New Understanding of Cement Hydration Mechanism

through Electrical Resistivity Measurement

and Microstructure Investigations
Lianzhen Xiao1 and Zongjin Li2
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Abstract: The new understanding for the hydration mechanism of cement has been achieved based on the noncontact electrical resistivity
measurement. The cement hydration process is divided into dissolution, dynamic balance, setting, hardening, and hardening deceleration
stages according to the characteristic points on the electrical resistivity development curve ␳共t兲 − t and the differential curve d␳共t兲 / dt − t.
The microstructure analysis corresponding to each hydration stage is conducted with scanning electron microscope, x-ray diffraction,
differential thermal analysis, and Fourier transform infrared spectroscopy techniques. This study provides the theoretical foundation for
understanding the relationship between setting behavior, hardening properties, and resistivity development.
DOI: 10.1061/共ASCE兲0899-1561共2009兲21:8共368兲
CE Database subject headings: Hydration; Microstructures; Electrical resistivity; Measurement; Cement.

Introduction fore, the electrical conductivity or resistivity of a cement mixture

Cement hydration is a complex physical–chemical process. Dur-
ing the process, a cement–water mixture is changed from a fluid
state to a porous solid state. An adequate understanding of the
mechanism of cement hydration is necessary for a full apprecia-
tion of cement concrete properties.
The cement hydration process was traditionally studied using
the calorimetric method. The hydration stages were identified by
the heat liberation measurement and the hydration mechanism
was explained based on the heat evolution. Some limitations
共Gartner et al. 2002兲 were pointed out, such as the liberated heat
content, which was neither simply proportional to the degree of
cement hydration nor to the development of physical properties.
This method only provides an approximation in understanding
cement hydration and leaves space for cement scientists and en-
gineers to explore more accurate ways to understand the process.
Chemically, cement hydration involves ion dissolution and
new chemical compound formation. Physically, cement hydration
involves microstructure formation and a porosity decrease pro-
cess. When water is added into cement, the soluble ions in the
cement dissolve into water. The ions in the pore solution are
conductive and can form an electrical current under certain elec-
trical fields. The conductivity of a cement mix depends mainly on
the concentration of the ion solution and microstructure, espe-
cially porosity and pore connectivity of the cement paste. There-
1 resistivity curve; and 共3兲 to correlate the electrical resistivity de-
Doctor, Dept. of Civil Engineering, The Hong Kong Univ. of Science
and Technology, Clear Water Bay, Kowloon, Hong Kong. E-mail:
xiaolz@gmail.com
2
Professor, Dept. of Civil Engineering, The Hong Kong Univ. of Sci-
ence and Technology, Clear Water Bay, Kowloon, Hong Kong 共corre-
sponding author兲. E-mail: zongjin@ust.hk
Note. This manuscript was submitted on January 18, 2007; approved
on January 22, 2009; published online on July 15, 2009. Discussion pe-
riod open until January 1, 2010; separate discussions must be submitted
for individual papers. This paper is part of the Journal of Materials in
Civil Engineering, Vol. 21, No. 8, August 1, 2009. ©ASCE, ISSN 0899-
1561/2009/8-368–373/$25.00.
can be used to interpret the cement hydration process.
Taylor and Arulanadan 共1974兲, Christensen et al. 共1994兲,
Tashiro et al. 共1994兲, McCarter et al. 共1981兲, Gu et al. 共1985兲, and
McCarter et al. 共2003兲 observed the electrical responses of the
cementitious hydration systems using an alternating current im-
pedance spectroscopy. However, since the experiments were car-
ried out with electrodes, the accuracy and consistency of the test
results were largely affected by contact problems, such as the
interface gap between the electrodes and shrunken cement paste
mixes.
In this paper, the cement hydration process is monitored with
an advanced monitoring technique: noncontact electrical resistiv-
ity measurement (using a process patented by Z. Li and W. Li
关“Contactless, transformer-based measurement of the resistivity
of materials,” U.S. Patent No. 6,639,401 共2003兲兴; see also Li et al.
2003; and Wei and Li 2005). The technique adopts a transformer
principle and has no electrodes in the setup, thus it completely
eliminates the contact problems and can provide more reliable
results. For the purpose of obtaining a clear understanding of the
relationship between the electrical resistivity development and the
hydration process, microstructure analysis is conducted and the
results are correlated to each stage of the hydration process.
In summary, the scope of the current investigation is 共1兲 to
obtain the electrical resistivity of cement paste using a noncon-
tacting electrical resistivity measurement; 共2兲 to identify hydra-
tion stages according to the characteristic points on the electrical
velopment to the hydration stages with microstructure analysis.
Experimental Methods and Sample Preparations
The experimental setup of a noncontact resistivity measurement is
shown in Fig. 1. The principle is described in Li et al. 共2003兲.
Ordinary Portland cement 共OPC兲 was used in the experiments.
Cement paste with a water/cement ratio of 0.4 was used in the
resistivity measurement and microstructure investigations. The

