ISO 29582-1:2009
(Main)Methods of testing cement — Determination of the heat of hydration — Part 1: Solution method
Methods of testing cement — Determination of the heat of hydration — Part 1: Solution method
ISO 29582-1:2009 describes a method of determining the heat of hydration of cements by means of solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram of cement. ISO 29582-1:2009 is applicable to cements and hydraulic binders whatever their chemical composition.
Méthodes d'essai des ciments — Détermination de la chaleur d'hydratation — Partie 1: Méthode par dissolution
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INTERNATIONAL ISO
STANDARD 29582-1
First edition
2009-07-15
Methods of testing cement —
Determination of the heat of hydration —
Part 1:
Solution method
Méthodes d'essai des ciments — Détermination de la chaleur
d'hydratation —
Partie 1: Méthode par dissolution
Reference number
ISO 29582-1:2009(E)
©
ISO 2009
---------------------- Page: 1 ----------------------
ISO 29582-1:2009(E)
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ii © ISO 2009 – All rights reserved
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ISO 29582-1:2009(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Principle. 1
4 Reagents and materials . 2
5 Apparatus . 2
6 Calorimeter calibration. 4
7 Determination of heat of solution . 6
8 Heat of hydration . 10
9 Test report . 10
Bibliography . 12
© ISO 2009 – All rights reserved iii
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ISO 29582-1:2009(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 29582-1 was prepared by Technical Committee ISO/TC 74, Cement and lime.
ISO 29582 consists of the following parts, under the general title Methods of testing cement — Determination
of the heat of hydration:
⎯ Part 1: Solution method
⎯ Part 2: Semi-adiabatic method
iv © ISO 2009 – All rights reserved
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INTERNATIONAL STANDARD ISO 29582-1:2009(E)
Methods of testing cement — Determination of the heat
of hydration —
Part 1:
Solution method
1 Scope
This part of ISO 29582 describes a method of determining the heat of hydration of cements by means of
solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram
of cement.
This part of ISO 29582 is applicable to cements and hydraulic binders, whatever their chemical composition.
NOTE 1 Another procedure, called the semi-adiabatic method, is described in ISO 29582-2. Either procedure can be
used independently.
NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 7 d for the solution
method in this part of ISO 29582 compared with 41 h for the semi-adiabatic method in ISO 29582-2.
2 Normative references
The following referenced documents are indispensable for the application 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.
EN 197-1, Cement — Part 1: Composition, specifications and conformity criteria for common cements
3 Principle
The method consists of measuring the heats of solution, in an acid mixture, of anhydrous cement and cement
hydrated under standardized conditions for a predetermined period of time, e.g. 7 days.
These standardized hydration conditions are as follows:
⎯ water/cement ratio of 0,40;
⎯ use of neat cement paste;
⎯ storage at a constant temperature of (20,0 ± 0,2) °C during the whole hydration process.
The heat of hydration for each period, H, is obtained from the difference between the heat of solution of
i
anhydrous cement, Q , and that of hydrated cement, Q .
a i
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ISO 29582-1:2009(E)
4 Reagents and materials
4.1 Acid mixture, analytical-reagent quality, obtained by adding 2,760 g of 40 % hydrofluoric acid (HF) per
100,0 g of (2,00 ± 0,01) mol/l nitric acid (HNO ), or 2,600 ml of hydrofluoric acid for every 100,0 ml of nitric
3
acid.
WARNING — Hydrofluoric acid can cause painful skin burns which heal only with difficulty and
precautions in handling this very corrosive substance should be strictly observed.
4.2 Acid mixture, proposed alternative, containing ammonium fluoride (NH F) instead of hydrofluoric acid,
4
prepared as follows.
Place about 400 g of (2,00 ± 0,01) mol/l nitric acid and 7,2 g of ammonium fluoride in the flask. Then, add
(2,00 ± 0,01) mol/l nitric acid to make a total mass of 425,0 g ± 0,1 g. Any other procedure in the preparation
of acid mixture can be adopted, provided that the same mass ratio of nitric acid to ammonium fluoride is
conserved.
The quantity (mass or volume) of acid used, which is common to all tests, shall be measured to ± 0,2 %.
