International Journal of Engineering Sciences, 2(8) August 2013, Pages: 361-367

TI Journals
ISSN
2306-6474

International Journal of Engineering Sciences

www.tijournals.com

Evaluation of Thickening Time of Oil Field Class G Cement Slurry

at High Temperature and Pressure using Experimental Design
K.K. Salam *1, A.O. Arinkoola 2, B. Ajagbe 3, O Sanni 4
1,2,3,4

Petroleum Engineering Unit, Department of Chemical Engineering, P.M.B. 4000, Ladoke Akintola University of Technology (LAUTECH),
Ogbomoso, Nigeria.

AR TIC LE INF O

AB STR AC T

Keywords:

The main objective of cementing technology is to cement casing string so as to facilitate zonal
isolation necessary to drill further or control production. To achieve this objective slurries are
design by adding certain additives to control density, filtration loss and pumpable/thickening time
needed for slurry placement.

Thickening time
Class G cement
Experimental design

Thickening time was evaluated at 6000psi and 400 o C using Experimental Design. Four factors
which include extender, accelerator, antifoam and dispersant was considered at two levels. Sixteen
experiments were conducted with the response replicated twice. The analysis was done using Yates
algorithms to determine the influence of different parameters on the thickening time.
A regression equation was developed for pumpable time as a function of the dependent variables.
The model developed has a correlation coefficient, R2 of 0.9998, coefficient of variance of
0.0000697 and standard error of 0.08838. The model is simple and easily programmable for initial
estimations on the field.
2013 Int. j. eng. sci. All rights reserved for TI Journals.

1.

Introduction

Oil well cement is used as a seal to secure and support casing inside the well and prevent fluid communication between the various
underground fluid-containing layers or the production of unwanted fluids into the well. It has been used as the primary sealant in oil and
gas wells throughout the world and is manufactured to meet specific chemical and physical standards set up by the API [1].
Accurate control of the thickening time, that is the time after initial mixing when the cement can no longer be pumped, is crucial in this
process. If the thickening time is too short, the cement fails to reach its required placement, whilst too long a thickening time leads to costly
delays [2]. Operational problems as a result of short thickening times are especially dramatic because the cement can set prematurely in the
casing or pumping equipment [3] .
The laboratory experiment is usually performed by simulating the wellbore pressure and temperature. The temperature distribution during
the placement process can be calculated by numerical simulations. The time that the surface temperature decreases to the bottom-hole
circulating temperature also can be calculated. Van Kleef et al (1993)[4] compared the strength and weaknesses of two different methods
used to determine thickening time of cement slurry by HTHP pressure equipment. They emphased the effect of shear and pressure on
settling time of cement slurry. Their work targeted at finding reliable way to duplicate downhole situation during laboratory testing, the
actual shear applied to a cement slurry when it is mixed and pumped in field operations. The result from their investigation show accurate
prediction of the pumpability and final hydration times of a certain cement pumpability and final hydration times of certain cement
formulation used in a particular cement job.
Deep water cementing has some challenges such as low temperature, low fracture gradient, narrow margin between pore pressure and
fracture gradient, shallow sea water and gas flow potential [5]. In all these circumstances, thickening time plays a central role during slurry
formulation because it is a measure of the time within which the cement is pumpable [4].
Experimental Design (ED) can be used to monitor both the main and interaction of parameters as they impact on the response factor(s) [6].
Factorial design (FD) have been successfully used in solving engineering problems some of which are: Prediction of Corrosion Rates in the
Drilling Mud using Factorial Design Approach [7]; Evaluation of rheological properties of beneficiated locally sourced mud [8]; Column
leaching of a manganese dioxide ore [9] and much more.
This study utilized FD to evaluate the influence of some major additives on the thickening time and developed a correlation that can be
easily used for timely estimate of the pumpable time for cement setting.
* Corresponding author.
Email address: kaykaysalam@yahoo.co.uk

K. K. Salam et al.

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Int ernational Journal of Engi neering Sc iences, 2(8) Au gust 2013

2.