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J. Mater. Civ. Eng. 2009.21:368-373.

 Current meter

Electrical resistivity rate (ohm.m/h)

I 0.3

Electrical resistivity (ohm.m)

I II III IV P2 V
Transformer
4 0.2
V
P1
2 0.1
(Primary coil)
M
L
Sample cast in the mould
0 0
(Second coil) 2 4 6 8 10 12 14 16 18 20 22 24
time (hours)
Fig. 1. Electrical resistivity measurement setup
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Mixing M L P1 P2

cement paste was mixed for 4 min and cast in a ring-shaped mold 0 tm tL tp1 t p2 hydration time

to measure the electrical resistivity with time. The measurements Setting time
were taken at intervals of 1 min for a 24 h period, under an am- Electrical resistivity response (ASTM C191)
bient temperature of 20⫾ 2 ° C. The hydrated cement samples tm tL t p1 t p2
initial final
t ini t fin
were prepared by stopping hydration using acetone at designated
ages and the samples were then dried in a vacuum oven for 24 h 0.73h 3.5h 6.7h 12.8h 3.75h 6.28h
for microstructure investigations.
Each sample for Fourier transform infrared spectroscopy
共FTIR兲 spectral observation was ground with potassium bromide
in an agate mortar to produce a homogeneous mixture and a thin 2
slice of the mixture was made by a pressing procedure. The in-
frared spectra were recorded using a FTS 6000 spectrometer 共Bio-
Rad, Calif.兲 in the range of 400– 4000 cm−1. M
L

