Adiabatic and Semi-Adiabatic Calorimetry To
Adiabatic and Semi-Adiabatic Calorimetry To
Adiabatic and Semi-Adiabatic Calorimetry To
Recommendations
The texts presented hereunder are drafts for general consideration. Comments should be sent to the TC Chairman, Professor
R. Springenschmid, Institute for Construction Materials, Technical University of Munich, Baumbachstr. 7,
D-81245 Munich, Germany, before 1st February 1998.
TC Membership: Chairman: R. Springenschmid, Germany; Secretary: M. Plannerer, Germany; Editorial Secretary: J.-L. Bostvironnois,
Germany; Members: P. Acker, France; S. Bernander, Sweden; R. Breitenbücher, Germany; K. van Breugel, Netherland; M.J. Coole, Great
Britain; M. Emborg, Sweden; H. Grube, Germany; H. Hamfler, Germany; M.J. Hammons, USA; H. Huber, Austria; C. Jaegermann, Israel;
F. Jung, Austria; M. Mangold, Germany; P. Morabito, Italy; P.K. Mukherjee, Canada; F.S. Rostásy, Germany; A.R. Solovjantchik, Russia;
T. Tanabe, Japan; P.J. Wainwright, Great Britain.
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TC 119-TCE
will have the same cylindrical shape as the sample and be The dimensions of the sample and the method of
made of steel or aluminium (the latter is to be preferred measuring the temperature are the same as for an adia-
because of its lower unit weight). Inside the jacket, water batic calorimeter. The ambient temperature where the
is circulated, the temperature of which is controlled by an vessel is placed is fixed at 20°C ± 1°C. The coefficient of
auxiliary thermal conditioning unit whose working tem- total heat loss shall not exceed 100 J/h/K. The vessel
perature should range from 5°C up to 80°C in order to be should be placed away from any heat sources and strong
able to simulate the hydration of concrete with the same air currents. The speed of the ventilation air around the
initial temperature as on site. Some form of insulation, calorimeter should be less than 0.5 m/s. When several
such as a flexible foamed polyurethane sheet 3 cm thick, tests are being carried out simultaneously, the minimum
should be provided between the sample and the thermal distance between vessels should be over 10 cm.
jacket; this improves the equalisation of the temperature
around the sample, will minimise the accidental risk of
supplying heat directly to the sample and will make the 5. CALIBRATION
degree of sensitivity of the temperature controller less crit-
ical. A second layer of thermal insulation inserted between The calculation of the adiabatic temperature increase
the jacket and the external shell will minimise any effects from the measured curves is given in Appendix 2 and
that the environmental temperature might have on the requires the knowledge of Cs, α, t and Ccal; the last three
test. The temperature of the jacket shall be regulated by a coeff icients depend on the characteristics of the
controller whose sensitivity inf luences the amount by calorimeter and therefore must be determined through a
which the temperature of the jacket cycles around the set calibration.
point, and consequently will affect the amount of heat The calibration sample shall be of distilled water (spe-
that is lost or gained. Since the temperature of the jacket cific heat equal to 4,186 J/kg/K in the range from 0°C to
must never be allowed to exceed the temperature of the 100°C) which is to be subjected to the following steps:
sample under test, the temperature of the jacket is set – heating of the sample
slightly lower than the sample temperature and the differ- – spontaneous cooling of the sample.
ence between the two is carefully controlled. A small
amount of heat loss is thus unavoidable.
The temperature difference must be such that the 5.1 Adiabatic calorimeter
temperature loss of the sample is less than 0.02 K/h and
to achieve this, temperature sensors having a sensitivity First, the total thermal capacity CT of the calorimeter
of ± 0.01 K should be used (PT100 or thermistors). containing the calibration sample is determined; then
that of the calorimeter alone is deduced.
The sample container is filled with distilled water and
left for a period of about 10 hours to stabilise the system.
After this time, the sample is heated at constant power
P [W] under adiabatic conditions for a time t- of about
20 h. The level of power should be such as to give a rise in
temperature θs equal to 30-40°C, the rate of temperature
increase should be maintained constant (α = const.). After
this time, the power is switched off and the sample is kept
under adiabatic conditions for 10 h to stabilise the system.
The power supplied is expressed as:
( )
Ts − Ta
( )
P ⋅ t = C T ϑ s + a ⋅ t = C T ϑ s +
τ
⋅ t
In order to determine τ, the temperature of the ther-
mal jacket is lowered to a temperature Tjo of about 10-
20°C; the sample will then cool spontaneously according
to the following expression:
Fig. 2 – Example of a semi-adiabatic calorimeter using a commer-
cial thermos vessel.
