Designation: C 186 – 05

Standard Test Method for

Heat of Hydration of Hydraulic Cement1
This standard is issued under the fixed designation C 186; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope Testing of Hydraulic Cements

1.1 This test method covers the determination of the heat of E 11 Specification for Wire-Cloth Sieves for Testing Pur-
hydration of a hydraulic cement by measuring the heat of poses
solution of the dry cement and the heat of solution of a separate IEEE/ASTM SI 10 Standard for Use of the International
portion of the cement that has been partially hydrated for 7 and System of Units (SI): The Modern Metric System
for 28 days, the difference between these values being the heat 3. Significance and Use
of hydration for the respective hydrating period.
1.2 The results of this test method may be inaccurate if 3.1 The purpose of this test is to determine if the hydraulic
some of the components of the hydraulic cement are insoluble cement under test meets the heat of hydration requirement of
in the nitric acid/hydrofluoric acid solution. the applicable hydraulic cement specification.
1.3 The values stated in SI units are to be regarded as the 3.2 This test may also be used for research purposes when it
standard. The values given in parentheses are for information is desired to determine the heat of hydration of hydraulic
only. cement at any age.
1.4 Values in SI units shall be obtained by measurement in NOTE 1—When tests are performed for research purposes, useful
SI units or by appropriate conversion, using the Rules for additional information can be obtained by determining fineness, chemical
Conversion and Rounding given in Standard IEEE/ASTM SI and compound compositions.
10, or measurements made in other units. 3.3 Determination of the heat of hydration of hydraulic
1.5 This standard does not purport to address all of the cements provides information that is helpful for calculating
safety concerns, if any, associated with its use. It is the temperature rise in mass concrete.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4. Apparatus
bility or regulatory limitations prior to use. 4.1 Calorimetric Apparatus:
4.1.1 Calorimeter—The calorimeter, such as that illustrated
2. Referenced Documents
in Fig. 1 shall consist of a 0.5-L (1-pt), wide-mouth vacuum jar,
2.1 ASTM Standards: 2 with cork stopper, or other suitable non-reactive stopper held in
C 109/C 109M Test Method for Compressive Strength of a suitably insulated container (See 4.1.2) to keep the vacuum
Hydraulic Cement Mortars (Using 2-in. or [50-mm] Cube jar in position and to protect the jar from undue temperature
Specimens) fluctuations. The vacuum jar shall be coated on the interior
C 114 Test Methods for Chemical Analysis of Hydraulic with a material resistant to hydrofluoric acid, such as a baked
Cement phenolic resin, a baked vinyl chloride acetate resin, or bees-
C 670 Practice for Preparing Precision and Bias Statements wax. The acid-resistant coating shall be intact and free of
for Test Methods for Construction Materials cracks at all times; it shall be examined frequently and renewed
C 1005 Specification for Reference Masses and Devices for whenever necessary. As another means of protecting the
Determining Mass and Volume for Use in the Physical vacuum jar, a plastic liner of suitable size may be used instead
of coating the interior of the jar. The contents of the vacuum jar
1
shall not change more than 0.001 °C/min per degree difference
This test method is under the jurisdiction of ASTM Committee C01 on Cement
and is the direct responsibility of Subcommittee C01.26 on Heat of Hydration. from room temperature when filled with 425 g of the acid
Current edition approved July 1, 2005. Published August 2005. Originally specified in 6.2, stoppered, and allowed to stand unstirred for
approved in 1944. Last previous edition approved in 1998 as C 186 – 98.
2
30 min. The temperature for this check shall approximate the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
starting temperatures to be used in making the determination.
Standards volume information, refer to the standard’s Document Summary page on 4.1.2 Insulated Container—The container shall have an
the ASTM website. insulating layer of a material such as non-reactive foam, cotton,