Experimental Results 0 2 4 6

Characteristic Points on the Electrical Resistivity
Development Curves
A typical electrical resistivity development curve with time
关 ␳ 共t兲 − t兴 and its differential curve 关d␳共t兲 / dt − t兴, which represents
the rate of resistivity development, are shown in Fig. 2. The mini-
mum point M and the level point L, which is in the end of a
relatively flat region after Point M, are marked on the curve
␳共t兲 − t. Peak Points P1 and P2 are marked on the curve
d␳共t兲 / dt − t. The times at which the characteristic points occurred
and the paste setting time are listed in the table in Fig. 2. Accord-
ing to the characteristic points, the hydration process is divided
into five stages: dissolution, dynamic balance, setting, hardening,
and hardening deceleration.
Microstructure Observations
To investigate the cement hydration mechanism, the microstruc-
ture investigations of the hydrated samples for the designated
ages, corresponding to the characteristic point occurrences, have
been conducted using a scanning electron microscope 共SEM兲 and
X-ray diffraction 共XRD兲, differential thermal analysis 共DTA兲, and
FTIR; the results are shown in Figs. 3–5, respectively.
The XRD patterns in Fig. 3 show the presence of crystalline
substances in anhydrous cement and in the hydrated samples at
the specified ages. At a very early age of hydration, the ettringite
共AFt兲 phase started to form with the consumption of sulfate,
which was detected in the sample at 0.73 h. The intensity of the
AFt peaks decreased and monosulfate 共AFm兲 appeared, as shown
in the hydrated sample for 12.8 h in comparison with that in the
6.7 h sample. The amorphous hydrates C–S–H cannot be detected
by the XRD technique. The relative density of the peaks of the
(Point L is the transition point from linear to curved shape)
Fig. 2. Electrical resistivity development and the rate in resistivity of
the cement paste during 24 h
crystal calcium hydroxide 共CH兲 became significant with time due
to the increase of CH content in the hydrated samples.
The DTA was performed for characterization of the hydration
products and the quantification of CH in the samples, as shown in
Fig. 4. The existence of four endothermic peaks was shown in the
detected temperature range. Peaks 1 and 2, located at 85 and
128° C, mainly characterize gypsum. The shift of the first peak
from 85° C to around 92° C and the reduced intensity of the sec-
ond peak with hydration time indicate that gypsum was consumed
and the AFt formation was at the expense of the gypsum peaks.
The third peak observed at about 165° C represents the decompo-
sition of AFm in the samples hydrated for 12.8 and 24 h. The
fourth peak at 465– 470° C is due to the CH. The shifts of the CH
peaks to the right with an increase in the ages shows that the CH
crystalline becomes denser and larger and an increase in tempera-
ture was needed for the decomposition of the CH crystalline. The
index of the formed CH content, which was estimated by deter-
mining the endothermic area of the CH peaks as an indication of
the hydration product contents, is marked in Fig. 4.
The FTIR spectra of the samples at the ages, as shown in Fig.
5, provide information on chemical bonding. CH gives a peak at
3643 cm−1. AFt has a strong peak at 3422 cm−1 and a weaker one
at 3545 cm−1, marked as A in Fig. 5. AFm has bands at 3260,
3333, 3402, 3458, and 3527 cm−1, which were separated from a
broadband of 3200– 3600 cm−1; the broadband was centered at
3402 cm−1, marked as B in Fig. 5.

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J. Mater. Civ. Eng. 2009.21:368-373.

 peak1 peak2 peak3 peak4

¦ ¤H = 9 . 5 5 J / g
a n h y d ro u s
cem ent
¦ ¤H = 1 1 . 9 4 J / g
0 .7 3 h
¦ ¤H = 1 4 . 5 2 J / g
3h
¦ ¤H = 2 2 . 7 6 J / g
6 .7 h
¦ ¤H = 7 6 .9 8 J / g
1 2 .8 h
A F m fo rm e d
g y p su m co n su m ed ¦ ¤H = 1 0 2 . 4 1 J / g
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24h

0 100 200 300 400 500 600

T e m p e r a tu r e ( oC )

Fig. 4. DTA results of cement and the hydrated pastes at the ages of
0.73, 3, 6.7, 12.8, and 24 h

The bands ␷3 共SiO4兲 and ␷4 共SiO4兲 in the anhydrous cement

are located at 924 and 523 cm−1. The hydration of the silicate
phases causes a shift in the band ␷3 共SiO4兲 from 924 to 978 cm−1
during 24 h. There was an obvious shift occurrence in the band ␷3
共SiO4兲 from 6.7 to 12.8 h, corresponding to a new Si–O bonding
formation during the period. The shift is likewise observed in the
band ␷4 共SiO4兲, from a wave number of 523 cm−1 in the anhy-
drous cement to a lower wave number of 518 cm−1 in the hy-
drated sample at 0.73 h, characterizing C3S initial hydration.

Discussions

Microstructure investigations can help one to understand the re-

lationship between electrical resistivity development and the hy-
dration process. The correlation of the microstructure analysis to
the hydration stages is described as follows.

