ISO 24144:2023

Thermal insulation — Test methods for specific heat capacity of thermal insulation for buildings in the high temperature range — Differential scanning calorimetry (DSC) method

This document specifies test methods for specific heat capacity under high temperature conditions from the normal temperature range to 1 600 K for insulation materials for buildings using the differential scanning calorimetry (DSC) method.

Isolation thermique — Méthodes d'essai relatives à la capacité thermique massique de l'isolation thermique des bâtiments dans la plage de température élevée — Méthode par calorimétrie à balayage différentiel (DSC)

General Information

• Status: Published
• Publication Date: 09-Jan-2023
• ICS: 91.120.10 - Thermal insulation of buildings
• Technical Committee: ISO/TC 163/SC 1 - Test and measurement methods
• Drafting Committee: ISO/TC 163/SC 1/WG 21 - Test method for Specific heat capacity of thermal insulation for buildings at elevated temperature range
• Current Stage: 6060 - International Standard published
• Start Date: 10-Jan-2023
• Due Date: 12-Jun-2022
• Completion Date: 10-Jan-2023

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 24144
First edition
2023-01
Thermal insulation — Test methods
for specific heat capacity of thermal
insulation for buildings in the high
temperature range — Differential
scanning calorimetry (DSC) method
Isolation thermique — Méthodes d'essai relatives à la capacité
thermique massique de l'isolation thermique des bâtiments dans la
plage de température élevée — Méthode par calorimétrie à balayage
différentiel (DSC)
Reference number
ISO 24144:2023(E)
© ISO 2023

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ISO 24144:2023(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
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Published in Switzerland
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ISO 24144:2023(E)
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principles . 2
4.1 General . 2
4.2 Heat-flux DSC . 2
4.3 Power-compensation DSC . 3
5 Method . 4
5.1 General . 4
5.2 Basic procedure . 5
6 Apparatus and materials .7
6.1 DSC apparatus . 7
6.2 Crucibles . 8
6.2.1 General . 8
6.2.2 Shape, material and mass . 8
6.2.3 Measurement temperature range . 8
7 Test specimen . 8
7.1 General . 8
7.2 Sampling . 9
7.3 Moulding . 9
8 Test conditions and specimen conditioning . 9
8.1 Test conditions . 9
8.2 Conditioning of specimens . 9
9 Calibration .9
9.1 General . 9
9.2 Calibration materials . 10
10 Procedure .10
10.1 Setting up the apparatus . 10
10.2 Loading the specimen into the crucible . 10
10.2.1 General . 10
10.2.2 Selection of crucibles . 10
10.2.3 Weighing the specimen crucible. 10
10.2.4 Loading the specimen . 10
10.2.5 Determination of the mass of the specimen . 11
10.3 Performing measurements . 11
10.4 Post-run checks . 11
11 Determination of specific heat capacities .11
11.1 General . 11
11.2 Calculation of specific heat capacities . 11
11.2.1 In case of near-match with isothermal baselines of DSC curves . 11
11.2.2 In case of discordance with isothermal baseline of DSC curves .12
11.3 Numerical rounding of the results .12
12 Test report .12
Annex A (normative) DSC apparatus for high temperature range .14
Annex B (normative) Moulding procedure of test specimen .15
Annex C (informative) Analysis method considering discordance of isothermal baseline .18
Annex D (informative) Materials for DSC calibrations .20
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ISO 24144:2023(E)
Bibliography .21
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ISO 24144:2023(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
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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).
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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 163, Thermal performance and energy use
in the built environment, Subcommittee SC 1, Test and measurement methods.
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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INTERNATIONAL STANDARD ISO 24144:2023(E)
Thermal insulation — Test methods for specific heat
capacity of thermal insulation for buildings in the high
temperature range — Differential scanning calorimetry
(DSC) method
1 Scope
This document specifies test methods for specific heat capacity under high temperature conditions from
the normal temperature range to 1 600 K for insulation materials for buildings using the differential
scanning calorimetry (DSC) method.
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.
1)
ISO 11357-1:20—, Plastics — Differential scanning calorimetry (DSC) — Part 1: General principles
ISO 11357-4:2021, Plastics — Differential scanning calorimetry (DSC) — Part 4: Determination of specific
heat capacity
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 11357-1, ISO 11357-4 and the
following apply.
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
specific heat capacity
c
p
quantity of heat necessary to raise the temperature of a unit mass of material by 1 K at constant
pressure
Note 1 to entry: It is given by the following formula:
1dQ
 
c =× (1)
 
p
m dT 
p
where
−1 −1
c is the specific heat capacity and is expressed in kilojoules per kilogram per K (kJ⋅kg ⋅K )
p
−1 −1
or in joules per gram per K (J⋅g ⋅K ); subscript p indicates an isobaric process;
m is the mass of material, expressed in kilogram (kg) or gram (g);
1) Under preparation. Stage at time of publication: ISO/FDIS 11357-1.
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ISO 24144:2023(E)
dQ is the quantity of heat dQ necessary to raise the temperature of the material by dT, expressed
 