−
[
d Tjo − Ts t( )] = dt
Tjo − T (t)
s
τ
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Materials and Structures/Matériaux et Constructions, Vol. 30, October 1997
where: t = elapsed time mined according to the same procedures used to deter-
Tso = temperature of the sample at starting time mine CT, with the difference that the calibration sample
of cooling is replaced by a concrete sample which has been allowed
Tst = temperature of the sample at point in time t to completely hydrate; so:
ln = natural logarithm.
Cs = CT – Ccal
If the temperature controller does not allow a steep
descent of the temperature of the jacket to be achieved,
an alternative way is to remove the sample from the 6.2 Calculated evaluation
calorimeter and keep it at about 50°C in an oven, reduce
the temperature of the jacket to Tjo and, when this tem- The heat capacity of concrete is temperature-dependent
perature is reached, replace the sample in the calorime- and also depends on the hydration rate during the adiabatic
ter. The cooling period should run for about 30 h. or semi-adiabatic tests. Consequently, the experimental val-
The apparent heat capacity is given by: ues are not better than the calculated values obtained from a
knowledge of the composition of concrete and the specific
Ccal = CT - 4186 ⋅ mw [J / K] heat of the components.
mw being the mass in kg of the water sample. Calculation of the heat capacity of the sample is per-
formed according to the following formula:
Cs = ms gi⋅ci
5.2 Semi-adiabatic calorimeter
with: ms = mass of the concrete sample in kg
The coefficient α is determined by measuring in steady gi = content by mass of mix components
state conditions the equilibrium temperature Ts for differ- ci = specific heat of mix components:
ent levels of constant electrical power P provided to the aggregate: ca = 0.7-0.9 kJ/kg/K
calibration sample. When stable conditions are achieved, cement: cce = 0.84 kJ/kg/K
the heat supplied is completely dissipated into the environ- water: cw = 4.186 kJ/kg/K
ment. The equation for the losses is expressed as:
P = α ⋅ ϑs
7. TESTING PROCEDURE
α should be independent of the temperature; however,
this should be checked at 5 points in the temperature The testing procedure is performed through the fol-
range observed during the hydration tests (for example, lowing two steps:
for temperature increases of 10, 17, 24, 31, 38 K) and a – hydration of the concrete sample;
mean constant value will be assumed. – calculation of τ.
The measurement of the thermal capacity Ccal is car- The volume of the batch should be more than the
ried out by the method of spontaneous cooling of the volume of the sample to be tested and all the con-
water sample. For this purpose, the sample is discon- stituents will be kept at the constant starting temperature
nected from the electrical power supply after reaching for one day prior to mixing. The temperature of the
the steady state condition for the last point of calibration fresh concrete should differ not more than ± 2 K from
to determine α. During cooling, the heat exchange the temperature of the calorimeter. The concrete is
equation is expressed as: placed inside the container, vibrated and weighed. The
measurement of the temperature increase starts no later
–CT ⋅dϑ = α ⋅ϑ⋅dt
than 10-15 minutes from the start of the mixing. The
whence: measuring period is usually over seven days and calcula-
tion of τ is carried out for each concrete sample tested by
CT = α ⋅ t spontaneous cooling at the end of the hydration period.
ϑ
ln o Finally, data reduction is performed according to the
ϑt
procedure given in Appendix 2.
with: t = elapsed time since disconnecting the power
supply
θo = temperature increase at starting time 7.1 Adiabatic test
θt = temperature increase at point in time t.
The difference Ts - Tj is set to a value such that the
coefficient of the temperature loss is less than 0.02 K/h.
6. EVALUATION OF THE HEAT CAPACITY The temperature of the thermal jacket is regulated con-
OF CONCRETE tinuously or at a rate of no more than every 30 s. Over
the whole period of hydration, data recording of Ts and
6.1 Experimental evaluation Tj is performed; the experimental evaluation of τ is car-
ried out as described in 5.1.
After the heat capacity of the calorimeter is known,
the heat capacity of the concrete specimen can be deter-
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TC 119-TCE
7.2 Semi-adiabatic test For each test the following data will be documented:
– concrete composition
The temperature of the thermos vessel is adjusted to – initial temperature of the mix
the ambient temperature. The temperature of the fresh – initial weight of the sample
concrete should be equal to the ambient temperature – duration of the measuring period
within ± 2 °C. After the measuring period, the specimen – time, temperature of the sample, ambient temperature
is removed from the vessel and stored to let hydration (for semi-adiabatic test), jacket temperature (for adiabatic
cease. Then the specimen in the closed container is test) at steps not greater than 0.5 h: these data can be tab-
heated up in an oven to about 50°C and inserted in the ulated or plotted
thermos vessel. By means of the measured temperature – final weight of the sample
loss the time constant τ is determined. – heat capacity of the sample (specify if calculated or
Because of the semi-adiabatic conditions, data reduc- measured)
tion leads to a temperature increase θHH which is a lower – time constant τ
estimate of the adiabatic temperature increase; an exam- – total heat quantity liberated by the unit weight of concrete.
ple of stepwise calculation is given in Appendix 3.