Dissolution Stage „I…

From the start of mixing to Point M 共0.73 h兲, the resistivity ␳共t兲
of the mixture deceases. When cement is mixed with water, the
mobile ions in cement, such as potassium 共K+兲, sodium 共Na+兲,
calcium 共Ca2+兲, hydroxyl ions 共OH−兲, and sulfate 共SO42−兲, dis-
solve into the water and thereby form an electrolytical solution
共Taylor 1997兲. The dissolving process of the ions causes the re-
sistivity to decrease in the hydration system.
It is observed that there is an immediate increase in resistivity
right after Point M, and it is inferred that some hydration products
have been formed. The SEM, XRD, DTA, and FTIR results are
used to verify this point.
C3A is the most active chemical compound in cement, and it
Fig. 3. Results of cement and the hydrated pastes at the ages of 0.73,
reacts with sulfate ions in the solution dissolved from the gypsum
3, 6.7, 12.8, and 24 h from SEM and XRD
attached on the cement grain surface, as shown in Fig. 3共a兲. The
hydration product, hexagonal crystal AFt—as short rods—is

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J. Mater. Civ. Eng. 2009.21:368-373.

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Fig. 5. FTIR spectra of anhydrous cement and the hydrated samples at the ages of 0.73, 3, 6.7, 12.8, 24 h

formed directly on the surface of the cement grains and was ob-
served in the SEM picture, as shown in Fig. 3共b兲. The picture
taken at a magnification of 5,000 shows that the AFt crystals are
not evenly distributed on the cement surface; one possibility is
that the AFt formed just on the surface of C3A.
When a certain supersaturation—with respect to CH—is
reached, the CH precipitates from the solution, as detected by the
DTA technique in the hydrated sample for 0.73 h, and is shown in
Fig. 4. The DTA results show that the index of the CH 共peak 4兲
content in the hydrated sample for 0.73 h 共⌬H = 11.94 J / g兲 is
larger than that of the CH formed from free lime by chemisorbed
water in anhydrous cement 共⌬H = 9.55 J / g兲 during storage, indi-
cating that new CH is formed during the period.
The shift of the band ␯4 SiO4 during 0.73 h indicates C3S
hydration occurred as mentioned earlier. It has been reported that
a gelatinous layer on the surface of the cement was observed in
the undried specimen soon after mixing by using an environmen-
tal cell and was identified as an amorphous colloidal product
共Ménétrier et al. 1979; Jennings and Pratt 1980兲.
Therefore, during this period, the resistivity decrease implies
that the process is dominated by the ion dissolution and identified
as the dissolution stage. There are also chemical reaction occur-
rences. The formation of hydration products AFt, a gelatinous
substance and CH consumed ions in the solution and also caused
a decreasing trend in the porosity. This led to the resistivity in-
crease from point M and ended the dissolution stage.

