Journal of ASTM International, Vol. 6, No.

10
Paper ID JAI102364
Available online at www.astm.org

Hugh Wang,1 Chengqing Qi,2 Waltter Lopez,3 and Hamid Farzam4

Use of Isothermal Conduction Calorimetric Method for

Measuring the Heat of Hydration of Cement

ABSTRACT: In the present study, an extensive test program is conducted to measure and compare the
heat of hydration obtained from both calorimeter and ASTM C186-05 test methods. A statistical analysis is
performed to evaluate the variations of the test data. The results indicate that the isothermal conduction
calorimeter method is a more reliable, less time-consuming, and less labor-intensive method than the
ASTM C186-05 test method. The heat of hydration at 3 days showed the least variation in all calorimeter
tests. These suggest that ASTM shall consider adopting the isothermal conduction calorimeter method for
measuring the heat of hydration of cement. The 3-day heat of hydration value can be used for specifying
the limit of heat release for type II cements.
KEYWORDS: cement, heat of hydration, ASTM C186-05, isothermal conduction calorimeter

Introduction
As part of the efforts to harmonize ASTM C150-07 关1兴 and AASHTO M85-08 关2兴, Standard Specification
for Portland Cement, ASTM Technical Committee C01 approved the inclusion of 7-day heat of hydration
共HoH兲 as an optional requirement for ASTM Standard C150-07 type II cement. It is required to determine
7-day HoH with ASTM C186-05 关3兴, Standard Test Method for Heat of Hydration of Hydraulic Cement.
The revised standard specification states that “7-day heat of hydration testing by Test Method C186 shall
be conducted at least once every six months. Such testing shall not be used for acceptance or rejection of
the cement, but results shall be reported for informational purposes.” It is noted that although the test result
of HoH is not mandatory information required for cement product certification, the producers have to
perform such a time-consuming and labor-intensive test by following the current ASTM C186-05 test
procedures.
The ASTM C186-05 is an indirect method to obtain the HoH of cement by determining the heat of
solution. Previously published research work by Killoh 关4兴 in the 1980s, “A Comparison of Conduction
Calorimeter and Heat of Solution Methods for Measurement of the Heat of Hydration of Cement,” clearly
summarized and compared the advantages and disadvantages of both heat of solution and conduction
calorimeter methods. It was concluded that “Isothermal heat of hydration of cement can be obtained more
readily and with greater precision using conduction calorimetry in place of the more laborious heat of
solution procedure.” In spite of the obvious advantages of the isothermal conduction calorimetric method,
the progress in developing a standard for HoH measurement based on this technology has been slow. After
many years of work by the members of ASTM C01.26 subcommittee, a proposed new standard test
method for measurement of heat of hydration of hydraulic cementitious materials using isothermal con-
duction calorimetry 关5兴 was drafted and is in the balloting process of the ASTM C01 Main Committee. The
research work in this paper is intended to develop some supplementary information, which may be useful
for current ASTM standard development efforts.
The main objectives of this paper are to

Manuscript received February 5, 2009; accepted for publication August 28, 2009; published online October 2009.
1
Director, CEMEX Technical Center, 6725 78th St., Riverview, FL 33578, e-mail: hugh.wang@cemex.com
2
Senior Scientist, CEMEX Technical Center, 6725 78th St., Riverview, FL 33578, e-mail: chengqing.qi@cemex.com
3
Director, Product Development and Cement Operations Support, CEMEX Technical Center, 6725 78th St., Riverview, FL 33578,
e-mail: waltter.lopez@cemex.com
4
Vice President, Technical Services and Quality Assurance, CEMEX USA, 920 Memorial City Way, Houston, TX 77024, e-mail:
hamid.farzam@cemex.com

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 2 JOURNAL OF ASTM INTERNATIONAL

TABLE 1—Cement chemistry, Blaine fineness, and mineral compositions.