In the case of a dispute , only the reference acid mixture containing hydrofluoric acid is used.
4.3 Zinc oxide (ZnO), analytical quality, used to determine the thermal capacity of the calorimeter and
prepare as follows.
Weigh 40 g to 50 g. Ignite at (950 ± 25) °C for 1 h. Cool in a desiccator. Grind to pass a 125 µm sieve. Store
in a desiccator.
4.4 Anhydrous cement, from which metallic iron has been removed with a magnet, stored in a sealed
container to avoid absorption of water or carbon dioxide.
Bring the test sample to ambient temperature and carefully homogenize it before use.
4.5 Hydrated cement, test sample prepared as follows.
Vigorously mix, either manually or mechanically, (100,0 ± 0,1) g of anhydrous cement with (40,0 ± 0,1) g of
distilled or deionized water for 3 min at ambient temperature. Place the resulting paste in plastic or glass
cylindrical vials (three for each hydration period being tested) so that each vial contains 15 g to 20 g of
material. Seal the vials by means of a stopper and, if necessary, with paraffin wax or similar material and store
them horizontally in a thermostatic bath maintained at a temperature of (20,0 ± 0,2) °C.
5 Apparatus
5.1 Calorimeter, comprised of the following (see Figure 1).
NOTE The method does not deal with the standardization of the calorimetric apparatus, or the measuring instruments.
Insulated flasks with a volume of about 650 ml have proved to be suitable.
5.1.1 Dissolution vessel, consisting of an insulated flask (e.g. Dewar flask), placed either in a heat
insulated container set inside a box constructed of insulating material (e.g. wood, plastics), or immersed in a
thermostatic water bath regulated to ± 0,2 °C; and an insulated stopper (made of cork or plastic) through
which holes are provided for the thermometer, the stirrer and the funnel used for introducing the sample.
The insulation of the calorimeter shall ensure that the thermal leakage coefficient, K, (determined in
accordance with 6.3) is less than 0,06 K per 15 min for each kelvin above ambient temperature. The internal
surface of the flask, that part of the thermometer immersed in the acid mixture and the lower part of the
stopper, shall be acid-mixture-resistant.
2 © ISO 2009 – All rights reserved
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ISO 29582-1:2009(E)
Key
1 stirrer motor 7 support
2 thermometer 8 flask support
3 ambient thermometer 9 box
4 flask 10 stirrer
5 insulating material 11 stopper
6 container 12 funnel
Figure 1 — Typical heat-of-solution calorimeter apparatus
5.1.2 Thermometer, either a Beckmann thermometer with a 5 °C to 6 °C scale and subdivisions every
0,01 °C, or other measurement apparatus of an equal or higher accuracy, such as a thermistor or platinum
resistance thermometer, positioned such that the end of the thermometer is at least 4 cm below the level of
the liquid surface.
Express temperature readings with a resolution of ± 0,002 °C. Adjust the zero of the Beckmann thermometer
so that the upper limit of the scale is approximately the ambient, or water bath, temperature. Calibrate the
thermometer in a thermostatic bath against a 0,01 °C graduated and calibrated thermometer.
© ISO 2009 – All rights reserved 3
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ISO 29582-1:2009(E)
5.1.3 Funnel, of acid-mixture-resistant plastics, through which the sample is introduced into the flask and
which extends below the lower part of the stopper by 5 mm to 6 mm and is sealed during the test.
5.1.4 Stirrer, of acid-mixture-resistant plastics, positioned such that the blades are as close as possible to
−1
the bottom of the flask and rotated by a motor at a speed of (450 ± 50) min . The motor shall have a low
power rating (e.g. a motor of a few watts) so as to prevent any excessive heat emission from affecting
measurements.
5.2 Thermostatic bath, e.g. water bath, for storing the hydrated samples at a temperature of
(20,0 ± 0,2) °C.