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 Dynamic Balance Stage „II…
From Point M 共0.73 h兲 to point L 共3.5 h兲, the electrical resistivity
slightly increases, by approximately 0.03 ⍀ m. Point L is the tran-
sition point from linear to a curved shape. The mixture is rela-
tively inactive which refers to a competitive balance between the
ion dissolution and CH, as well as the precipitation of other hy-
drates, and is identified as a dynamic balance stage.
The C–S–H formation can be observed in the dried sample as
small acicular shapes 共diamond Type I, fibrillar morphology兲
among AFt rods in the sample hydrated for 3 h, from the SEM
picture shown in Fig. 3共c兲. During this stage, the mix retains its
fluidity. The DTA results show that the CH content index ⌬H
increases from 11.94 to 14.52 J / g, and the FTIR show that bands
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␯3 共SiO4兲 peak shift from 922 to 925, which confirms C–S–H
formation during this period.
Setting Stage „III…
From point L 共3.5 h兲 to point P1 共6.7 h兲, the resistivity signifi-
cantly increases, indicating a rapid change in the microstructure
during this period. It can be seen in the sample hydrated for 6.7 h,
as shown in Fig. 3共d兲, that a great amount of C–S–H is formed in
bundles compared with 3 h, and the cement particles are sur-
rounded by the C–S–H bundles. The solid phases in the hydration
system are closely connected to each other, resulting in a perco-
lation of the solid phase, i.e., a setting in process. The initial
setting time and the final setting time of the paste are 3.75 and
6.28 h, respectively, obtained by a Vicat needle penetration. The
inital setting time is close to the end of the dynamic balance
period, and the final setting time is close to the time of the point
P1 occurrence. Thus this period is identified as the setting stage.
The XRD result at 6.7 h shows a significant increase of the CH
peak intensity.
Therefore, the setting of cement paste appears to be a conse-
quence of C3S hydration and the formation of sufficient C–S–H
and CH hydrates. The C3S hydration dominates the setting period
and the C–S–H formations lead to normal cement paste set.
Hardening Stage „IV…
From Point P1 共6.7 h兲 to Point P2 共12.8 h兲, the resistivity con-
tinuously increases at a temporarily reduced rate and then the rate
increases again. When the hydration proceeds to 12.8 h, gypsum
Table 1. Stages of the Hydration Process
Hydration stage Kinetics of hydration
I. Dissolution Ion dissolution dominating
共mixing to Point M兲
II. Dynamic balance A competition process of the
共Points M to L兲 dissolution precipitation
III. Setting The formation of hydration product
共Points L to P1兲 C–S–H dominating
IV. Hardening Continuous formation of hydration products,
共Points P1 to P2兲 large increase in the volume of solids
V. Hardening deceleration Chemical reaction slows down,
共Point P2 onwards兲 diffusion control
372 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / AUGUST 2009
J. Mater. Civ. Eng. 2009.21:368-373.
is significantly consumed, the AFt peak disappears, and AFm ap-
pears in the XRD pattern in Fig. 3共e兲. This indicates the transfor-
mation of phase AFt to phase AFm occurring during the period of
6.7– 12.8 h. When SO42− is sufficient in the pore solution, the AFt
forms and remains stable. After SO42− is consumed and no suffi-
cient SO42− reaches the C3A, the AFt is transformed into AFm.
The DTA results at 6.7 and 12.8 h, as shown in Fig. 4, confirm the
phase transformation occurrence by the disappearance of the gyp-
sum peak 共Peak 2兲 and the appearance of the AFm peak 共Peak 3兲
at 12.8 h. Additionally, the FTIR pattern, as shown in Fig. 5, from
6.7 to 12.8 h, and the shift of the band SO42− from a wave num-
ber of 3,422 to 3,402 supports the observation. This transforma-
tion process may follow one of the two chemical reactions as
shown in Eqs. 共1兲 and 共2兲. The reaction in Eq. 共1兲 共Abo El-Enein
et al. 1995兲 leads to an increasing trend in ion concentration due
to the releasing of SO42− and Ca2+ and a decreasing trend in the
solid volume fraction due to phase AFm possessing a higher den-
sity than phase AFt. The reaction in Eq. 共2兲 共Hewlett 1998兲 leads
to the latter effect only. No matter which way takes place, the
consequence is that there is a decreasing trend in resistivity. How-
ever, the C3S hydration continuously progresses and the forma-
tions of hydrates C–S–H largely increase the solid phase in the
hydration system, which compensates the resistivity decreasing
trend caused by the phase transformation. The phase transforma-
tion slows down the rate of resistivity development, however, it
does not change the increasing trend of the resistivity. This cor-
responds to the resistivity increase at a lowered rate 关d␳共t兲 / dt兴.
When the balance between the phase transformation and AFt for-
mation process is achieved—by releasing and consuming ions of