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 C 186 – 05

FIG. 1 Calorimeter

or fiber-glass, which shall be at least 25 mm (1 in.) in thickness be either a Beckman type (See Note 2), which is a mercury-
and shall encase the sides and bottom of the vacuum jar, but in-glass type that only outputs temperature differentials, or a
shall be so arranged as to permit easy removal of the jar. digital type that gives actual temperature outputs. If a Beckman
4.1.3 Thermometers—Two thermometers are required. One type is used, it shall be graduated to at least 0.01 °C, with
is a high precision thermometer required to determine tempera- readings to 0.001 °C that can be estimated by interpolation
ture rise associated with dissolution of cement during determi- between these graduations. It shall also have a temperature
nations. For purposes of this test method, this thermometer is range of at least 6 °C.
called the solution thermometer. The other thermometer is used NOTE 2— If the part of the thermometer that will be in contact with the
for measuring sample temperature before introduction into the test solution is sensitive to the nitric and hydrofluoric acids in the test
calorimeter and air temperature during the determination. For solution, then it is recommended that this part of the thermometer be
purposes of this test method, it is called the reference ther- coated with a resistant material to prolong the service life of the
mometer. thermometer.
4.1.3.1 Solution thermometer—The solution thermometer 4.1.3.2 Reference thermometer—The reference thermom-
shall be readable to 0.001 °C. The solution thermometer may eter shall be any type that reads to a precision of at least 0.1 °C.

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 C 186 – 05
4.1.4 Funnel—The funnel through which the sample is 4.3 Storage—Storage space with temperature controlled at
introduced into the calorimeter shall be glass or plastic and 23.0 6 2.0 °C (73.5 6 3.5 °F).
shall have a stem inside diameter of at least 6 mm (See Note 3). 4.4 Mortar, approximately 200 mm (8 in.) in diameter, and
pestle for grinding the partially hydrated samples.
NOTE 3—The minimum diameter is to prevent clogging of the pow-
dered cement sample. The length of the stem will need to be adjusted so 4.5 Drying Oven, maintained at 100 to 110 °C.
that the sample is delivered without the tip becoming wet from the acid 4.6 Sieves, 150-µm (No. 100) and 850-µm (No. 20), con-
solution, which will cause the funnel to become clogged and necessitate forming to Specification E 11.
aborting the determination. The angle of the stem will need to be adjusted 4.7 Crucibles, platinum, 30-mL capacity, with covers, for
so that sample is not delivered onto the rotating stirrer, which will cause loss on ignition determination.
sample to cake at the liquid line. 4.8 Muffle Furnace, or suitable burners capable of maintain-
4.1.5 Stirring Assembly—The stirrer shall be a three-bladed ing a temperature of 900 to 950 °C.
polyethylene propeller having the dimensions shown in Fig. 2, 4.9 Analytical Balance and Analytical Weights, conforming
and shall extend as closely as possible to the bottom of the to the requirements prescribed in Test Methods C 114 for
calorimeter. The motor shall be of the constant-speed type, at weighing out calorimetric samples and for loss on ignition
least 37 W (1⁄20 hp), and shall be equipped with a geared speed weighings.
reducer so that one speed, in the range of 350 to 700 r/min, can 4.10 Weights and Weighing Devices, conforming to the
be maintained constant. requirements of Specification C 1005. The weighing device
NOTE 4—The stirrer shown in Fig. 2 may be readily made from a
shall be evaluated at a total load of 1000 g.
commercially available three-bladed polyethylene propeller having a
propeller diameter of 34 mm (13⁄8 in.), shaft diameter of 6 mm (1⁄4 in.), and 5. Reagents and Materials
a shaft length of approximately 455 mm (18 in.). The function of the 5.1 Purity of Reagents—Reagent grade chemicals shall be
stirrer is two-fold: to maintain uniform temperature throughout the liquid used in all tests. Unless otherwise indicated, it is intended that
and to supply sufficient agitation to keep the solid in suspension in the acid
all reagents shall conform to the specifications of the Commit-
mixture. Since a stirrer capable of keeping the solid in suspension
generates considerable heat in the calorimeter, it is important that the tee on Analytical Reagents of the American Chemical Society,
stirrer speed, and hence the rate of heat generation, be maintained
constant. Because such constancy is difficult to achieve with other types of
motors, a synchronous motor with a geared speed reducer is recom-
mended.
4.2 Mixer—A moderate-speed mechanical mixer, such as a
milk-shake type stirrer, capable of intimately mixing the
cement and water to a uniform paste.

