Heat of Hydration: IS 4031 (part 9)

This test method covers the determination of the heat of hydration of a hydraulic cement
by measuring the heat of solution of the dry cement and the heat of solution of a separate portion
of the cement that has been partially hydrated for 7 and for 28 days, the difference between these
values being the heat of hydration for the respective hydrating period.
Significance and use:
The purpose of this test is to determine if the hydraulic cement under test meets the heat
of hydration requirement of the applicable hydraulic cement specification.
This test may also be used for research purposes when it is desired to determine the heat
of hydration of hydraulic cement at any age.
Determination of the heat of hydration of hydraulic cements provides information that is
helpful for calculating temperature rise in mass concrete.
Apparatus Used:
Calorimetric apparatus having calaorimeter, insulated container, thermometers, funnel
and stirring assembly.
Mixer: A moderate speed mechanical mixer to mix the cement paste and water
Sieves
Crucibles
Muffle furnace
Weighing balance
Reagents Used:
Hydrofluoric ancid
Nitric acid
Parrafin wax
Zinc oxide
Determination of heat capacity
Measure 9.6 0.1 ml of hydrofluoric acid and 388 0.1 ml of 2.0 N Nitric acid in the
calorimeter. The acid solutions have a temperature in the range of 27 2oC.
Ignition of Zinc oxide: ZnO is ignited for 1 h at 900 to 950oC in muffle furnace and then
cooled in a desiccator containing anhydrous calcium chloride and grind it to pass a 150
IS sieve.
About 7.0 g of ignited ZnO is taken and is again heated to 900 to 950oC in muffle furnace
1
for 5 minutes and then colled for not less than 2 2 hours and not more than 5 hours in

a desiccator containing anhydrous CaCl2.

In the calorimeter, run the stirrer for atleast 5 min to allow the temperature to uniform and
measure the temperature at every 1 min to determine the initial heating or cooling
correction.

Then the ignited ZnO is poured into the calorimeter through funnel steadily within a
period of 1 to 2 min.
Take temperature reading at every 1 min interval until steady state of heating or cooling
of calorimeter is obtained. This is called solution period and it should not exceed 20 min.
Continue the reading for further 5 minutes to determine the final heating or cooling
correction.
Plot initial and final heating or cooling rates against the corresponding calorimeter
temperature readings namely Beckmann readings at the beginning of the solution period
and at the end and join the two points by a straight line.
Using this graph, the corrections are read off for each temperature reading during the
solution period and it is added or subtracted to the observed temperature rise.
Mass of ZnO
Heat Capacity=
X ( 1072+ 0.4 ( 30 ) +0.5 ( o ) )
Corrected Temperature rise

Where,
1072 = heat of solution of ZnO at 30oC
0.4 = negative temperature coefficient of heat of solution
= final temperature of calorimeter
o = room temperature
0.5 = specific heat of ZnO
Preparation of cement sample:
Measure 60 g of cement and 24 ml of distilled water and it is mixed in hand.
Fill this mixture in 3 plastic vials and seal the wax.
Store the specimen vials with mixture in a vertical position at 272oC.
Determination of heat of solution of the unhydrated cement:
Weigh a cement sample of 3.0 g and also take 7.0 g of sample for heat of solution and
ignition loss
Carry out the test to determine the temperature rise in the calorimeter exactly as described
for ZnO.
Heat Capacity of theunhydrated cement paste=

Heat capacity X Corrected Temperature rise

0.8(o)
Mass of sample corrected for ignitionloss

Where,
0.8 is the specific heat of unhydrated cement
Determination of heat of solution of the hydrated cement:
Open the plastic vial and remove the wax placed over the cement and grind the cement
rapidly to avoid carbonation and pass the sample in 850 IS sieve.
Weigh 4.2 g and 7.0 g of sample for heat of solution and ignition loss
Carry out the test to determine the temperature rise in the calorimeter exactly as described
for ZnO.

Heat Capacity of thehydrated cement paste=

Heat capacity X Corrected Temperature rise

1.7 ( o)
Mass of sample corrected for ignitionloss

Where,
1.7 is the specific heat of hydrated cement
Determination of mass of sample corrected for ignition loss:

The sample is placed in a muffle furnace 900 50 oC for 3 to 4 h and then cool it in a
desiccators containing anhydrous CaCl2 and it is weighed after half an hour