Cement Chemistry 共%兲 Blaine Fineness Mineral Composition 共%兲

Cement ID SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2Oeq f -CaO Blaine C 3S C 2S C 3A C4AF
C-01 20.42 4.21 3.33 64.95 1.12 2.62 0.58 2.00 3850 68.72 6.69 5.52 10.13
C-02 20.41 4.98 3.65 64.60 0.52 3.15 0.40 1.40 4050 60.20 13.11 7.04 11.09
C-03 21.03 5.54 3.74 62.58 0.90 3.28 0.38 0.78 4010 43.06 27.80 8.34 11.38
C-04 20.65 5.21 3.96 63.47 0.86 3.40 0.39 0.62 4000 51.05 20.69 7.11 12.05
C-05 20.33 5.01 4.14 63.75 1.04 3.51 0.30 0.95 3850 55.41 16.49 6.26 12.60
C-06 20.47 4.07 3.87 62.90 2.45 2.33 0.55 1.25 4010 61.03 12.64 4.22 11.78
C-07 20.43 3.90 3.78 63.65 1.78 2.66 0.61 1.34 4010 64.62 9.82 3.95 11.50
C-08 19.63 4.72 2.92 62.01 4.71 3.02 0.82 0.82 3770 58.75 11.97 7.56 8.90
C-09 19.57 5.42 4.16 63.23 1.69 2.83 0.52 1.45 3830 58.32 12.10 7.31 12.66
C-10 20.91 4.53 3.53 63.60 2.12 2.64 0.71 1.03 3480 56.93 17.01 6.03 10.75
C-11 20.44 4.45 3.28 64.32 1.05 3.09 0.76 0.88 3970 63.15 10.95 6.23 9.99
C-12 20.65 5.13 4.09 63.97 0.90 3.20 0.35 0.91 3650 54.05 18.41 6.69 12.44
C-13 20.56 5.12 4.16 64.17 0.92 2.91 0.36 1.12 3800 56.38 16.40 6.52 12.67
C-14 21.11 4.23 4.45 63.44 0.76 3.93 0.52 1.20 4210 51.80 21.45 3.69 13.55
C-15 20.50 4.94 3.35 62.74 2.55 2.91 0.48 1.04 3840 53.37 18.51 7.43 10.19
C-16 19.81 5.20 3.52 62.66 2.98 2.55 0.49 2.00 3930 57.31 13.56 7.82 10.70
C-17 20.76 3.54 3.38 63.00 4.71 2.62 0.42 1.07 3690 62.55 12.34 3.67 10.28

共1兲 evaluate the isothermal conduction calorimetric technique 共calorimeter兲 for HoH determination of
cement;
共2兲 establish practical operational procedures with a specific commercial calorimeter instrument;
共3兲 study the statistical implication of the data collected from calorimeter tests;
共4兲 evaluate and compare HoH results obtained from calorimeter and ASTM C186-05 methods; and
共5兲 relate HoH values obtained from calorimeter and ASTM C186-05 to the early-age strength devel-
opment.

Experimental Program

Materials
All cement samples used in this test program were from commercial sources. In order to have represen-
tative data, cements produced at various locations on different production dates were selected for evalu-
ations. The chemistry, Blaine fineness, and mineral compositions of these cements are summarized in
Table 1.

Testing Techniques

ASTM C186-05 method [3]—This test method determines the HoH of 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 mixed with water and hydrated to a specified age; the difference between the heats of solution of dry
cement and hydrated cement is the value of HoH for this cement at the specified age. ASTM C186-05
requires a fixed w / c ratio of 0.40 for preparing the cement paste and specifies the limit of 7-day HoH value
for cement certification. The heat of solution of hydrated and unhydrated cement is determined through
many steps involving tedious preparation of hydrated cement sample, the use of chemical agents, and
analytical skills of wet chemistry. Full details of the analytical and calculation process are given in ASTM
C186-05.

Calorimeter Instrument and Calorimetric Test Method—The calorimeter used in this program was a
commercial instrument, namely, TAM Air, manufactured by Thermometric AB, Sweden. TAM Air is an
eight-channel isothermal heat conduction calorimeter. Based on the manufacture’s technical datasheet, “the
calorimeter measures heat flow in the milliwatt range. The operating temperature range is 5 – 60° C. All
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 WANG ET AL. ON ISOTHERMAL CONDUCTION CALORIMETRIC METHOD 3

TABLE 2—Calorimeter test operations.