FIG. 2 Stirrer

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 C 186 – 05
where such specifications are available.3 Other grades may be Brush any ZnO clinging to the funnel stem into the acid
used, provided it is first ascertained that the reagent is of mixture by means of a small “camel’s-hair” brush.
sufficiently high purity to permit its use without lessening the
NOTE 6—The temperature of the sample shall be identical with that of
accuracy of the determination.
the room when the sample is introduced into the calorimeter.
5.2 Hydrofluoric Acid (sp gr 1.15)—Concentrated hydrof-
luoric acid (HF). 6.3 Read the temperature, to the nearest 0.001 °C, at 20 min
5.3 Nitric Acid (2.00 N)—The 2.00 N HNO3, for use in the and again at 40 min after beginning the introduction of the
calorimeter, shall be prepared and standardized in large quan- sample. The temperature rise in the first 20 min includes
tities. Optionally, the dilute HNO3 may be made up with 127 temperature rise due to the heat of solution of the sample and
mL of concentrated HNO3(sp gr 1.42) per litre of solution, any heat gain or heat loss to the environment. This is called the
provided that heat capacity determinations are made with each solution period. The temperature change during the second
batch of diluted HNO3 so prepared. 20-min period is due to heat loss or gain to or from the
5.4 Wax—Paraffin wax, or other suitable wax, for sealing environment. It is used to correct the temperature rise in the
vials. solution period to give the actual heat of solution of the sample.
5.5 Zinc Oxide (ZnO)—The ZnO shall be heated at 900 to The second 20-min period is called the correction period.
950 °C for 1 h, then cooled in a desiccator, ground to pass a 6.4 Calculate the corrected temperature rise as follows:
150-µm (No. 100) sieve, and stored. Immediately prior to a Ro 5 u20 2 u0 (1)
heat capacity determination, 7 g of the ZnO so prepared shall
R 5 Ro 2 ~u40 2 u20!
be heated for not more than 5 min at 900 to 950 °C, cooled to
room temperature in a desiccator, and weighed accurately for where:
introduction into the calorimeter. Ro = observed temperature rise, °C,
NOTE 5—The rate of solution of the ZnO varies with the preliminary u20 = calorimeter temperature at the end of the solution
treatment. The procedure described results in a product which dissolves at period,
about the same rate as the dry cement. u0 = calorimeter temperature when sample was intro-
duced,
6. Determination of Heat Capacity of Apparatus R = corrected temperature rise, °C, and
6.1 To determine the heat capacity of the system (that is, the u40 = calorimeter temperature at the end of the correction
number of joules or calories required to raise the temperature period.
of the calorimeter and contents 1 °C), measure the corrected 6.5 Calculate the heat capacity of the calorimeter and
temperature rise obtained by dissolving 7 g of ignited ZnO in contents as follows (See Note 7):
the specified acid mixture (See 6.2-6.7). W[1072 1 0.4~30 2 t! 1 0.5~T 2 t!#
6.2 Transfer approximately 400 g of the 2.00 N HNO3, C5 R (2)
which has been cooled to the temperature indicated by the
lower range of the Beckmann thermometer (ordinarily about 4
to 5 °C below room temperature), into the vacuum jar, add 8.0 where:
mL of HF (sp gr 1.15), weigh, and add sufficient additional C = heat capacity, kJ/°C,
2.00 N HNO3 to bring the total weight of the solution to 425.0 W = mass of ZnO, g,
t = final temperature of the calorimeter, °C (u20 plus
g. Then, assemble the calorimeter and start the stirring motor.
temperature, °C, at which the Beckmann thermometer
Take care that the stirrer blades or shaft do not touch the
reading is zero),
thermometer, the sides or bottom of the jar, or the cork stopper.
T = temperature of the ZnO (room temperature), °C, when
The lower end of the funnel stem shall extend approximately 6
introduced into the calorimeter, and
mm (1⁄4 in.) below the lower surface of the stopper and at least R = corrected temperature rise, °C.
12 mm (1⁄2 in.) above the level of the liquid. The upper end of
the bulb of the Beckmann thermometer shall be at least 38 mm NOTE 7—The heat of solution of ZnO is 1072 kJ/kg (256.1 cal/g) at 30
(11⁄2 in.) below the surface of the liquid. Place it at the same °C. This value increases 0.4 kJ/kg (0.1 cal/g) for each degree decrease in
depth in all determinations. After an initial stirring period of at temperature below 30 °C. The heat capacity of ZnO is 0.5 kJ/kg·K (0.12
cal/g·°C). The heat required to bring the ZnO to the final temperature of
least 20 min to allow the temperature of the system to become
the calorimeter must be included in the effective heat of solution.
uniform, record the temperature of the room to the nearest 0.1
°C, the temperature of the acid to the nearest 0.001 °C, record 6.6 If more than a trace of ZnO is found adhering to the tip
the time, and then immediately introduce the prepared ZnO of the funnel or to the stopper when the calorimeter is opened,
through the funnel at a uniform rate (See Note 6). Complete the reject the test.
introduction of the ZnO in not less than 1 or more than 2 min. 6.7 Redetermine the heat capacity at the following times:
6.7.1 When the Beckmann thermometer (if used) is reset,
3
Reagent Chemicals, American Chemical Society Specifications, American
6.7.2 When a new coating is applied to the solution ther-
Chemical Society, Washington, DC. For suggestions on the testing of reagents not mometer, stirrer, or flask,
listed by the American Chemical Society, see Analar Standards for Laboratory 6.7.3 When a new solution thermometer, stirrer, or flask is
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
put in service,
MD. 6.7.4 When a new batch of acid is used, and