5.3 Mortar or electric grinder, for crushing the hydrated samples.
5.4 Plastic or glass vials, of capacity approximately 20 ml, for storing the hydrated paste.
5.5 Sieve, of mesh size 125 µm.
5.6 Sieve, of mesh size 600 µm.
5.7 Chronometer, graduated in seconds, for timing the temperature readings.
5.8 Two platinum crucibles, of capacity approximately 20 ml, for ignition of samples.
5.9 Electric furnace, naturally ventilated, capable of operating at (950 ± 25) °C, for ignition of samples.
5.10 Analytical balance, capable of weighing to an accuracy of ± 0,000 1 g.
5.11 Balance, of capacity 2 kg, capable of weighing to an accuracy of ± 0,2 g.
6 Calorimeter calibration
6.1 Principle
Calibration of the calorimeter is carried out in order to determine its thermal capacity and thermal leakage
coefficient. These characteristics are determined by dissolving the ignited zinc oxide (4.2) in the acid mixture
(4.1) and measuring the temperature of the calorimeter at fixed intervals of time. The temperature of the acid
mixture shall be so set that after the dissolution reaction, the calorimeter temperature is at least 0,5 °C below
the ambient temperature. Where a water bath is used, the temperature of the bath is considered to be the
ambient temperature for the calorimeter.
6.2 Procedure
Measure a quantity of acid mixture (4.1) by mass or volume to ± 0,2 % such that the liquid level is
approximately 2 cm below the calorimeter stopper. Place the acid mixture in the flask. Immediately before the
determination of the thermal capacity, ignite the zinc oxide at (950 ± 25) °C for a maximum of 5 min and cool
in a desiccator to room temperature. The mass of zinc oxide, m , being used, weighed to ± 0,000 1 g, is that
ZnO
required to satisfy Equation (1):
m
acid
=±60 1 (1)
m
ZnO
where m is the mass of the acid mixture (4.1).
acid
4 © ISO 2009 – All rights reserved
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ISO 29582-1:2009(E)
Carry out the procedure as follows.
a) Preliminary period: Stir the acid mixture for 40 min to 50 min.
b) Pre-period: When the rate of temperature increase is constant, start the timing using the
chronometer (5.7) and record the initial temperature.
c) Sample introduction: After 15 min, record the temperature, T , and immediately add
...
DRAFT INTERNATIONAL STANDARD ISO/DIS 29582-1
Attributed to ISO/TC 74 by the Central Secretariat (see page iii)
Voting begins on Voting terminates on
2007-03-05 2007-08-05
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION
FAST-TRACK PROCEDURE
Methods of testing cement — Determination of the heat of
hydration —
Part 1:
Solution method
Méthodes d'essai des ciments — Détermination de la chaleur d'hydratation —
Partie 1: Méthode par dissolution
ICS 91.100.10
THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS 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, TECHNOLOGICAL, COMMERCIAL AND 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 NATIONAL REGULATIONS.
©
International Organization for Standardization, 2007
---------------------- Page: 1 ----------------------
ISO/DIS 29582-1
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shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
Copyright notice
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under the applicable laws of the user's country, neither this ISO draft nor any extract from it may be
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ii © ISO 2007 — All rights reserved
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ISO/DIS 29582-1
NOTE FROM THE ISO CENTRAL SECRETARIAT
This draft International Standard is submitted for voting to ISO member bodies under the fast-track procedure.
ISO 29582-1 was prepared by CEN (as EN 196-8) and is submitted for approval under a special “fast-track
procedure”, by Technical Committee ISO/TC 74, Cement and lime, in parallel with its approval by the ISO
member bodies (see the ISO/IEC Directives, Part 1, 2004, Annex F, F.2.1.1).
F.2 “Fast-track procedure”
F.2.1 Proposals to apply the fast-track procedure may be made as follows.
F.2.1.1 Any P-member or category A liaison organization of a concerned technical committee may propose that
an existing standard from any source be submitted for vote as an enquiry draft. The proposer shall obtain the
agreement of the originating organization before making a proposal. The criteria for proposing an existing
standard for the fast-track procedure are a matter for each proposer to decide.
F.2.1.2 An international standardizing body recognized by the ISO or IEC council board may propose that a
standard developed by that body be submitted for vote as a final draft International Standard.
F.2.1.3 An organization having entered into a formal technical agreement with ISO or IEC may propose, in
agreement with the appropriate technical committee or subcommittee, that a draft standard developed by that
organization be submitted for vote as an enquiry draft within that technical committee or subcommittee.