Mixing Method External Internal

Cement testing laboratory, CCRL inspected
Laboratory condition and meets ASTM C109-05 specified temperature and humidity conditions
Cement sample size 50 g 3.333 g
Water source Distilled water Distilled water
Cement and water were equilibrated to room Cement was loaded into testing cell and
Cement and water temperature temperature before use equilibrated to the testing temperature
5 g of paste was transferred to the testing cell of
calorimeter for HoH measurement after completing Inject distilled water into testing cell and follow
Mixing and handling specified mixing procedures specified mixing procedures

calorimetric channels are of twin type, consisting of a sample and a reference vessel, each with a volume
of 20 mL. The thermostat uses circulating air and an advanced temperature regulating system to keep the
temperature very stable within ⫾0.02 K.” The calorimeter was fully calibrated based on the calibration
procedures specified by the manufacturer. All the calibration parameters met manufacturer’s specifications.
The energy change during hydration is collected and registered by an automated data acquisition program.
The energy value is based on the unit weight of cement mass.
The sample preparation, testing conditions, and procedures for the calorimeter test are summarized in
Table 2.
Before calorimeter tests were conducted for data collection and data analysis purposes, a series of test
procedures was examined with the objective of selecting a standard operating procedure for testing. These
include the following:
• Mixing tool selection—Several mixing tools were experimented for both external mixing 共EM兲 and
internal mixing 共IM兲 procedures. A kitchen blender MixMaster 2524, manufactured by Sunbeam®,
was selected for the EM procedure. The EM procedure involves mixing cement paste outside the
calorimeter for certain amount of time and then transferring the paste to the testing vial for data
collection. In this testing procedure, the HoH is not counted during the period of EM. A modified
mini-electrical drill mixer was chosen for IM procedure. The IM was conducted by pre-loading
cement material into the testing vial and then injecting water into the sample vial followed by
mixing action. The HoH was simultaneously collected during the mixing operation. These tools and
subsequent procedures were used throughout this program.
• Paste w / c ratio determination—Mixtures with different water to cement ratios were evaluated. A
fixed w / c ratio of 0.50 was adopted in this study. Based on the observations, if the w / c ratios were
below 0.50, the paste appeared insufficiently flowable to facilitate effective transfer of the paste
from the mixing bowl to the testing vial. Whereas, when the w / c ratios were higher than 0.50, the
slurry had the tendency of segregation during the paste transferring process.
• Mixing time determination—When experimenting with the EM procedure, various mixing times
were examined before loading paste into the test vial. The objective was to evaluate the sensitivity
of the heat release signature to the EM time.

Cement Strength Test—It is widely accepted that cement strength development is directly related to the
hydration heat release 关6,7兴. This is particularly true during the early stages of cement hydration and
strength development. The objective of the strength test was to establish a strength database and compare
the strength development with the heat release. ASTM C109-05 procedure was used for all the strength
testing in this study 关8兴.

Results and Discussions

Effects of Mixing Time on the Heat Release (External Mixing Procedure)

Three mixing procedures were evaluated for the EM method. The detailed descriptions of the procedures
are listed in Table 3. The first number in the mix code in Table 3 represents the premixing time 共30 s兲, and
the second number describes the intense mixing time 共45, 75, and 120 s兲 at speed position 3. The
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TABLE 3—Mixing procedure for calorimeter test with EM method.

Mix Code 30–45 30–75 30–120

Procedure Premixing 30 s at speed position number 1
Intense mixing 45, 75, and 120 s at speed position number 3, respectively