 
−1 −1
in kilojoules per K (kJ⋅K ) or in joules per K (J⋅K ), measured at constant pressure.
dT
 
p
3.2
specimen
item which is cut from thermal insulation material and processed into powder form or compression
moulded for measurement by differential scanning calorimetry (DSC)
Note 1 to entry: See Annex B for further information on moulding procedure.
3.3
reference material
material of known specific heat capacity (3.1)
Note 1 to entry: See ISO 11357-4:2021, Annex A for further information.
3.4
calibration material
material of known temperature and heat of fusion
Note 1 to entry: See Annex D for further information on calibration materials.
3.5
three-step temperature control method
method that consists of isothermal maintenance at the start temperature, constant heating step at the
middle temperature and isothermal maintenance at the end temperature
3.6
differential scanning calorimetry
DSC
method in which the difference in energy inputs into a substance and a reference material is measured
as a function of temperature while the substance and reference material are subjected to a controlled
temperature programme
[SOURCE: ISO/TS 80004-6:2021, 6.2.1]
4 Principles
4.1 General
DSC is a method in which the difference in energy inputs into a substance and a reference material is
measured as a function of temperature while the substance and reference material are subjected to a
controlled temperature programme.
The difference between the rate of heat flow into a specimen and the rate of heat flow into a reference
crucible is measured as a function of either temperature or time, or both, while the specimen and the
reference are subjected to the same temperature-control programme under a specified atmosphere.
The measurements can be undertaken using two types of DSC: heat-flux DSC and power-compensation
DSC.
4.2 Heat-flux DSC
The specimen and reference positions are subjected to the same temperature-control programme by a
single heater. A difference in temperature, ΔT, occurs between the specimen position and the reference
position because of the difference in heat capacity between the specimen and the reference. From
this temperature difference, the difference in the rates of heat flow into the specimen and reference
positions is derived and is normally recorded against the temperature of the reference, T , or against
ref
time.
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ISO 24144:2023(E)
A schematic drawing of a heat-flux DSC instrument is shown in Figure 1.
Key
1 sample holder 6 heating furnace
2 reference holder T temperature at sample holder (T )
1 specimen
3 crucible T temperature at reference holder (T )
2 ref
4 stage ΔT temperature difference between sample and reference holder
5 thermopile
Figure 1 — Schematic diagram illustrating the basic principles of heat-flux DSC
4.3 Power-compensation DSC
In power-compensated DSC, individual heaters are used for the specimen and reference positions.
The difference in electrical power required to maintain both the specimen position and the reference
position at the same temperature is recorded against temperature or time, while each position is
subjected to the same temperature-control programme.
For power-compensated isoperibolic calorimeters, the surrounding temperature (i.e. the temperature
of the heat sink) shall be kept constant.
A schematic drawing of a power-compensation DSC instrument is shown in Figure 2.
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ISO 24144:2023(E)
Key
1 specimen position 6 heat-flux compensation circuit
2 reference position 7 surrounding heat sink
3 thermometers T temperature at specimen position (T )
1 specimen
4 individual heaters T temperature at reference position (T )
2 ref
5 measurement circuit for T and
specimen
T
ref
Figure 2 — Schematic diagram illustrating the basic principles of power-compensation DSC
5 Method
5.1 General
This document specifies methods for the measurement of specific heat capacity according to the heat-
flux DSC method and the power-compensation DSC method, based on the three-step temperature
control method.
The apparatus for both methods comprises two measuring cells (sample holders) housed in a furnace
which provides overall system heating. One cell contains the test specimen within a crucible, and the
other contains an empty crucible only.
a) Power-compensation DSC method
Each cell has an individual heater to compensate for temperature variations from the overall heating
programme. The power which is supplied to either cell heater to maintain equal temperatures
during heating is measured.
b) Heat-flux DSC method
Power is exchanged between each cell and its respective surrounding during the heating
programme. The difference in power exchange between the two cells is measured.
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