F.2.2 The proposal shall be received by the Chief Executive Officer, who shall take the following actions:
a) settle the copyright and/or trademark situation with the organization having originated the proposed
document, so that it can be freely copied and distributed to national bodies without restriction;
b) for cases F.2.1.1 and F.2.1.3, assess in consultation with the relevant secretariats which technical
committee/subcommittee is competent for the subject covered by the proposed document; where no
technical committee exists competent to deal with the subject of the document in question, the Chief
Executive Officer shall refer the proposal to the technical management board, which may request the Chief
Executive Officer to submit the document to the enquiry stage and to establish an ad hoc group to deal with
matters subsequently arising;
c) ascertain that there is no evident contradiction with other International Standards;
d) distribute the proposed document as an enquiry draft (F.2.1.1 and F.2.1.3) in accordance with 2.6.1, or as a
final draft International Standard (case F.2.1.2) in accordance with 2.7.1, indicating (in cases F.2.1.1 and
F.2.1.3) the technical committee/subcommittee to the domain of which the proposed document belongs.
F.2.3 The period for voting and the conditions for approval shall be as specified in 2.6 for an enquiry draft and
2.7 for a final draft International Standard. In the case where no technical committee is involved, the condition for
approval of a final draft International Standard is that not more than one-quarter of the total number of votes cast
are negative.
F.2.4 If, for an enquiry draft, the conditions of approval are met, the draft standard shall progress to the
approval stage (2.7). If not, the proposal has failed and any further action shall be decided upon by the technical
committee/subcommittee to which the document was attributed in accordance with F.2.2 b).
If, for a final draft International Standard, the conditions of approval are met, the document shall progress to the
publication stage (2.8). If not, the proposal has failed and any further action shall be decided upon by the
technical committee/subcommittee to which the FDIS was attributed in accordance with F.2.2 b), or by
discussion between the originating organization and the office of the CEO if no technical committee was
involved.
If the standard is published, its maintenance shall be handled by the technical committee/subcommittee to which
the document was attributed in accordance with F.2.2 b), or, if no technical committee was involved, the
approval procedure set out above shall be repeated if the originating organization decides that changes to the
standard are required.
© ISO 2007 — All rights reserved iii
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EN 196-8:2003 (E)
ISO/DIS 29582-1
Contents
page
Foreword .3
1 Scope.4
2 Normative references.4
3 Principle .4
4 Materials.4
4.1 Acid mixture.4
4.2 Zinc oxide (ZnO).5
4.3 Anhydrous cement.5
4.4 Hydrated cement .5
5 Apparatus.5
5.1 Calorimeter .5
6 Calorimeter calibration .7
6.1 Principle .7
6.2 Procedure.7
6.3 Calculation of calibration characteristics.8
6.3.1 Corrected temperature increase, DT . .8
c
6.3.2 Thermal leakage coefficient, K .8
6.3.3 Thermal capacity, C .8
7 Determination of heat of solution.9
7.1 Heat of solution of anhydrous cement.9
7.1.1 Procedure.9
7.1.2 Calculation .10
7.1.3 Expression of results.11
7.2 Heat of solution of hydrated cement.11
7.2.1 Procedure.11
7.2.2 Correction for bound water.11
7.2.3 Calculation .12
7.2.4 Expression of results.13
8 Heat of hydration.13
8.1 Calculation of results.13
8.2 Reporting of results .13
8.3 Precision .13
8.3.1 Repeatability.13
8.3.2 Reproducibility .13
Bibliography .14
2 © ISO 2007 — All rights reserved
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EN 196-8:2003 (E)
ISO/DIS 29582-1
Foreword
This document (EN 196-8:2003) has been prepared by Technical Committee CEN/TC 51, ‘Cement
and building limes’, the secretariat of which is held by IBN.
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 2004, and conflicting national standards shall
be withdrawn at the latest by April 2004.