Methodology

The API thickening time test is the accepted method for measuring how long cement slurry should remain pumpable under simulated
down-hole temperature and pressure conditions. The test was performed in a high-pressure/high temperature (HPHT) Consistometer that is
o

usually rated at pressure up to 6,000 psi and temperatures up to 400 F also, BHST at 600C and BHCT at 500C.
The test involved mixing the cement slurry according to current API procedures, placing the slurry into the slurry cup, and then placing the
slurry cup into the Consistometer for testing. The testing pressure and temperature were controlled to simulate the conditions the slurry will
encounter in the well. The test concluded when the slurry reached a consistency considered unpumpable in the well. The time to reach this
consistency is called thickening time or pumpable time. The test was said to be set after attaining a consistency of 100 Bearden Consistency
(BC) unit under a dynamic state using the HPHT Consistometer.
Se experiments were run with the selected slurry systems and measurements are made for thickening time of oil well class G cement. The
experiment follows the American Petroleum Institute (API) speculation [10].
2.1 Cement Slurry Preparation and thickening time measurement
In order to prepare a cement slurry sample, 297g of Class G oilwell cement were mixed (35 seconds on Waring Blender at high speed) with
447mls of fresh water, subsequently followed by the addition of additives such as 30g of Bentonite ( i.e 10% BWOC) and 26mls antifoam;
(subsequently additives are added according to Table 1). The mixture is mixed using Constant Speed Mixer Model 30-60 of Chandler
Engineering Company according to API Recommended Practice 10B-2 at 12000 rpm 500 in other to achieve the pre-calculated slurry
density of 11.5 ppg. The steps involves in the analysis of thickening time of oil well cement are:

Formulation of slurry design.

Preparation of equipment and apparatus.
Measuring of slurry material
Mixing
Filling of metal cup with slurry.
Computation of consistometer i.e. conditioning it to the required temperature and pressure.
Installation of slurry cup into the consistometer.
Wait for testing period.
Obtain the Result

2.2 Experimental Design

The number of experimental runs performed for the model development is full factorial design which is governs by the equation 1:

N Lk (1)
Where L denotes factors which are 4 in this case, k is no of levels which is 2 and N is the total number of experimental runs which is 16.
The design of the experiement is tabulated in Table 1.

Table 1. Full factorial Design for 4-variables at 2-levels

Run

X1

X2

X3

X4

Run

X1

X2

X3

X4

+1

-1

-1

-1

+1

-1

-1

+1

+1

-1

+1

+1

10

-1

+1

+1

-1

-1

+1

-1

-1

11

-1

-1

+1

+1

-1

-1

-1

+1

12

+1

+1

-1

-1

-1

+1

+1

+1

13

+1

-1

+1

-1

-1

-1

+1

-1

14

+1

+1

+1

+1

+1

+1

-1

+1

15

-1

-1

-1

-1

+1

+1

+1

-1

16

-1

+1

-1

+1

X1,X2,X3 and X4 are the factors considered and the proportions are presented in table 2

Evaluation of Thickening Time of Oil Field Class G Cement Slurry at High Temperature and Pressure Using Experimental Design

363

Internat ional Jour nal of Engineeri ng Science s, 2(8) Au gust 2013

Table 2. Factor Level Settings

FACTORS

LEVELS (%)
Standard (0)
10
5
5.9
2.9

Low (-1)
5
0
0
0

Extender (X1)
Accelerator(X2)
Antifoam (X3)
Dispersant (X4)

High (+1)
15
10
7.9
4.2

2.2.1 Response Variable

The response variable for this experiment is the thickening time. Sixteen (16) experimental runs were performed according to a full
factorial design of four (4) factors using Table 1 as the guide to different formulations of slurry preparations and combination of the factors.
We use ' - ' to indicate low level and '+' for high level.
2.2.2 Model Development
Running the full complement of all possible factor combinations means that we can estimate all the main and interaction effects. In this
experiment, there are 4 main effects, 6 two-factor interactions, 3 three-factor interactions and 1 four-factor interaction, all of which appear
in the full model as follows:

Y 0 1 X 1 2 X 2 3 X 3 4 X 4

12 X 1 X 2 13 X 1 X 3 14 X 1 X 4 23 X 2 X 3 24 X 2 X 4 34 X 3 X 4
123 X 1 X 2 X 3 124 X 1 X 2 X 4 134 X 1 X 3 X 4 234 X 2 X 3 X 4
1234 X 1 X 2 X 3 X 4 e.......... .......... .......... .......... .......... .......... .......... .......... .( 2 )
3.