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 C 186 – 05
6.7.5 At other times when, according to the judgment of the then place the sample in a muffle furnace at 950 6 50 °C
operator, the need is indicated. overnight, or bring to constant mass. Reduce the mass of the
cement sample that was introduced into the calorimeter to the
7. Sampling and Test Specimens ignited mass basis for use in the final calculations as follows:
7.1 Preparation of Cement Paste—Store the cement and the Wi 5 ~A/B!W (3)
mixing water in a constant-temperature room at 23.0 6 2.0 °C
(73.5 6 3.5 °F) until the materials are at ambient temperature where:
before preparation of the paste. Mix 150 g of cement and 60 Wi = mass of calorimetric sample, on ignited basis, g,
mL of distilled water by means of a spatula, and then A = mass of ignited sample, g,
vigorously stir the mixture with a mechanical stirrer for 5 min. B = mass of sample before ignition, g, and
Place approximately equal representative portions of the paste W = mass of calorimetric sample, g.
in four or more plastic vials, filling the vials to within about 13 8.3.2 Blended Hydraulic Cements—In addition to the pro-
mm (1⁄2 in.) of the top. Immediately after filling the vials, close cedures described in 8.3.1, determine the loss on ignition by
them with tight-fitting stoppers or caps. (If there is any doubt the reference method given in Test Methods C 114 for portland
regarding the tightness of the seal, the sealed ends of the vials blast-furnace slag cement and slag cement.
should be dipped in molten paraffin wax.) Store the vials in an 8.3.2.1 Determine the SO3 content by the reference method
upright position in a water bath at 23 6 2.0 °C until the time given in Test Methods C 114 (See Note 8). Also determine the
of test. SO3 content of a portion of the same cement that has not been
7.2 Preparation of Partially Hydrated Sample for Heat of ignited, using the same procedure.
Solution Test—At the specified age of test or age of interest, 8.3.2.2 Calculate the percentage of mass gain from sulfide
remove a vial of the partially hydrated sample from storage sulfur as follows:
within the test time tolerances of Test Method C 109/C 109M, G 5 0.8 ~S1 2 S2! (4)
and, during a 20-min initial stirring period of the calorimeter,
break the plastic away from the sample and rapidly crush the where:
entire sample with a mortar and pestle so that all the material G = percent mass gain in ignited sample,
will pass through a 850-µm (No. 20) sieve; then quickly place S1 = SO3 determined on ignited sample, and
the sample in a well-stoppered weighing bottle. Take care, S2 = SO3 determined on unignited sample.
particularly with the 7-day partially hydrated sample, to expose 0.8 = molecular weight ratio of 4(0)/SO3
the sample to the air as little as possible, and thus minimize the NOTE 8—Some of the acid used for dissolving the sample may first be
action of CO2 or the loss of moisture from the sample. warmed in the platinum crucible to dissolve any adhering material.