This European Standard on the methods of testing cement comprises the following Parts:
EN 196-1 Methods of testing cement — Part 1: Determination of strength
EN 196-2 Methods of testing cement — Part 2: Chemical analysis of cement
EN 196-3 Methods of testing cement — Part 3: Determination of setting time and soundness
EN 196-5 Methods of testing cement — Part 5: Pozzolanicity test for pozzolanic cements
EN 196-6 Methods of testing cement — Part 6: Determination of fineness
EN 196-7 Methods of testing cement — Part 7: Methods of taking and preparing samples of cement
EN 196-8: Methods of testing cement — Part 8: Heat of hydration - solution method
EN 196-9: Methods of testing cement — Part 9: Heat of hydration — semi-adiabatic method
EN 196-21: Methods of testing cement — Part 21: Determination of the chloride, carbon dioxide and
alkali content of cement
EN 196-21 is currently being revised and incorporated into EN 196-2.
Another document, ENV 196-4 Methods of testing cement — Part 4: Quantitative determination of
constituents, has been drafted and will be published as a CEN Technical Report.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg,
Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and the United
Kingdom.
© ISO 2007 — All rights reserved 3
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EN 196-8:2003 (E)
ISO/DIS 29582-1
1 Scope
This European Standard describes a method of determining the heat of hydration of cements by
means of solution calorimetry, also known as the solution method. The heat of hydration is expressed
in joules per gram of cement.
This standard is applicable to cements and hydraulic binders whatever their chemical composition.
NOTE 1 Another procedure, called the semi-adiabatic method, is described in EN 196-9. Either procedure can
be used independently.
NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 7 days for
the solution method (EN 196-8) compared with 41 h for the semi-adiabatic method (EN 196-9).
2 Normative references
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text, and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of any
of these publications apply to this European Standard only when incorporated in it by amendment or
revision. For undated references the latest edition of the publication referred to applies (including
amendments).
EN 197-1, Cement — Part 1: Composition, specifications and conformity criteria for common
cements.
3 Principle
The method consists in measuring the heats of solution, in an acid mixture, of anhydrous cement and
cement hydrated under standardized conditions for a predetermined period of time, e.g. 7 days.
These standardized hydration conditions are as follows:
water/cement ratio 0,40;
use of neat cement paste;
o
storage at constant temperature of (20,0 ± 0,2) C during the whole hydration process.
The heat of hydration for each period, H , is obtained from the difference between the heat of solution
i
of anhydrous cement, Q , and that of hydrated cement, Q .
a i
4 Materials
4.1 Acid mixture
Analytical reagent quality acid mixture, obtained by adding 2,760 g of 40 % hydrofluoric acid (HF) for
every 100,0 g of (2,00 ± 0,01) mol/l nitric acid (HNO ), or 2,600 ml of hydrofluoric acid for every
3
100,0 ml of nitric acid.
WARNING Hydrofluoric acid can cause painful skin burns which heal only with difficulty and
precautions in handling this very corrosive substance should be strictly observed.
4 © ISO 2007 — All rights reserved
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EN 196-8:2003 (E)
ISO/DIS 29582-1
The quantity (mass or volume) of acid to be used, which is common to all tests, shall be measured to
± 0,2 %.
4.2 Zinc oxide (ZnO)
Use zinc oxide of analytical quality to determine the thermal capacity of the calorimeter. Weigh 40 g to
o
50 g. Ignite at (950 ± 25) C for one hour. Cool in a desiccator. Grind to pass a 125 mm sieve. Store in
a desiccator.
4.3 Anhydrous cement
Store anhydrous cement, from which metallic iron has been removed with a magnet, in a sealed
container to avoid absorption of water or carbon dioxide. Bring the test sample to ambient
temperature and carefully homogenize it before use.
4.4 Hydrated cement
Prepare the hydrated cement test sample by vigorously mixing, either manually or mechanically,
(100,0 ± 0,1) g of anhydrous cement with (40,0 ± 0,1) g of distilled or deionised water for 3 min at
ambient temperature. Place the resulting paste in plastics or glass cylindrical vials (three for each
hydration period to be tested) so that each vial contains 15 g to 20 g of material. Seal the vials by
means of a stopper and, if necessary, with paraffin wax or similar material and store them horizontally
o
in a thermostatic bath maintained at a temperature of (20,0 ± 0,2) C.
5
Apparatus
5.1 Calorimeter
NOTE The method does not deal with the standardization of the calorimetric apparatus, or
...
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