premixing was conducted at lower speed 共position number 1 on the blender speed control dial gage兲.
During this period, any lumps in the cement paste were broken down. After premixing, intense mixing at
a higher speed 共position number 3 on the blender speed control dial gage兲 was applied. Three different
intense mixing times of 45, 75, or 120 s were evaluated.
A typical ASTM C150-07 T II cement was used for evaluating the effect of the EM procedures on the
HoH. For each mixing procedure, tests were conducted in pairs. The heat release values are summarized
in Table 4. With 45 s of intense mixing, the heat release at 30 min and 24 h is slightly lower than the heat
release with the other two longer intense mixing procedures of 75 and 120 s. This was likely due to the
insufficient mixing time to disperse the cement particles. The highest heat release is from 75 s of the
intense mixing procedure. The longest intense mixing time of 120 s also reduced the heat release. This is
probably caused by the loss of the hydration heat during the EM time.
It is interesting to note that the heat release variation among the different intense mixing times mainly
occurred during the first 30 min of cement hydration. The heat release from 30 min to 24 h for 75 and 120
s of intense mixing time remains the same.
Figure 1 shows the actual hydration profiles of the cement pastes with different mixing procedures.
The heat release rates during the first 30 min are illustrated in Fig. 1共a兲. Relatively large variation was
observed during this period. However, all heat release rates returned to approximately the same baseline
after 30 min. This indicates that hydration is stabilized from the rapid initial heat release in the early
minutes. The heat release variation was also reflected in the cumulative heat release as shown in Fig. 1共b兲.
Figure 1共c兲 shows the heat release rates from 30 min to 24 h. By and large, no significant variation can
be seen regardless of the intense mixing duration. The total heat release profiles shown in Fig. 1共d兲
indicates that the 30–45 mixing procedure releases slightly less heat than the other two procedures of
30–75 and 30–120. This difference in the total heat release largely originated from the early period as
shown in Table 4.
Regardless of the variation in the early minutes, the final total heat release at 24 h did not appear to be
significantly different. Therefore, for the purpose of standardizing the mixing procedure, 30 s of premixing
followed by 75 s of intense mixing was used throughout the rest of this study.

Internal Mixing versus External Mixing

There is a strong interest in the technical community to understand the HoH variation when the cement and
water are mixed inside of the testing vial of the calorimeter versus the procedure when it is mixed
externally prior to transferring the paste into the testing vial. The argument has been largely focused on the
unknown amount of heat not accounted for when the EM method is used. Extensive experiments were
conducted to compare the heat release changes between IM and EM methods. In addition, statistical
evaluation was also conducted on the heat release data collected from both mixing methods. Table 5 shows
the HoH values obtained from both EM and IM methods at various ages up to 7 days. Several essential

TABLE 4—Heat release comparison with different mixing procedures.

Mix Code

30–45 30–45 30–75 30–75 30–120 30–120

Time Energy 共kJ/kg兲
30 min 17.8 18.9 21.3 22.1 20.5 17.5
30 min average 18.3 21.7 19.0
24 h 208 210 214 214 213 210
24 h average 209 214 211

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 WANG ET AL. ON ISOTHERMAL CONDUCTION CALORIMETRIC METHOD 5

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statistical parameters such as mean 共␮兲, standard deviation 共␴兲, and coefficient of variation 共CV兲 are also
summarized in Table 5. In addition, the statistical information from ASTM C186-05 is also listed in Table
5 for comparison purpose.
• Heat loss from the EM procedure: Not surprisingly, the HoH with the EM method is lower than the
HoH with the IM method across all test ages. The amount of HoH loss is generally around 14–19
kJ/kg depending on the hydration ages 共Table 6兲. In general, most of the heat loss takes place in the
first 30 min. About 41 % heat was lost during the first 30 min, while only 3.8 % heat was lost at 7
days. The heat loss at the early ages is mostly related to the unaccounted heat release before the
cement paste was loaded into the test vial.
• Statistical variation ␴: Statistically, both IM and EM methods show more or less the same trend in
␴, except at the age of 30 min. After 12 h, ␴ showed an increasing trend with the increase in the

TABLE 5—HOH results from calorimeter and ASTM C186-05 test methods.

Calorimeter Method

HoH 共kJ/kg兲 IM Statistical Data ASTM C186-05

Time IM-1 IM-2 IM-3 IM-4 IM-5 IM-6 IM-7 ␮ 共kJ/kg兲 ␴ 共kJ/kg兲 CV 共%兲 ␴ 共kJ/kg兲
0.5 h 32 35 38 37 33 31 33 34 2.6 7.69 Within lab Between lab
12 h 167 175 177 176 174 169 171 173 3.7 2.15
1 day 246 251 256 256 253 248 252 252 3.9 1.53
2 days 297 302 308 309 305 300 306 304 4.4 1.43
3 days 324 329 336 337 333 327 335 332 4.9 1.48
7 days 362 368 380 382 382 369 387 376 9.3 2.47

Time EM-1 EM-2 EM-3 EM-4 EM-5 EM-6 EM-7 EM statistical data

0.5 h 21 19 17 18 20 22 22 20 1.8 8.88

12 h 155 153 155 156 157 154 156 155 1.4 0.93
1 day 235 231 233 234 236 231 234 234 1.8 0.78
2 days 289 283 286 288 289 282 287 286 2.9 1.01
3 days 318 310 316 318 318 309 316 315 4.0 1.26
7 days 365 350 366 371 369 348 361 361 9.1 2.52 14.8 16.9

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TABLE 6—The amount of HoH loss from EM.

