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
General Information
Standards Content (Sample)
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 2009
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© ISO 2009
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ii © ISO 2009 – All rights reserved
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
Foreword
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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
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
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
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,
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
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.
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
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 the zinc oxide
sample to the acid mixture, taking not more than 1 min.
d) Dissolution period: Stir the mixture for 30 min, after which the dissolution is considered as being
complete, and then record the temperature, T . Record the ambient
temperature, T . If th
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