Results and Discussion

The quantity of each of the variables under low and high is presented in Table 2 above. Each experimental run was conducted twice and the
result of the response variable is recorded in Table 3.
Table 3: Experimental Results

RESPONSE

RUN

X1Extender

X2-Accelerator

X3Antifoam

X4-Dispersant

-1

-1

-1

-1

-1

-1

-1

6
7

Average
Tt (min)

Tt (min) I

Tt (min) II

-1

228

225

226.5

-1

-1

480

450

465

-1

-1

120

130

125

-1

-1

257

260

258.5

-1

-1

268

260

264

-1

-1

200

210

205

-1

-1

380

380

380

-1

-1

250

240

245

-1

205

200

202.5

10

-1

230

240

235

11

-1

238

240

239

12

-1

260

250

255

13

-1

372

350

361

14

-1

200

190

195

15

-1

236

240

238

16

130

140

135

(AV)

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Int ernational Journal of Engi neering Sc iences, 2(8) Au gust 2013

A Yates algorithm is used to calculate the main and interaction effect. These values are recorded in table 4
Table 4. Coefficient and values of the factors

Contrast

Effect

Coefficient

Values

Contrast

Effect

Coeficient

Values

253.375

253.75

X4

-39.0625

X1

-4.9375

-2.46875

X1*X4

-52.75

X2

-38.9375

-19.4688

X2*X4

3.25

X1*X2

-14.25

-7.125

X1*X2*X4

29.9375

X3

2.3125

1.15625

X3*X4

-1.125

X1*X3

-114

-57

X1*X3*X4

32.8125

X2*X3

28

14

X2*X3*X4

-95.1875

X1*X2*X3

15.3125

1
2
12
3
13
23
123

7.65625

X1*X2*X3*X4

1.875

4
14
24
124
34
134
234
1234

-19.5313
-26.375
1.625
14.96875
-0.5625
16.40625
-47.5938
0.9375

These values are substituted for a corresponding value in equation 3 and fully expressed in equation 3 which is express below:

3.1 Effect of the variables on Thickening time

Effect of each of the selected variables was considered with respect to thickening time and the model developed will be compared with the
experimental data.
3.1.1
Effect of change in percentage composition of accelerator, extender, antifoam and dispersant on Thickening Time
The experimental evaluation has shown that the thickening time reduces as the percentage of accelerator and antifoam in the slurry
composition increases which can be represented graphically in figure 1. The optimum accelerator percentage for this research work is 4.5%
above which it is not advisable to add accelerator to the slurry because it will have a detrimental effect on the thickening time. However,
this research work has shown that the thickening time increased as the percentage composition of extender and dispersant increased or
reduced which are graphically represented in figure 1 and 2.
In deep wells, at least three to four hours of pumping time are usually required to allow adequate placement time. However, there are
several complicating factors which need to be examined. As the length of the casing string or liner increases, the problem of achieving a
cement seal becomes more severe. The graphs below show the effect of percentage change of accelerator, extender, anti foam and
dispersant in the cement slurry.
Figure 1 show the relationship between the thickening time and extender. It was observed that increase in the percentage of extender from
5% to 15% lead to corresponding increase in the thickening time; however, this is not the significant function of extender in cement slurry
but poses effects on thickening time of cement slurry.

Figure 1. Effect of extender on the thickening time of cement slurry

Evaluation of Thickening Time of Oil Field Class G Cement Slurry at High Temperature and Pressure Using Experimental Design

365

Internat ional Jour nal of Engineeri ng Science s, 2(8) Au gust 2013

Effect of accelerator on thickening time of cement slurry was illustrated in Figure 2.Inccrease in the value of accelerator to 5% lead to a
slight increment in value of thickening time by 4.35%. Further increase in percentage of accelerator in cement slurry decreased the value of
thickening time by 17% after adding 10% of accelerator to the slurry.

