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Determination of Concrete Setting Time Using Electrical Resistivity


Measurement

Article  in  Journal of Materials in Civil Engineering · May 2007


DOI: 10.1061/(ASCE)0899-1561(2007)19:5(423)

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Determination of Concrete Setting Time Using Electrical
Resistivity Measurement
Zongjin Li1; Lianzhen Xiao, Ph.D.2; and Xiaosheng Wei3

Abstract: The hydration process of fresh concretes with different proportions was studied using electrical resistivity measurement. The
minimum point 共Pm兲 and the transition point 共Pt兲 were identified on the electrical resistivity development curves. The time tm at which Pm
Downloaded from ascelibrary.org by New York University on 02/12/15. Copyright ASCE. For personal use only; all rights reserved.

occurred, represented the time when the curve dropped to a minimum and before increasing as a result of the onset of hydration. The time
tt at which Pt occurred, marked the time when the kinetics of hydration transition changed from the setting to the hardening stage. To
evaluate the significance of tm and tt in terms of the setting process, they were compared to the initial setting time 共ti兲 and final setting time
共t f 兲 measured with the traditional penetration resistance method. The quantitative relationships between the setting time of concrete and
the electrical resistivity critical points were developed. The equations can be used to estimate the setting times of concrete as an alternative
method.
DOI: 10.1061/共ASCE兲0899-1561共2007兲19:5共423兲
CE Database subject headings: Concrete; Penetration resistance; Measurement; Electrical resistivity.

Introduction regular intervals. Moreover, the test results can be largely affected
by the skill of operators. For these reasons, there have been at-
Concrete setting time is a crucial parameter for construction tempts to use alternative techniques, such as the impact-echo
progress and concrete quality control. When the setting time is method 共Pessiki and Carino 1988兲 and ultrasonic measurement
known, the times of mixing, transporting, casting and finishing 共Ozturk et al. 1999; Subramaniam et al. 2005; Lee et al. 2004;
can be regulated and the effectiveness of various set-controlling Voigt et al. 2005兲 to determine the setting time for concretes. The
admixtures can be decided. Typically, the initial and final setting impact-echo method defines the setting time of concrete as the
time of concrete are measured by the penetration method that has condition when the wave velocity begins to increase. However, it
been standardized in ASTM C 403 共1995兲. ASTM C 403 defines is hard to be applied to early age concrete and is thus not practi-
two points as the initial setting time and the final setting time, cal. The ultrasonic method is based on the generation, transmis-
corresponding approximately to the point at which the concrete sion and reflection of mechanical waves in concrete. Preliminary
will no longer be plastic under compaction, and the concrete studies have shown good correlation between the measured wave
strength has increased to a value gain of about 0.7 MPa, respec- reflection factor and the hydration process. Electrical resistivity
tively. The initial and final setting of concrete are determined by measurement is another nondestructive technique for monitoring
the times at which the penetration resistance reaches 3.5 and the setting and hardening process of fresh concrete 共McCarter et
27.6 MPa, when a designated needle penetrates 25.4 mm into the al. 2003; Gu et al. 1994b; Gu and Beaudoin 1997; Tumidajski
mortar, which has been sieved from the fresh concrete. It is hard 2005; Li et al. 2003; Wei and Li 2005兲, and has the potential to
work to remove the mortar fraction through a 4.75 mm sieve from determine the setting time of concrete. The setting time of cement
fresh concrete, especially for concretes with poor fluidity. Addi- was studied with electrodes as early as the 1930s 共Michelsen
tionally, for concrete having a retarder incorporated it probably 1933兲. The retardation effect of setting due to the incorporation of
takes an operator more than 10 h to finish the test, working at superplasticizers, using impedance spectros, was observed by Gu
and Torrents 共Gu et al. 1994a; Torrents et al. 1998兲. The results
1 obtained from these alternative methods for the interpretation of
Professor, Dept. of Civil Engineering, The Hong Kong Univ. of
Science and Technology, Clear Water Bay, Kowloon, Hong Kong. the setting behavior mentioned above, were compared with the
E-mail: zongjin@ust.hk conventional penetration method. However, no quantitative rela-
2
Visiting Scholar, Dept. of Civil Engineering, The Hong Kong Univ. tionship between the ultrasonic response or electrical response
of Science and Technology, Clear Water Bay, Kowloon, Hong Kong. and conventional setting time was proposed.
E-mail: xiaolz@ust.hk In this paper, the noncontacting electrical resistivity response
3
Associate Professor, Dept. of Civil Engineering, Huazhong Univ. of is used to determine the setting time of concrete, based on mini-
Science and Technology, 1037 Luoyu Rd., Wuhan, 430074, China. mum point 共Pm兲 and the transition point 共Pt兲 of a resistivity curve.
E-mail: weixiaosheng@gmail.com Meanwhile, the penetration resistance is measured as specified in
Note. Associate Editor: Carl Liu. Discussion open until October 1, ASTM C 403 as a parallel investigation. From comparison and
2007. Separate discussions must be submitted for individual papers. To
regression, quantified setting time equations are proposed as a
extend the closing date by one month, a written request must be filed with
the ASCE Managing Editor. The manuscript for this paper was submitted function of the critical points 共tm and tt兲 to determine the initial
for review and possible publication on September 13, 2005; approved on setting time and final setting time of concrete.
March 28, 2006. This paper is part of the Journal of Materials in Civil In summary, the scope of the current investigation is: 共1兲 to
Engineering, Vol. 19, No. 5, May 1, 2007. ©ASCE, ISSN 0899-1561/ measure concrete electrical resistivity using a noncontacting elec-
2007/5-423–427/$25.00. trical resistivity device; 共2兲 to obtain the critical points on the

JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2007 / 423

J. Mater. Civ. Eng. 2007.19:423-427.


Li and W. Li, “Contactless, transformer-based measurment of the
resistivity of materials,” U.S. Patent No. 6,639,401 共2003兲兴, in
which the transformer principle was adopted. As shown in Fig. 1,
the generator produced an alternating current at a frequency of
1,000 Hz. When an input voltage was applied to the primary coil,
a toroidal voltage V was generated in the ring concrete sample
that acted as the secondary coil of the transformer. The toroidal
current, I could be measured by a leakage current meter. The
resistivity of the concrete was calculated through V and I based
on Ohm’s law. There were no electrodes in the apparatus such that
the contact resistance problems between the electrodes and the
concrete sample were eliminated.
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Setting Time
The setting time of concrete was obtained by means of penetra-
tion resistance measurements, in accordance with ASTM C 403.

Preparing the Mixes and Experimental Procedures


Type I Portland cement and fly ash cement were used in Mixes
1–10 and Mix 11, respectively, as the cementitious materials.
Table 1 shows the mix proportions of the eleven concretes used in
the experiments. The water to cement ratio 共W / C兲 ranged from
0.3 to 0.5, with Mixes 1–8 having a W / C of 0.3, Mix 9 with a
W / C of 0.5 and Mixes 10 and 11 having a W / C of 0.4. A
naphthalene-based superplasticizer 共sp1兲 was incorporated in
Mixes 2–4, and a polycarboxylate superplasticizer 共sp2兲 was used
in Mixes 5–7, CaCl2 was used in Mix 8 as an accelerator.
Fig. 1. Determination of the relationship for resistivity response and
Each sample was mixed and cast in a mold to measure the
setting time
electrical resistivity with time. Measurements were taken at inter-
vals of 1 min for 24 h, under an ambient temperature of 20± 2 ° C.
measured electrical resistivity curves; 共3兲 to measure the initial The mixtures for measuring the setting time were prepared in the
setting time and final setting by penetration resistance 共PR兲, and same proportions as shown in Table 1, excluding the coarse
共4兲 to develop a relation between the electrical resistivity critical aggregate.
points and the setting times. The flowchart of the determination of
the relationship for the resistivity response and setting time is
shown in Fig. 1.
Experimental Results and Discussions

Test Method Minimum Point and Transition Point on the Bulk


Electrical Resistivity Curves
Electrical Resistivity Apparatus and Principle
In the investigation, eleven mixes, involving concretes with dif-
The electrical resistivity of concrete was measured by a noncon- ferent W / C’s, different cement types or containing admixtures,
tacting electrical resistivity apparatus that has been patented 关Z. have been tested. Three examples of the bulk electrical resistivity

Table 1. Mix Proportions of Concrete per Cubic Meter 共kg/ m3兲


Coarse
Mix number Name Water Cement Sand aggregate Sp1 Sp2 CaCl2
1 Control 165 550 602 1,070
2 Sp1-0.6 165 550 602 1,070 3.3
3 Sp1-0.8 165 550 602 1,070 4.4
4 Sp1-1 165 550 602 1,070 5.5
5 Sp2-0.15 165 550 602 1,070 0.825
6 Sp2-0.25 165 550 602 1,070 1.375
7 Sp2-0.35 165 550 602 1,070 1.925
8 Accelerator 165 550 602 1,070 11
9 WC-0.5 208 415 602 1,070
10 WC-0.4 190 475 602 1,070
11 WC-0.4 190 475 602 1,070
FA cement

424 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2007

J. Mater. Civ. Eng. 2007.19:423-427.


Table 2. Times of Occurrence of Critical Points in the Resistivity
Response and the Setting Times of Concrete
Resistivity response Setting time 共ASTM C 403兲