The estimate can be improved by considering the
influence of the temperature on the hydration by means 9. SOME REMARKS ON THE CHOICE OF
of a maturity function. In general, the temperature factor ADIABATIC OR SEMI-ADIABATIC TEST
kT of Arrhenius gives a good approximation for the tem-
perature dependence of the hydration of cement: Although both types of testing method make it possible
EA 1
to determine the adiabatic temperature increase of a given
− 1
kT = e R 293 273 + T concrete sample, semi-adiabatic tests are generally easier to
conduct. On the other hand, hydration curves from adia-
with:T temperature in °C batic calorimeters are determined quite accurately.
EA activation energy in J/mol The choice of the test type will depend on the degree
R universal gas constant = 8.314 J/(mol·K) of accuracy with which the laboratory test should simu-
late the hydration in the real structure. For thermal
E A 4000 for T ≥ 20°C for Portland
= analysis of mass concrete structures where the tempera-
R 4000 + 175 20 − T ( ) for T < 20°C cements ture increase is expected to be almost adiabatic, or when
the true adiabatic temperature increase and heat of
EA
= 6000 for slag cements hydration are required, the use of an adiabatic calorime-
R ter is recommended.
The assumed maturity function is: In structures of smaller size where heat losses are
t expected, greater precision in the prediction of the tem-
∫
M = k T dt perature increase can only be achieved from a knowledge
0 or estimate of the expected temperature loss. This of
The correction is done stepwise according to the fol- course is an extremely difficult figure to calculate, but
lowing equations: assuming it to be possible, then either the calorimeter
could be designed to reproduce this loss or adjustments
ϑad(t) = ϑHH(M)
could be made to the measured curve. In both cases, a
M
semi-adiabatic test may be more favourable: the semi-
∫k
with time t = 1 dM
adiabatic hydration curve could be in relatively close
T
0 agreement already with the hydration process as it actu-
and Ts = To + ϑHH(M) = To + ϑad(t), To being the initial ally develops in the structure; inaccuracy of any adjust-
temperature of the specimen. An example for the calcu- ment that allows for minor deviations of the actual tem-
lation scheme is given in Appendix 4. perature in the structure from the semi-adiabatic curve
can be kept to a minimum.
8. TEST RESULTS
The test report will document the characteristic para-
APPENDIX 1: THERMAL COMPENSATION
meters of the apparatus and the relevant data of the test. FOR THE APPARENT HEAT CAPACITY OF
For the apparatus the following data will be given: THE CALORIMETER
– working principle (adiabatic or semi-adiabatic)
– volume of the sample The thermal compensation technique consists of
– apparent heat capacity of the calorimeter supplying, by the electrical resistor, an external heat
– coefficient of heat losses α source equal to that accumulated from the apparent heat
– date of the last calibration capacity Ccal while the hydration test is in progress.
– ambient temperature Ta for semi-adiabatic calorimeter For this, the testing time is divided into intervals ∆ti
– the assigned value of Ts - Tj for adiabatic calorimeter. equal to 0.5 h. Starting from the second interval from
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Materials and Structures/Matériaux et Constructions, Vol. 30, October 1997
the beginning of the hydration, the heat to be supplied environment in which the apparatus is placed; Ta shall be
in each interval ∆ti is calculated according to the follow- kept constant (20°C) so the difference Ts(t) – Ta(t) is
ing expression: equal to θs(t).
Ei = [Ts(ti-1) – Ts(ti-2)]⋅Ccal
The power to be supplied is given by: APPENDIX 3: EXAMPLE OF A STEPWISE
Ei CALCULATION TO DETERMINE THE
Pi =
∆t i INTRINSIC TEMPERATURE INCREASE
The corresponding temperature increase at the end FROM A SEMI-ADIABATIC TEST
of the test is corrected for the apparent heat capacity of
the calorimeter, so data reduction will take into account The temperature θ HH of the concrete specimen
the heat losses alone. according to the defined semi-adiabatic conditions is
A check of the reliability of the thermal compensa- given by:
tion technique should be made at the end of the test
through the following verification:
C
[
ϑ HH = 1 + cal ⋅ ϑ s +
Cs ∑ a ⋅ ∆t]
C cal ET
= Table 1 shows an example for the calculation scheme.