Heat Loss from External Mixing

Time kJ/kg %
0.5 h 14.0 41.3
12 h 17.3 10.0
1 day 18.2 7.2
2 days 17.6 5.8
3 days 16.4 4.9
7 days 14.2 3.8

testing ages. This trend is graphically shown in Fig. 2. EM shows a lower standard deviation than
the IM.
• Statistical variation CV: Based on the absolute value of ␴, it seems that ␴ trended up drastically.
However, the ␮ value also significantly increased with the progress of hydration time. The observed
increase in ␴ is potentially related to the increase in ␮. Therefore, in order to compare the variation
without the interference of ␮, another very important parameter, CV, was used to evaluate the
variation of the data sets in this study. CV is a statistical measure of the dispersion of data points in
a data series around the mean and represents the ratio of the standard deviation to the mean 共CV
= ␴ / ␮兲. This measure is a useful parameter for comparing the degree of variation from one data
series to another, even if the means are drastically different from each other. From Table 5, it can
be seen that the variation in CV is very high in the first 30 min and is drastically reduced to the
lowest level from 1 to 3 days. There is a slight up-trend in CV at 7 days. The CV trend is also
graphically shown in Fig. 2.
In general, the variation in EM is slightly lower than the variation observed with IM. This is largely
due to the exclusion of heat release during the EM period. The heat release in the early minutes is highly
variable; hence, its exclusion helps improve the statistical variances.

Statistical Data Comparison between Calorimeter and ASTM C186-05 Methods

The statistical comparison in Table 5 shows that the published ␴ in ASTM C186-05 is 14.8 kJ/kg for the
tests conducted within the laboratory and 16.8 kJ/kg for the tests conducted between laboratories. In our
calorimeter testing, the ␴ obtained within the laboratory are 9.3 kJ/kg for the IM method and 9.1 kJ/kg for
the EM method. Generally speaking, calorimeter results based on either the EM or IM procedure showed
reduced statistical variation comparing with the heat of solution method of ASTM Standard C186-05.

FIG. 2—IM and EM statistical trend comparison.

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 WANG ET AL. ON ISOTHERMAL CONDUCTION CALORIMETRIC METHOD 7

TABLE 7—HoH and compressive strength comparison.

HoH 共kJ/kg兲

Strength 共MPa兲 Calorimeter

Cement ID 1 day 3 days 7 days 28 days 1 day 3 days 7 days ASTM C186-05
C-01 14.8 27.4 32.3 41.1 187 276 322 277
C-02 16.2 28.0 34.8 45.0 204 289 348 314
C-03 16.6 25.7 32.8 46.3 183 275 337 307
C-04 18.0 29.2 39.2 47.0 197 301 368 317
C-05 13.9 25.0 32.8 47.9 188 268 326 288
C-06 15.7 24.4 30.8 38.8 192 272 347 287
C-07 18.6 28.3 34.1 42.1 205 293 356 318
C-08 21.7 30.5 37.5 45.2 226 326 372 277
C-09 17.0 27.2 34.1 46.0 201 289 372 286
C-10 15.9 27.9 35.8 46.5 201 293 360 300
C-11 16.3 29.0 37.4 44.8 213 310 364 269
C-12 10.5 23.5 31.5 45.6 180 272 335 277
C-13 15.4 24.0 32.5 44.6 192 272 343 313
C-14 17.1 28.5 37.4 49.6 201 276 310 268
C-15 12.1 23.4 29.3 38.8 188 259 293 279
C-16 10.8 18.2 25.6 38.1 176 243 301 272
C-17 11.8 25.6 32.8 46.0 188 280 326 274