8. Procedure 8.3.2.3 Calculate the mass of the dry calorimetric sample on

8.1 Calorimetric Procedure, Dry Cement—Determine the the ignited basis as follows:
heat of solution of the dry cement sample according to the
procedure described for the heat capacity determination (See Wi 5
S BG
A 2 100 D W
(5)
Section 6), but use a 3-g sample (weighed to the nearest 0.001 B
g) of the dry cement instead of the prepared ZnO (See Note 6).
where:
(Exercise care in securing a uniform and representative Wi = mass of dry calorimetric sample, on ignited basis, g,
sample.) Calculate and report the results on the ignited mass A = mass of ignited dry sample, g,
basis (See 8.3). B = mass of dry sample before ignition, g,
8.2 Calorimetric Procedure, Partially Hydrated Sample— G = percentage mass gain from sulfide sulfur, and
For the heat of solution of the partially hydrated sample follow W = mass of dry calorimetric sample, g.
the same procedure as for the dry cement described in 8.1, but Calculate the mass of the partially hydrated calorimetric
use a 4.18 6 0.05-g calorimetric sample of the partially sample on the ignited basis as follows: (See Note 9)
hydrated cement, weighed to the nearest 0.001 g (See Note 6).
Calculate the results on the ignited basis.
8.3 Loss on Ignition: Wi 5
S G
A W 1 2 100 D (6)
B
8.3.1 Portland Cement—Immediately before and after the
calorimetric sample is being weighed out, weigh a sample of where:
similar amount into a platinum crucible for determination of Wi = mass of calorimetric sample, on ignited basis, g,
loss on ignition, the value to be used being the average of the A = mass of partially hydrated sample after ignition, g,
two determinations. Ignite the dry cement at 950 6 50 °C for B = mass of partially hydrated sample before ignition, g,
at least 11⁄2 h or to constant mass. Immediately place the G = percentage mass gain from sulfide sulfur, and
crucible containing the sample in a desiccator and allow to cool W = mass of partially hydrated calorimetric sample, g.
to room temperature; then quickly weigh the crucible. When NOTE 9—An assumption is made in the calculation that the same
determining the loss on ignition of the hydrated cement, first percentage of sulfide sulfur is present prior to ignition in the partially
dry the weighed sample in an oven at 100 to 110 °C for 1 h; hydrated sample as was determined in the cement. Tests have confirmed

