SIST EN ISO 11357-1:2023

SLOVENSKI STANDARD
oSIST prEN ISO 11357-1:2022
01-april-2022
Polimerni materiali - Diferenčna dinamična kalorimetrija (DSC) - 1. del: Splošna
načela (ISO/DIS 11357-1:2022)
Plastics - Differential scanning calorimetry (DSC) - Part 1: General principles (ISO/DIS
11357-1:2022)
Kunststoffe – Dynamische Differenzkalorimetrie (DSC) – Teil1: Allgemeine Grundlagen
(ISO/DIS 11357-1:2022)
Plastiques - Analyse calorimétrique différentielle (DSC) - Partie 1: Principes généraux
(ISO/DIS 11357-1:2022)
Ta slovenski standard je istoveten z: prEN ISO 11357-1
ICS:
17.200.10 Toplota. Kalorimetrija Heat. Calorimetry
83.080.01 Polimerni materiali na Plastics in general
splošno
oSIST prEN ISO 11357-1:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN ISO 11357-1:2022

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oSIST prEN ISO 11357-1:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 11357-1
ISO/TC 61/SC 5 Secretariat: DIN
Voting begins on: Voting terminates on:
2022-01-25 2022-04-19
Plastics — Differential scanning calorimetry (DSC) —
Part 1:
General principles
Plastiques — Analyse calorimétrique différentielle (DSC) —
Partie 1: Principes généraux
ICS: 83.080.01
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
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USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 11357-1:2022(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 2022

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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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 . 14
8.5.1 General . 14
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 . 17
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
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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 .30
Annex E (informative) General recommendations .32
Bibliography .34
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This fourth edition cancels and replaces the third edition (ISO 11357-1:2016), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— the examples of materials given for temperature and enthalpy calibration has been updated;
— the data of sapphire to be used for calibration of heat flow rate have been updated.
A list of all parts in the ISO 11357 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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.
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oSIST prEN ISO 11357-1:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 11357-1:2022(E)
Plastics — Differential scanning calorimetry (DSC) —
Part 1:
General principles
1 Scope
The ISO 11357 series 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).
The ISO 11357 series is applicable 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 document 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 the ISO 11357 series (see
Foreword).
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.
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 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.
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(E)
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
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:
dQ
Q =∫ dt
dt
3.5
change in heat
ΔQ
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:
t
2 dQ
ΔQ= dt
∫
t
dt
1
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(E)
or
T
60 2 dQ
ΔQ= dT
∫
T
β dt
1
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 );
−1
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
c
p
quantity of heat necessary to raise the temperature of unit mass of material by 1 K at constant pressure:
1dQ
 
c =×
p  
m dT 
p
or
160 dQ
 
c =× ×
 
p
m β  dt 
p
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;
−1
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 ).
p
−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,
p
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).
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(E)
Key
dQ/dt heat flow rate 2 virtual baseline
T temperature 3 instrument baseline
t time 4 quasi-stationary range
dQ/dt vs. t 5 isothermal start baseline
T vs. t 6 isothermal end baseline
a
1 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).
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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)
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oSIST prEN ISO 11357-1:2022
ISO/DIS 11357-1:2022(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
temperature differences in kelvins (K) and characteristic times in seconds (s) or minutes (min) (see Figure 2).
Note 4 to entry: The DSC curve can also be plotted using time, t, as the abscissa instead of temperature, T.
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