Calorimetric Test Application and Comparison with ASTM C186-05 Method

After the groundwork in the previous sections, an extensive test program was conducted to evaluate the
effectiveness of calorimetric method for determining the cement HoH. A total of 17 cements were tested
in this program. The calorimeter testing condition was set at 23° C, and the w / c ratio was fixed at 0.50.
The EM procedure with 30 s premixing and 75 s intense mixing time was used. At the same time, the
HoHs of the 17 cement samples were determined using the ASTM C186-05 test method. Compressive
strength of these cements was tested in accordance with the ASTM C109-05 method. HoH values obtained
from both calorimeter and the ASTM C186-05 methods, along with the strength results at various ages, are
summarized in Table 7.
It is noticed that the HoH values from calorimeter tests are higher than the HoH values from ASTM
C186-05 tests at the corresponding age of 7 days. The difference in HoH values is not understood at this
point. However, it is important to point out that the calibration process of the calorimeter could potentially
affect the heat value. The calorimeter instrument used in this work was calibrated in the absence of cement
material. Strictly speaking, calorimeter equipment should be calibrated with a standard cement with known
“true” HoH value to ensure that the registered heat value is the “actual” representation of hydration heat
release.
As previously stated, when cement is mixed with water, HoH represents the progress of cement
hydration, which in turn dictates cement strength development. The relationship of HoH of cement and
strength development has been studied by many scientists and engineers. It is generally agreed that a
relatively strong relationship exists between HoH and strength development 关6,7兴. The objective to estab-
lish a strength-HoH relationship in this paper is primarily focused on the comparison between strength-
HoH 共calorimeter兲 and strength-HoH 共ASTM C186-05兲. The degree of relative relationship is used to
assess the relative reliability of HoH obtained from the calorimeter and ASTM C186-05 methods.
The 1-, 3-, and 7-day strengths were used for establishing correlation with 1-, 3-, and 7-day HoHs
obtained from the calorimeter test. For discussion purposes, the 7-day strength was used to establish
correlation with the HoH value obtained from the ASTM C186-05 test.
Figure 3共a兲 shows the relationship of 1-day strength and 1-day HoH value obtained from the calorim-
eter test; a relatively strong relationship exists between the strength and HoH. This strong correlation
between the strength and HoH is also shown at 3 days 共Fig. 3共b兲兲. The R2 at 3 days is 0.7938, the highest
among the tested ages. Figure 3共c兲 shows the comparison of 7-day strength and 7-day HoH obtained from
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 8 JOURNAL OF ASTM INTERNATIONAL

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FIG. 3—Relationship of compressive strength and HoH.

the calorimeter and from ASTM Standard C186-05 test methods, respectively. The 7-day HoH determined
with the calorimeter shows better correlation with 7-day strength than the HoH obtained by ASTM
Standard C186-05 test method.
The stronger relationship of the strength and HoH indicates that the calorimeter method is a better
method for HoH measurement of cement than ASTM C186-05 method. This may be attributed to the
following:
• much simpler operational process with less operational related errors and variations;
• direct measurement of hydration heat flow;
• better mixing process;
• independent of the type of cement and cement physical properties;
• sensitive digital data acquisition system; and
• better instrumentation technology.

Conclusions and Recommendations

共1兲 There is a stronger relationship between strength and the HoH measured from the calorimeter
method. This suggests that calorimeter test is a better method for HoH measurement of cement
than ASTM C186-05 method.
共2兲 3-day heat release value from the calorimeter test appeared to have the lowest variation, and
therefore it is recommended to be used as the limit of the HoH testing period.
共3兲 Although both are acceptable, HoH results from the EM method showed smaller variation than
those from the IM method. Therefore, the EM method is preferably used as a standard mixing
procedure.
共4兲 There is an urgent need for a “round-robin” test to further evaluate the calorimeter test procedure
and to verify the statistical variations in the test results. Standard cement may be recommended for
users to calibrate the calorimeter instruments.

References

关1兴 ASTM C150-07, 2007, “Standard Specification for Portland Cement,” Annual Book of ASTM Stan-
dards, Vol. 04.01, ASTM International, West Conshohocken, PA, pp. 1–8.
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 WANG ET AL. ON ISOTHERMAL CONDUCTION CALORIMETRIC METHOD 9

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