CT ϑs ⋅Cs + ET
being ET = Ei the total heat supplied during the test. Cs = 4040 J/K Ccal = 800 J/K τ = 24.8h
a=
(
α Ts − Ta ) (2)
CT
CT
τ= (3)
α
Ts − Ta
a= (4)
τ
Equation (1) can be written in terms of heat of
hydration Q given off by a unit weight of concrete:
CT ⋅ ϑs t ( )+C t
()
Qt =
ms
T
ms ∫ ()
⋅ a t dt
0
(5)
∫ [ () ( )]
t
=
CT
ms s
()
ϑ t + 1 α Ts t − Ta t dt
ms 0
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TC 119-TCE
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Materials and Structures/Matériaux et Constructions, Vol. 30, October 1997
σc = 1 ⋅ σg
(K /K )
g c
(1) Fig. 2 – Schematic drawing of the stress meter.
Fig. 2 shows schematically the stress meter used. The 4.1.1 Variation of temperature within the concrete:
device consists of a load cell which is fixed at one end of This measurement should be carried out at a location
an open box made of wire mesh. The prism and the out- close to the one where the stress is being monitored.
side concrete are “monolithic” through the anchor that is
provided at one end. A similar anchor is provided at the (*) Addresses of suppliers of the stress meter may be obtained from the Institute
load cell. The lid of the box is also made of wire mesh and for Construction Materials, Technical University of Munich, Baumbachstr. 7,
is used to cover the concrete prism after casting. The ther- D-81245 Munich, Germany, Fax: +49 89 289-27064,
mal stresses generated in the concrete due to restraint, etc. E-Mail: [email protected]
458
TC 119-TCE
4.1.2 Variation of strain within the concrete: This Age after placing Frequency of collecting data
measurement should also be recorded at a location close
Up to 1 day Every hour
to the one where the stress is being monitored. 1-3 days Every 6 hours
3-7 days Every 24 hours
4.1.3 Variation of the atmospheric temperature: This After 7 days Every 48 hours
is an important parameter in determining the develop-
ment of thermal stresses in concrete and should be It is recommended that the measurements be contin-
recorded at 2 or 3 suitable locations in the neighbour- ued till the temperature of the concrete reaches the
hood of the structure. ambient temperature.
It may, however, be noted that the stresses can be
accurately measured only so far as no cracks are formed
4.2 Installation of stress meter in concrete in the neighbourhood of the stress meter.
The stress meter can be installed within concrete in a
horizontal, vertical or any other position, to measure the 5. RESULTS
thermal stresses in that direction. The stress meter needs to
be fixed rigidly in place for accurate measurement of the A typical example of the results obtained using the
stress in the desired direction. The steps in the installation stress meter, in terms of the stress history in a 1.5 m thick
of the stress meter can be briefly outlined as given below. concrete, is shown in Fig. 3. The variation of temperature
(1) Make a suitable holder which can be used to sup- recorded is also given in Fig. 4 for reference. The figures
port the stress meter. Reinforcing bars, or any other suit- show the initial compressive stresses generated during the
able material can be used for this purpose, provided the period when the internal temperature rises, and the subse-
meter can be securely held in place during concreting quent transition to tensile stresses on account of the “cool-
and that the stand provides the minimum restraint to the ing” of the concrete. A sudden change in the measured
movement of the concrete in the direction of measuring. stress values indicates possible formation of cracks in the
(2) Secure the holder within the formwork before neighbourhood of the meter and may be taken to mean
the concrete is cast. During casting, when the level of that subsequent the stress values recorded are not accurate.
concrete reaches the level at which it is desired to install
the stress meter, remove a sample of the concrete and fill
the stress meter with it. It must be established that the
following conditions are satisfied:
– the width of the stress meter is more than twice the
size of the maximum size of the aggregate,
– the blotting paper and the felt lining of the stress meter
have been moistened thoroughly before pouring con-
crete into it,
– the concrete placed in the meter (prism) should be
compacted using a tamping rod or by vibrating.
(3) Once the meter has been completely filled with
concrete, cover it with the upper lid and tie it securely
using binding wires.
(4) Wrap the assembly using cloth and moisten with
water until the stress meter is completely enclosed by Fig. 3 – Development of measured stress in concrete structure.
concrete. Secure it to the holder within the formwork.
(5) The vibration in the neighbourhood of the stress
meter may be carried out using mechanical needle vibra-
tors. Care should be taken not to disturb the stress meter
from its position.
