsibility of the user of this Standard to establish appropriate health and safety practices and to
determine the applicability of regulatory limitations Prior to use.
1 Scope
This International Standard specifies a method for the thermal analysis of polymers such as thermoplastics and
including moulding materials and composite materials, using differential scanning
thermosetting plastics,
calorimetry (DSC).
Various determinations tan be made on polymers by using differential scanning calorimetry. These determinations
are dealt with in park 2 to 7 of this Standard (see the foreword).
2 Normative reference
The following Standard contains provisions which, through reference in this text, constitute provisions of this part of
ISO 11357. At the time of publication, the edition indicated was valid. All Standards are subject to revision, and
Parties to agreements based on this part of ISO 11357 are encouraged to investigate the possibility of applying the
most recent edition of the Standard indicated below. Members of IEC and ISO maintain registers of currently valid
International Standards.
ISO 291 :-V, Plastics - Standard atmospheres for conditioning and testing.
3 Definitions
For the purposes of this International Standard, the following definitions apply:
3.1 differential scanning calorimetry (DSC): A technique in which the differente between the heat flux (power)
into a test specimen and that into a reference specimen is measured as a function of temperature and/or time while
the test specimen and the reference specimen are subjected to a controlled temperature Programme.
lt is common practice to record, for each measurement, a curve in which temperature or time is plotted on the x-axis
and heat flux differente is plotted on the y-axis.
1) To be published. (Revision of ISO 291:1977)

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
@ ISO
ISO 113574 : 1997(E)
.
3.2 reference . A known specimen which is usually thermally inactive over the temperature and time
range of interes
NOTE - Generally an empty pan identical to the one containing the test specimen is used as the reference specimen.
3.3 Standard reference material: A material for which one or more of the thermal properties are sufficiently
homogeneous and well established to be used for the calibration of DSC apparatus, for the assessment of a
measurement method or for assigning values to materials.
3.4 heat flux; thermal power: The amount of heat transferred per unit time (dQ/dt).
NOTE - The total quantity of heat transferred Q corresponds to the time integral of the heat flux
dQ
dt
dt
where Q is expressed in joules or in joules per unit mass (J-kg-1 or J-g-1).
3.5 Change in enthalpy, AH: The quantity of heat absorbed (AH positive) or released (AI!! negative) by a test
specimen undergoing a Chemical or physical Change, and/or a temperature Change, at constant pressure. M is
expressed in joules or in joules per unit mass (J-kg-1 or J-g-1):
AH =
r,
3.6 specific heat capacity at constant pressure, cp: The quantity of heat necessary to raise the temperature of
unit mass of material by 1 “C at constant pressure, with all other intensive Parameters constant:
1
JQ
=-
cp mx aT
( 1
P
where
dQ is the quantity of heat, expressed in joules, necessary to raise the temperature of material of mass m by aT
degrees Celsius at constant pressure;
cp is expressed in joules per kilogram degree Celsius [J/(kg.OC)] or joules per gram degree Celsius [J/(g.“C)].
When analysing polymers, care must be taken to 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: The part of the recorded curve outside, but adjacent to, the reaction or transition Zone. In this part of
the recorded curve, the heat flux differente is approximately constant.
3.8 virtual baseline: An imaginary line drawn through a reaction and/or transition Zone assuming that the heat of
reaction and/or transition is Zero. lt is commonly drawn by interpolating or extrapolating the recorded baseline. lt is
normally indicated on the DSC curve for convenience (see figure 1).
3.9 peak: The part of the DSC curve which departs from the baseline, reaches a maximum, and subsequently
returns to the baseline.
The Start of the peak corresponds to the Start of the reaction or transition.
NOTE -
3.9.1 endothermic peak: A peak in which the energy supplied to the test specimen is greater than the energy
corresponding to the virtual baseline.
3.9.2 exothermit peak: A peak in which the energy supplied to the test specimen is less than the energy
corresponding to the virtual baseline.

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
@ ISO ISO113574:1997(E)
In accordance with the accepted conventions of thermodynamics, the enthalpy Change is negative when the
NOTE -
reaction or transition is exothermit and positive when the reaction or transition is endothermic. The direction corresponding to
exothermit or endothermic is normally indicated on the DSC curve.
3.9.3 peak height: The distance between the virtual baseline and the Point of maximum height of a peak. The
height is expressed in milliwatts. The height is not proportional to the mass of the test specimen.
3.10 characteristic temperatures: The following are the characteristic temperature on a DSC curve:
- onset temperature
Ti
- extrapolated onset temperature Tei
- peak temperature
TP
- extrapolated end temperature
Te f
- end temperature
Tf
T
PC
Vi
c
.-
=”
.-
PE
fuL
LaJ
r!z=
eo
mt
kW
D
2
w
m = melting
g = glass transition
c = crystallization
/
T
Pm
Temperature, “C
Figure 1 - Typical DSC curve
4 Principle
The differente between the heat flux into a test specimen and that into a reference specimen is measured as a
function of temperature and/or time, while the test specimen and the reference specimen are subjected to a
controlled temperature Programme under a specified atmosphere.
Two types of DSC, power-compensation DSC and heat-flux DSC, may be carried out. They are distinguished by the
NOTE -
design of instrumentation used for measurement, as follows:
a) Power-compensation DSC: The differente between the heat flux into the test specimen and that into the reference
specimen is measured as a function of temperature or time while varying the temperature of the specimens in accordance
with a controlled Programme, keeping the temperature of both specimens equal.
b) Heat-flux DSC: The differente in heat flux derived from the temperature differente between a test specimen and a
reference specimen is measured as a function of temperature or time while varying the temperature of the specimens in
accordance with a controlled Programme. In this type of measurement, the differente in temperature between the Pest
specimen and reference specimen is proportional to the differente in heat flux.

