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DOI 10.1007/s13369-014-1028-4
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2 Experimental Method
Five batches of cement slurry were mixed with tap water at Fig. 1 Schematic of core holder in the CoreTestSystem™
water–cement ratio (w/c) of 0.55, 0.5, 0.4, 0.3 and 0.25. In
this case, some samples with w/c of 0.25 and 0.55 acted Then the mixing speed was increased to 12,000 rpm and the
as a controller variable. In this study, API cement Class G mixing process was continued for another 35 min. During
High Sulfate Resistant (G-HSR) with the specific gravity of the first 30 min, cement powder was poured gently into the
3.2 g/cm3 obtained from LaFarge Malaysia was used. The mixer that had been filled with water until it was well mixed;
cement composition measured by XRF analysis was given in then the mixing was continued for 35 min longer. Once the
Table 1. It was mixed in a constant speed mixer at 4,000 rpm slurry has been prepared, it was immediately placed into a 1-
for 30 min according to API 10A recommended practice [14]. in.-diameter × 1-in.-length cylinder rubber jacket. Then the
sample was weighed using a digital balance, and the weight
measurement was used as an input in the electrical conduc-
Table 1 Composition of Class G-HSR cement
tivity measurement.
Raw oxide wt.% Bogue phasesa wt.%
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1 0.25 70 3,000
2 0.3 25 14.7
3 0.3 40 1,500
4 0.3 65 3,000
5 0.4 25 14.7
0.2 MHz
Bulk
6 0.4 40 1,500
Resistivity
7 0.4 65 3,000
8 0.5 25 14.7
9 0.5 40 1,500
10 0.5 65 3,000
11 0.55 70 3,000 Fig. 2 Typical Nyquist plot of early age cement sample at w/c = 0.5
at atmospheric conditions
apparatus, the cement samples were first jacketed by a flexi- To adjust and enhance data quality, it was done by bal-
ble rubber to avoid leakage or fluid loss. To measure electrical ancing Z-meter interfacing box with a reference resistor and
properties, the electrode was carefully aligned with each end by selecting the reference resistor that most closely matched
of the sample. The standardized electrode materials consist- to the effective (low frequency) resistance of the sample,
ing of porous silver membrane filters produced by Osmonics respectively. This effectively balanced the voltage that was
Inc were used here. measured by the two amplifiers. In addition, correcting for
Samples were inserted in a core-holder component con- parasitic impedances at high frequencies required the refer-
sisting of two silver electrical contacts embedded in the face ence resistor to be equal to or larger than the effective resis-
of each end cap. Here, the frequency measurement, totally tance of the sample.
involving 25 data points of frequencies for each execution The effect of elevated temperature on conductivity mea-
stored, was set from 0.2 MHz to 1 Hz in a logarithmic sweep. surement was corrected using Hammond and Robson corre-
These measurements were performed repeatedly until the lation [17]. This equation was theoretically generated using
sample reached 24 h of hydration which is considered as Arrhenius equation that expressed the influence of tempera-
early hydration period [16]. The device can apply both ele- ture on conductivity on various cements and concretes. The
vated pressure and temperature simultaneously. The confin- equation is shown below:
ing pressure of 3,000 psi, on the other hand, was manually
σ (T ) 1 1
conditioned using a hydraulic pump. The output from the ln =α − (2)
σ (Tref ) Tref T
measurement system subsequently was recorded by the data
acquisition system. The system temperature of about 65 ◦ C where T (K) and Tref (K) are the absolute and reference tem-
was then obtained by heating the oil chamber and recorded perature and α (K) is an empirical coefficient. The authors
by an integrated thermocouple of the system. Measurements suggested a = 2,900 (K) for concrete and a = 2,200 (K)
were gradually collected at several 30-min intervals for the for cement paste.
first 5 h, followed by the 1-hour increment for the next mea- Pore fluid was obtained through an extraction of the
surement up to 10 h and continued at the 2-h interval until cement sample at certain pressure using Fann 175 ml HPHT
reaching 24 h of hydration. The experimental conditions for API Filter Press which could be pressurized to 1,800 psig on
this measurement are presented in Table 2. the cell and 750 psig on the back pressure receiver. At this
A typical Nyquist plot is shown in Fig. 2. The cement point, the maximum operating temperature was at 350 ◦ F
bulk conductivity (σb ) is calculated from the bulk resistivity (177 ◦ C). Pore fluid consisted of a filter paper connected to
(Rb ) in the Nyquist plot at the cut-off frequency after it has the orifice for fluid expulsion. Once removed, it was collected
been normalized for geometry factor (k), according to the directly into a glass flask for the conductivity measurement.