Note: The above method for the installation of the
stress meter may be suitably modified depending upon
the type of the structure in question or the location cho-
sen for monitoring the thermal stresses.
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Materials and Structures/Matériaux et Constructions, Vol. 30, October 1997
6. REPORT
A report giving the details of the measurement of
thermal stress, carried out as outlined in this recommen-
dation, must give the following details:
460
TC 119-TCE
The longitudinal steel bars have a diameter of must be at least 40 kN. Thus, a displacement between
100 mm. To guarantee minimal thermal deformation of the bars and cross-heads during the change from com-
the steel bars, a special steel with a low coefficient of pression to tension will be prevented.
thermal expansion has to be used. For this purpose, steel The formwork is made using a thermal insulating
containing 36% nickel is suitable. The cross-heads con- material, e.g. polystyrene with a thickness of 50 mm and
sist of normal steel. A dovetailed opening is located in 24 mm thick wood as a stabilizing element (Fig. 3).
the centre of each cross-head to fix the specimen when Inside the formwork (next to the concrete specimen),
tensile stresses occur (Figs. 2a and 2b). a 0.2 mm thick copper plate is fixed on the polystyrene.
The cross-heads should be enlarged to the top by an This causes the heating of the specimen to be similiar to
angle of about 2°, to enable easy removal of the speci- that of a concrete member of about 50 cm in thickness
men. The two cross-heads must be fixed to the bars with and without any external heating. To enable additional
prestressed screws of at least 30 mm in diameter. heating or cooling within the thermal insulation, copper
Additionally, the steel bars must be prestressed against pipes (6 mm in diameter) are installed which are in con-
the cross-heads in the longitudinal direction by screws tact with the copper plates. Water can be pumped through
(16 mm in diameter) and springs; the prestressing force these pipes.
462
TC 119-TCE
Fig. 3 – Formwork.
The 1.65 m long specimen is fixed within the dove- Before a test is carried out in the cracking frame, the
tails of the cross-heads. To prevent notch stresses in the strain gauges have to be calibrated. This can be done
specimen near the cross-heads, the formwork must be with, for example, two steel bars between the two cross-
formed in a sector of 200 mm in front of the cross-heads heads which are connected with a loading cell and a
in such a way that the specimen is enlarged in a parabolic screw. With the latter, the frame can be loaded under
form continuously without any edge. Thus the specimen compression (i.e. tensile stress in the concrete beam).
has a constant cross-section of 150 × 150 mm2 over a
length of 0.85 m.
To prevent the specimen from drying out during the 4. PREPARATION OF THE CONCRETE
test, the formwork is wrapped additionally with a SPECIMEN
0.3 mm thick polyethylene foil.
Before the concrete is placed into the cracking frame,
the bottom and the two sides of the formwork must be
3.2 Measurements fixed at the frame. A joint of 2-3 mm between the cross-
heads and the formwork must be present on each side,
During the test, the temperature in the centre of the otherwise the deformations of the specimen are addition-
specimen and the stresses in the specimen have to be ally restrained in an uncontrolled way. These joints have to
measured continuously. be sealed with a plastic material, e.g. silicone. In the same
For temperature measurement, thermometers (e.g. way, the joints between the formwork elements have to be
PT 100) are installed in the specimen soon after casting sealed. The fresh concrete is placed directly into the crack-
and finishing of the fresh concrete. This requires only a ing frame. The temperature of the fresh concrete should be
small hole (maximum 3 mm in diameter) for the inser- 20 ± 1°C. After compaction with an internal vibrator, the
tion of the thermometer (otherwise an artificial failure surface is finished in the conventional manner. The surface
will be located). is covered by sticking a polyethylene sheet to the sides of
For the determination of the stress within the speci- the formwork and the cross-heads. The open ends of the
men, strain gauges must be fixed on both of the longitudi- dovetailed cross-heads are then connected with a steel plate
nal steel bars of the cracking frame in the form of a (40 × 10 mm2), each with screws on the upper surface.
Wheatstone bridge. The elastic deformations of the steel This prevents opening of the cross-heads due to tension in
bars due to the restraint force of the concrete specimen can the specimen. The same plates must be screwed onto the
then be measured. In view of the cross-section and the bottom of the cross-heads before the lower formwork is
stiffness (modulus of elasticity) of the steel bars, the actual fixed to the frame.
force (i.e. stress) in the specimen can be determined, The thermometer is then installed in the centre of
because the force in the specimen is of the same value as the specimen. Finally, the thermally-insulated upper
that in the steel bars, however with the opposite sign. formwork is fixed onto the specimen.
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Materials and Structures/Matériaux et Constructions, Vol. 30, October 1997
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