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
ISO 11357-1: 1997(E)
5 Apparatus and materials
5.1 Differential scanning calorimeter, the main features of which are as follows:
the capability to generate constant heating and cooling rates between 0,5 “C/min and 20 “Umin;
a)
the capability to maintain the test temperature constant to within & 0,5 “C for at least 60 min;
W
the capability to carry out step heating or any other heating mode;
Cl
a gas-flow rate in the range IO mI/min to 50 mI/min, controllable to + 10 %;
d)
temperature Signals with 0,l “C resolution and noise below 0,5 “C;
e>
facilities for calibration and use with a minimum test specimen mass of 1 mg (or with smaller quantities if
f )
required by specific applications);
a recording device which is capable of automatically recording the DSC curve, and of integrating the area
9)
between the curve and the virtual baseline with an error of less than 2 %;
a specimen holder assembly which has one or more holders for Pans.
h)
5.2 Pans, for test specimens and reference specimens, all made of the same material and of equal mass. The
pans shall be physically and chemically inert under the measurement conditions to both the test specimen and the
atmosphere.
The pans should preferably be made of a material with a high thermal conductivity. They shall be able to be fitted
with lids and sealed so that they tan withstand the overpressure which tan arise during measurement.
53 . Balance, capable of measuring the specimen mass with an accuracy of + 0,Ol mg.
54 . Standard reference materials (see annex A).
55 .
Gas supply, analytical grade.
6 Test specimen
The test specimen may be in the liquid or solid state. If in the solid state, it may be in the form of a powder, pellets or
granules, or may be tut from Sample pieces. The test specimen shall be representative of the Sample being
examined and shall be prepared and handled with care. If the specimen is taken from Sample pieces by cutting,
care shall be taken to prevent heating, polymer reorientation or any other effect that may alter the properties.
Operations such as grinding that could Cause heating or reorientation and could therefore Change the thermal
history of the Sample shall be avoided. When aggregates or powders are involved, two or more specimens shall be
taken. The method of sampling and test specimen preparation shall be stated in the test report.
NOTE - Incorrect specimen preparation tan affect the properties of the polymers examined. For further information, see
annex B.
7 Test conditions and specimen conditioning
7.1 Test conditions
Prior to any testing, switc :h the equipment on for at least 0 ne hour to allow the electronics to temperature-equilibrate.
Maintain and operate the instrument in an atmosphere as specified in ISO 291.
NOTE - It is advisable to protect the instrument from air draughts, exposure to direct sunlight and/or sharp changes in
temperature, pressure or electric supply during measurements.

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SIST EN ISO 11357-1:1999SIST EN ISO 11357-1:1999
@ ISO ISO 11357-1: 1997(E)
7.2 Conditioning of test specimens
Condition test specimens before meas urements as specified in the relevant material Standard or by a method
agreed between the interested Parties.
NOTES
Unless other conditions are specified, it is recommended that test specimens are conditioned in accordance with ISO 291.
affected by conditioning.
2 Results obtained by DSC tan be greatly
8 Calibration
8.1 General
Calibrate the energy and temperature measurement devices of the calorimeter at least in accordance with the
instrument manufacturer’s recommendations.
NOTES
1 The calibration function K(7) (see 8.3) cannot be expressed as a simple proportionality factor since it varies with
temperature. lt is essential therefore to carry out calibration with at least two Standard reference materials for each Parameter,
i.e. temperature and energy. Most recommended Standard reference materials, as given in annex A, tan be used for both
temperature and energy calibrations.
2 Calibration is affected by:
- the type of calorimeter used;
- the gas used and its flow rate;
- the type of specimen pan used, its dimensions and its Position in the specimen holder;
- the mass of the test specimen;
- the heating and cooling rates;
- the type of cooling System used.
lt is therefore advisable to define the conditions of the actual determination as precisely as possible and carry out the
calibration using the same conditions. Computer Systems associated with DSC instruments may automatically correct some of
the Parameters.
3 lt is advisable to carry out calibrations regularly. lt is considered good practice to check the temperature and energy
measurement de
...