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 C 186 – 05
that the assumption is reasonably correct and will not alter the precision th = final calorimeter temperature at end of
of the test method.
determination on partially hydrated
9. Calculation sample, °C.
9.3 Heat of Hydration—A final calorimeter temperature of
9.1 Heat of Solution of Dry Cement—Calculate the cor- 25 °C shall be considered as the basis to which the heat of
rected temperature rise as described in 6.3 and 6.4. Also, hydration shall be referred, and the effects of variation in that
correct the heat of solution value if the final calorimeter temperature should be kept in mind when considering test
temperature of the heat of solution test is different from the results. An increase in the final temperature raises the heat of
temperature of the calorimetric sample when introduced. Thus, hydration approximately 0.4 kJ/kg·K (0.1 cal/g·°C) of ignited
for the dry cement, which has a specific heat of approximately cement. For example, if the final temperature is 27 °C, 0.8
0.8 kJ/kg·K (0.2 cal/g·°C), if the final calorimeter temperature kJ/kg (0.2 cal/g) should be subtracted from the observed heat
exceeds the temperature of the cement sample at the time it was of hydration in order to refer the results to 25 °C. In borderline
introduced, add a correction of 0.8 kJ/kg·K (0.2 cal/g·°C) cases, proper correction should be made for the effects of final
difference in those temperatures when calculating the heat of calorimeter temperature. Calculate the heat of hydration of the
solution. Calculate the heat of solution of the dry cement as cement to the nearest kilojoule, as follows:
follows:
H 5 H1 2 H2 2 0.4~th 2 25.0! (9)
H1 5 ~RC/Wi! 2 0.8~T 2 td! (7)
where:
where: H = heat of hydration of ignited cement, kJ/kg,
H1 = heat of solution of dry cement, kJ/kg, H1 = heat of solution of dry cement (See 9.1),
R = corrected temperature rise, °C, H2 = heat of solution of partially hydrated sample (See
C = heat capacity, kJ/°C, 9.2), and
Wi = mass of sample on ignited basis, g, th = the same numerical value as in 9.2.3
T = room temperature, when sample is introduced, °C,
and NOTE 10—To convert cal/g to kJ/kg multiply by 4.184 in accordance
td = final calorimeter temperature at end of determination with Standard IEEE/ASTM SI 10.
on dry cement, °C. 10. Retests
9.2 Heat of Solution of Partially Hydrated Sample—
Calculate the heat of solution of the partially hydrated sample 10.1 In case of failure to meet the 28-day requirement for
in the same way as for the dry cement (See 9.1), except make heat of hydration, a reserve sample of paste may be tested at a
additional corrections, as follows: later age and a correction of 2.1 kJ/kg (0.5 cal/g) per day of
excess age added to bring the retested heat of solution to a
9.2.1 Since an increase of 1 °C in the temperature at which
28-day basis. The period over which this correction may be
the heat of solution test occurs causes a decrease of approxi-
made shall be limited to 4 days. In case of failure to meet the
mately 1.3 kJ/kg (0.3 cal/g) in the heat of solution, if the
7-day requirement, a complete retest including mixing of the
temperature of the heat of solution test of the partially hydrated
paste should be made.
sample exceeds the temperature of the dry cement determina-
tion, a correction of 1.3 kJ/kg·K (°C) difference in temperature
11. Report
shall be added to the heat of solution value obtained for the
partially hydrated sample (See Eq 8). 11.1 Report the following information:
9.2.2 Also, correct the heat of solution value if the final 11.1.1 Sample identification, which may include the source
calorimeter temperature of the solution test is different from the and type of hydraulic cement and sampling date, and
temperature of the calorimetric sample when introduced. Thus, 11.1.2 The heat of hydration results at each of the test ages
for the partially hydrated sample, which has a specific heat of required by the applicable specification.
approximately 1.7 kJ/kg (0.4 cal/g) of ignited cement, if the
final calorimeter temperature exceeds the temperature of the 12. Precision and Bias
sample at the time it was introduced, add a correction of 1.7 12.1 Precision:
kJ/kg·K (°C) difference in those temperatures when calculating 12.1.1 Single-Operator Precision—The single-operator
the heat of solution (See Eq 8). standard deviations have been found to be 12.2 kJ/kg(1s) (2.91
9.2.3 Calculate the heat of solution of the partially hydrated cal/g)(1s) and 14.8 kJ/kg(1s) (3.54 cal/g)(1s) for the determi-
sample as follows: nations of heat of solution and heat of hydration, respectively.
H2 5 ~RC/Wi! 2 1.7~T 2 th! 2 1.3~td 2 th! (8)
Therefore, results of two properly conducted tests by the same
operator on samples of the same cement should not differ from
where: each other by more than 34 kJ/kg (8 cal/g) in the determination
H2 = heat of solution of partially hydrated of heat of solution or 42 kJ/kg (10 cal/g) in the determination
sample, kJ/kg, of heat of hydration.4
R, C, Wi, and T = the same definition as in 9.1 except that
they relate to the partially hydrated
sample, 4
These numbers represent, respectively the (1s) and (d2s) limits as described in
td = the same numerical value as in 9.1, and Practice C 670.

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 C 186 – 05
12.1.2 Multilaboratory Precision—The multilaboratory 12.2 Bias—Since there is no accepted reference material, no
standard deviations have been found to be 18.5 kJ/kg(1s) (4.42 statement on bias is being made.
cal/g)(1s) and 16.9 kJ/kg(1s) (4.03 cal/g)(1s) for the determi-
nations of heat of solution and heat of hydration respectively. 13. Keywords
Therefore, results of two properly conducted tests from two
different laboratories on samples of the same cement should 13.1 blended cement; heat of hydration; heat of solution;
not differ from each other by more than 52 kJ/kg (13 cal/g) in hydraulic cements; portland cement
the determination of heat of solution or 48 kJ/kg (11 cal/g) in
the determination of heat of hydration.4

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