equation below: To obtain about 5 ml, the pore fluid was collected at several
points of time period that were about 1, 3, 5, 10, 16 and 24 h
G
σb = (1) of hydration period and then followed by sealing off the ori-
Rb
fice using filter press. The pressure profile was generated by
where G = l/A is the geometry factor, l is the length of the pumping Nitrogen (N2 ) until reaching the desired pressure.
specimen (2.54 cm), and A is the surface area perpendicular At last, the conductivity measurement after fluid extraction
to the direction of electrical current (5.06 cm2 ). was immediately performed using conductivity meter.
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5 10 16 24
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Fig. 7 Generalized relationship of measured permeability and normal- Fig. 8 Generalized relationship of measured permeability and pore
ized conductivity diameter
be identical with the individual plot in the form of power the following correlation equation:
law as presented in Fig. 7. The least square error showed
k = 2 × 10−7 (dc2 )2.326 (4)
a number of about 0.909. The correlation obtained has the
following form of equation.
2.16 3.3 Empirical Equation for Permeability Prediction
σb
k = 11.06 (3)
σo
To have a comprehensive correlation for permeability pre-
It has been suggested that the microstructural parameter in the diction that represented the pore diameter and normalized
form of characteristic length was sensitive to the permeability conductivity, a multiple non-linear regression analysis was
profile. The permeability depended mainly on the connected performed by nominating permeability as the independent
pores and pore length scale at which the former represented variable, whilst normalized conductivity and pore diameter as
normalized conductivity, and the latter corresponded to char- the dependent variables. A non-linear plot is shown in Fig. 9
acteristic length. The length scale could be generated from and the following equation was obtained after the regression
Mercury Intrusion Porosimetry (MIP) experiment that cor- analysis:
responded to the pore diameter at the inflection point on a
1
cumulative volume versus pressure diagram [4]. However, in k= (σb /σ0 )1.15 (dc2 )1.25 (5)
this study the pore length of cement sample was calculated 828
using a simple particle expansion model [26] which was easy, The natural log symbols for each axis in Fig. 9 were meant
fast and comparably accurate. This model simulated cements to provide an ease in calculating a non-linear form by taking
a regular cubic lattice in the form of a spherical particle that the natural log of the data, performing the multiple linear
had the same radius and growth, and then the pore size was regressions on the logged data, and then transforming the
estimated to be a diameter of the pore between the edge to resulting equation into the non-linear form by taking the nat-
edge. The resulting relationship between normalized conduc- ural exponential of both sides. The resulting Eq. (5) is similar
tivity and pore length scale complied to power law with the to that of proposed by Katz–Thompson equation with differ-
least square error of about 0.910 as can be seen in Fig. 8 with ent constant values.
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References
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22. Scherer, G.W.; Funkhouser, G.P.; Peethamparan, S.: Effect of pres- 26. Ridha, S.; Irawan, S.; Ariwahjoedi, B.: Microstructure parameter
sure on early hydration of class H and white cement. Cem. Concr. estimation in permeability calculation of well cement during early
Res. 40(6), 845–850 (2010) hydration by a simple particle expansion model. In: National Post-
23. Appleby, S.; Wilson, A.: Permeability and suction in setting graduate Conference (NPC), pp. 1–5 (2011)
cement. Chem. Eng. Sci. 51(2), 251–267 (1996) 27. Nyame, B.K.; Illston, J.M.: Relationships between permeability
24. Galle, C.: Effect of drying on cement-based materials pore struc- and pore structure of hardened cement paste. Mag. Concr. Res.
ture as identified by mercury intrusion porosimetry: a comparative 33(116), 139–146 (1981)
study between oven, vacuum, and freeze-drying. Cem. Concr. Res.
31(10), 1467–1477 (2001)
25. Torquato, S.: Random Heterogeneous Materials; Microstructure
and Macroscopic Properties. Springer, New York (2002)
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