Point Pm Point Pt Initial Final


Mix 共tm兲 共tt兲 共ti兲 共t f 兲
number Name 共h兲 共h兲 共h兲 共h兲
1 Control 0.33 5.08 3.5 4.73
2 Sp1-0.6 0.70 8.35 5.82 8.02
3 Sp1-0.8 0.93 11.77 8.4 11.77
4 Sp1-1 1.62 13.45 9.42 13.12
5 Sp2-0.15 1.02 11.58 7.22 11.4
6 Sp2-0.25 1.27 15.92 9.38 14.2
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7 Sp2-0.35 2.07 17.95 11.83 16.8


8 Accelerator 0.24 3.98 2.91 3.85
9 W-C0.5 0.90 10.90 4.58 10.23
10 W-C0.4 0.62 7.70 3.75 6.88
11 W-C0.4 0.73 8.03 3.83 7.83
FA cement

curve then becomes linear again with a much steeper slope than
that of the first part. There is a transition point 共Pt兲 for each mix
located at the maximum curvature of the transition region, de-
scribing the transition of fresh concrete from conditions of setting
to hardening, and indicating a gain in strength of the concrete.
The times of occurrence of transition point 共tt兲 for Mixes 1, 3, and
10 were 305 min 共5.08 h兲, 706 min 共11.77 h兲 and 462 min
共7.70 h兲 after mixing. Comparing Mixes 1 and 10, the higher
W / C ratio 共Mix 10兲 shows a later transition time, corresponding
to a later start of solidification. And comparing Mixes 1 and 3, the
incorporation of superplasticizer in Mix 3 leads to the longest
Fig. 2. Electrical resistivity response of concretes: 共a兲 minimum time to reach its transition point.
point Pm and three development periods on curves ␳ – t; 共b兲 transition The values of tm and tt of the all 11 mixes, are given in Table
point Pt on curves ␳ – t 共log scale兲 2. It can be seen that tm and tt are obviously related to the different
setting processes caused by W / C, incorporated admixtures or ce-
ment type. The experimentally observed changes in the electrical
development with time 共␳ – t兲 for the control concrete 共Mix 1兲, the response can be further analyzed. The electrical resistivity re-
concrete containing a superplasticizer 共Mix 3兲 and concrete with a sponse of concrete can be divided into three different develop-
higher water cement ratio 共Mix 10兲 are plotted in Figs. 2共a and b兲. ment periods based on Pm and Pt, as shown Fig. 2共a兲, and the
Fig. 2共a兲 shows the resistivity ␳ change with time up to 400 min characteristics of each period are described as follows.
and the critical points, Pm, are marked as solid dots on the curves. The dissolving period 共I兲 occurs from the start of mixing to
Fig. 2共b兲 shows the resistivity ␳ change up to 1,440 min on a point Pm. Bulk resistivity ␳共t兲 deceases largely due to the increase
logarithmic scale and the second critical points Pt, are identified of ions in the liquid phase during this period. After water is added
on the curves. to the cement, the dissolution of ions from the cement takes place
As shown in Fig. 2共a兲, the electrical resistivity response 共␳ – t兲 and mobile ions, such as potassium 共K+兲, sodium 共Na+兲, calcium
exhibits a minimum point, Pm, in the first stage after mixing. Pm 共Ca2+兲, hydroxyl ions 共OH−兲, sulfate 共SO2− 4 兲 are released. These
represents a maximum conducting point corresponding to each free mobile ions favor the conductivity of the matrix solution. The
mix, indicating the solution in the hydration system reaches satu- variable admixtures, the W / C, or the cement type can cause
ration with dissolution progress, suggesting the onset of hydra- changes in the ion concentration or composition of the liquid
tion. The occurrence times of the minimum point 共tm兲 for Mixes phase 共Li et al. 2003; Torrents et al. 1998; Wei and Li 2005兲. The
1, 3, and 10 were 20 min 共0.33 h兲, 56 min 共0.93 h兲, and 37 min time to reach the saturation point for each mix is therefore af-
共0.62 h兲, respectively. As compared to Mix 1, the higher W / C of fected by the W / C, the type and dosage of the admixture, and the
Mix 10 leads to a longer time to reach saturation, which agrees to cement type.
the results observed by Li et al. 共2003兲. Moreover, an obviously The setting period 共II兲 is from point Pm to the transition point
delayed Pm in Mix 3 shows the effect of the incorporation of a Pt. In this period, the electrical resistivity gradually increases with
superplasticizer. time, indicating a decrease in porosity and increase in tortuosity.
As shown in Fig. 2共b兲, the ␳ – t 共log scale兲 relationship of each The hydrate nuclei form from the saturated solution, consuming
mix exhibits a similar distinctive feature, dividing the curve into the ions in the solution and at the same time reducing the porosity.
three parts. The first part, at earlier ages, has a linear pattern with The hydration progress results in a percolation of the matrix, and
a very slight upward slope, and is followed by a transition region the fluid concrete then transits to a rigid state. From point Pm to a
in which the slope starts to increase in a curved manner. The time of about 2 h, for the control sample, the change in resistivity

JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2007 / 425

J. Mater. Civ. Eng. 2007.19:423-427.


is approximately only 0.1 ⍀ m, indicating that the concrete is
relatively inactive and remains in a plastic state. Afterwards, the
rapid hydration leads to significant increase in the resistivity. At
the time of occurrence of the transition point, the early hardening
stage begins. Mixes 3 and 10 follow similar trends.
The accelerator in Mix 8 is principally to influence the rate of
hydration of the alite phase of the cement, resulting in an increase
in CSH gel formation at early ages, thereby shortening the setting
time 共Hewlett 1998兲. The various factors involving higher poros-
ity in the concretes with higher W / C, of reactivity retardation by
the superplasticizers and of the slower reaction rate in fly ash
cement, have increased the time at which the transition point Pt
occurs as compared with the control sample, suggesting that the
mixes stay fluid or in a semifluid state for a longer time after
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mixing.
Hardening period 共III兲: This period commences from point Pt
onwards, which indicates a change in the rate of increase of ␳共t兲.
The hydration progress leads to the matrix having more tortuosity
and the resistivity continually increases with time. The reaction
rate decreases, controlled by ion-diffusion when the thicker hy-
drates on the cement particle surface form 共Mindess et al. 2003兲.

Correlation of the Setting Time Measured by ASTM


C 403 and the Time of Critical Points Occurring on
the Resistivity Response

To correlate the setting time of concrete with the critical points on


the resistivity response, setting times of concrete have been mea-
sured by the ASTM C 403 procedure mentioned earlier. The set-
ting time results are listed in Table 2. It can be seen in Table 2 that
the initial set and final set occur between tm and tt, and the chang-
ing trends in the setting time 共ti, t f 兲 are the same as those observed
in the resistivity response 共tm, tt兲 caused by the incorporation of an
admixture or variable W / C compared with the control. The retar-
dation increases with increase in the superplasticizer dosage or
W / C; a longer time also appears in Mix 11 having fly ash cement, Fig. 3. Correlation of ti, t f measured with penetration resistance and
when compared with Mix 10. On the other hand, the time points tm, tt on the electrical resistivity response: 共a兲 correlation of ti and
of Mix 8 are shifted to the earliest time due to an accelerator tm , tt; 共b兲 correlation of t f and tt
being used, which indicates that the electrical resistivity response
is directly related to the setting behavior of the concrete. Thus, the
resistivity measurement monitors changes in the setting behavior accelerator, higher W / C and the superplasticizer on setting
introduced by admixtures or variable W / C or the cement type, behavior.
with a high level of sensitivity. Final setting time is when fresh concrete starts to gain
Initial setting time measured by the penetration needle is used strength. Based on the physical meaning of the final setting time
to control the schedule of handling and placing. It is assumed that and the fact that tt is close to t f , a quantitative relationship is
at the initial setting the mixture starts to lose plasticity due to obtained as
hydrates being formed. The initial setting time is quantified in
t f = 0.9202tt + 0.2129, R2 = 0.9895 共2兲
terms of the time of onset of hydration 共tm兲 and time at which the
transition point 共tt兲 occurs. Based on the current study, ti can be where t f = final setting time 共h兲.
expressed as the following equation and the correlation is shown In the previous analysis, the electrical resistivity response ␳共t兲
in Fig. 3共a兲: provides an indication of setting behavior. The relationships 关Eqs.
共1兲 and 共2兲兴 have been developed based on the critical points on
the resistivity response. By plotting the measured 共ti, t f 兲 and cal-
ti = 1.8807tm + 0.4429tt, R2 = 0.8950 共1兲
culated 共ti, t f 兲 with the line of equality, it indicated that a good
where ti = initial setting time 共h兲; tm and tt = times of occurrence of correlation can be established as shown in Fig. 4.
the minimum point and transition point 共h兲, from the resistivity The electrical resistivity method provides practical advantages
response. over the conventional penetration resistance method because it
It can also be seen in Table 2 that the value of tt is close to the can continuously measure the data immediately after mixing and
final setting time. The relationship between tt and t f are schemati- can be used directly on concrete rather than on sieved mortar. The
cally shown in Fig. 3共b兲, and a good linear correlation can be electrical resistivity measurement 共ERM兲 only needs about
observed. The four mixes from Mixes 1, 2, 8, and Mix 10, as 0.0016 m3 of fresh concrete, but the penetration method needs at
examples, are highlighted in Fig. 3共b兲, presenting the effect of the least 0.01 m3 of mortar sieved from fresh concrete. The ERM has

426 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2007

J. Mater. Civ. Eng. 2007.19:423-427.


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