Ca2+ and SO42−,—the factors leading to the d␳共t兲 / dt decrease
become minor or disappear. Eventually, a larger increase in
C–S–H and the other hydrate contents dominates the resistivity
development and the rate 关d␳共t兲 / dt兴 increases again
C3A · 3CaSO4 · 32H2O共AFt兲 → C3A · CaSO4 · 12H2O共AFm兲
+ 2CaSO4 共1兲
C3A · 3CaSO4 · 32H2O共AFt兲 + 2C3A + 4H2O
→ C3A · CaSO4 · 12H2O共AFm兲 共2兲
When gypsum is insufficient, there is also a trend for forming
hexagonal plate C4AH19, as shown in Fig. 3共e兲 共Hewlett. 1998兲,
which belongs to the broad group of AFm. This process leads to a
Main chemical phenomena Chemical reaction
Initial rapid chemical reaction C3A + 3共CS̄H2兲 + 26H → C6AS3H32
of C3A
CH nucleation Ca2+ + OH− → Ca共 O H兲2
Chemical reaction control of C3S C3S + 11H → C3S2H8 + 3CH
C3S hydration; phase transfer C3S + 11H → C3S2H8 + 3CH
from AFt to AFm 2C2S + 9H → C3S2H8 + C H
C6AS̄3H32 → C4AS̄H12 + 2CaSO4
C6AS̄3H32 + 2C3A + 4H → 3C4AS̄H12
The second reaction of C3A; C3S C3A + 3共CS̄H2兲 + 26H → C6AS3H32
and other components of hydration
C3S + 11H → C3S2H8 + 3CH
2C2S + 9H → C3S2H8 + CH
 similar effect on electrical resistivity development to the forma-
tion of phase AFm. The SEM picture shows that C–S–H becomes
denser at 12.8 h compared with that at 6.7 h. The FTIR spectra of
the samples at 6.7 and 12.8 h show new C–S–H hydrates forma-
tion, as described earlier. With the thickness of hydration products
increasing, the solution in the pores must go through the thick
layer of the products for further hydration and the rate of the
chemical reactions then decreases, which is corresponding to a
decreased rate of d␳共t兲 / dt − t from Point P2.
Hardening Deceleration Stage „V…
After point P2 共from 12.8 h onwards兲, the resistivity increases at
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a decreasing rate. The decreasing rate d␳共t兲 / dt describes a slow-
down in the chemical reaction rate, and the process is controlled
by ion diffusion, with the thickness of the hydrates on the cement
particle surface 共Mindess et al. 2003兲.
The hydration proceeds up to the age of 24 h, shown in Fig.
3共f兲, and the C–S–H bundles and long rods of AFt intersect each
other to form solid networking for strength gain. Meanwhile the
free water space decreases, porosity decreases, and tortuosity in-
creases for conduction paths. Hydration product contents increase
with the hydration time can also be represented by the increase in
CH hydrate content as the endothermic heat of CH in Fig. 4. The
stages of the hydration process are summarized in Table 1.
From a macro-point-of-view, fresh concrete changes from the
fluid to the solid state. From the micro-point-of-view, there are a
series of the physical and chemical reactions occurring and the
consequence leads to microstructure formation. Microstructure
formation and concrete property time-dependence are essentially
correlated. Electrical resistivity can dynamically record the mi-
crostructure changing process and related concrete properties.
Therefore, the electrical resistivity response ␳共t兲 can provide an
indication of setting behavior and strength development as a non-
destructive test method.
Conclusions
The following conclusions can be drawn from the current study:
1. The hydration process is reclassified as dissolution, dynamic
balance, setting, hardening, and hardening deceleration
stages based on the electrical resistivity measurement.
2. During the dissolution period, the ion dissolving process
dominates the resistivity development. The formation of AFt,
CH, and a gelatinous substance leads to an increase in resis-
tivity and an end to the dissolution stage.
3. The slight increase of the resistivity development marks a
competition process between the ion dissolving and the solid
phase nucleation in the hydration system. The significant in-
crease of the resistivity signals the start of setting the stage
due to the hydration products reaching an intersection.
3. The formation of C–S–H products dominates the set stage,
and the first peak on the differential the curve approximately
identifies the final setting occurrence. It has practical signifi-
cance for separating setting behavior from a continuous hy-
dration process and identifying the setting stage in obtaining
information of engineering parameters, such as setting time
and strength gain.
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J. Mater. Civ. Eng. 2009.21:368-373.
5. After setting, the hydration process enters the hardening
stage. The temporally decreasing rate on the resistivity dif-
ferential curve reflects the phase transformation from AFt to
AFm.
6. More and denser hydration products form a solid network for
an increase in the load carrying capacity of the cement
mixture.
Acknowledgments
The support from China 973 project under 2009CB623200 and
the Hong Kong Research Grant Council under 616008 is grate-
fully acknowledged.
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