Figure 2. Effect of accelerator on the thickening time of cement slurry

Figure 3 show the effect of antifoam on thickening time of cement slurry. Increase in the percentage of antifoam initially increased the
thickening time value until it reached 6%, after which the value of thickening time reduced with further increase in percentage of antifoam.
However, this is not the significant function of antifoam in cement slurry; the antifoam functions by spreading on the surface of the foam or
entering the foam during mixing, since the film formed the spread of antifoam on the surface of a foaming liquid does not support foam, the
foam situation is alleviated. In well cementing, very small concentrations are necessary to achieve adequate foam prevention, usually less
the 0.1% by weight of mix water.

Figure 3. Effect of antifoam on the thickening time of cement slurry

Effect of Dispersant on thickening time was illustrated in Figure 4. The figure show that increase in Dispersant percentage to 4.2% in
cement slurry lead to a corresponding proportional increament in the value of thickening time from 228min when no dispersant was added
to the slurry to 250min when 4.2% of dispersant was added to the slurry.

Figure 4. Effect of dispersant on the thickening time of cement slurry

Result of the investigation show that there is a close agreement between the experimental and predicted data. Figure 5 gave the comparison
of model prediction data plotted alongside experimental data for the confirmation of accuracy of the model.

K. K. Salam et al.

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Int ernational Journal of Engi neering Sc iences, 2(8) Au gust 2013

3.2 Statistical analysis of the model

The summary of main and interaction effects between the factors used for the development of the model was given in Table 4 and Table 5
show the residual, Degree of Freedom, Mean square and F-value for the various combination of the interaction effects leading to the
development of the model. Figure 5 gives the comparison of model prediction data plotted alongside experimental data for confirmation of
accuracy. The fitted model gave a correlation coefficient (R2 ) value of 1 with standard error of 0.08838 which shows that the model have
an accuracy value 99.9998%. The deviation of the developed model from the experimental values was obtained by the analysis of variance
with the calculation of sum of contrast and mean square value of 1.125 and 0.070313.
Table 5. Analysis of variance of randomised full factorial design

Contrast

Coeficient

(Contrast)

sum of square

Residue

DOF

Mean Sq

Fvalue

584.375

64947481

2029608.781

2029608.8

101480.4391

X1

-2.65625

7225

225.78125

225.78125

11.2890625

X2

-17.40625

310249

9695.28125

9695.2813

484.7640625

X1*X2

-8.40625

72361

2261.28125

2261.2813

113.0640625

X3

1.03125

1089

34.03125

34.03125

1.7015625

X1*X3

-55.21875

3122289

97571.53125

0.5

97571.531

4878.576563

X2*X3

14.03125

201601

6300.03125

0.125

6300.0313

315.0015625

X1*X2*X3

6.78125

47089

1471.53125

1471.5313

73.5765625

X4

-19.28125

380689

11896.53125

11896.531

594.8265625

X1*X4

-24.90625

635209

19850.28125

19850.281

992.5140625

X2*X4

1.59375

2601

81.28125

0.125

81.28125

4.0640625

X1*X2*X4

14.21875

207025

6469.53125

6469.5313

323.4765625

X3*X4

-1.34375

1849

57.78125

0.125

57.78125

2.8890625

X1*X3*X4

15.53125

247009

7719.03125

0.125

7719.0313

385.9515625

X2*X3*X4

-43.96875

1979649

61864.03125

61864.031

3093.201563

X1*X2*X3*X4

3.15625

10201

318.78125

0.125

318.78125

15.9390625

1.125

1.125

16

2029608.8

Residue
Total

4.

31

Conclusion

Experimental Design has been successfully employed in this study for the prediction of thickening time of cement slurry at high
temperature and pressure conditions. Effect of addition of extender, accelerator, antifoam and dispersant produced different trend on
behaviour of thickening time of class G cement slurry. There was a close agreement between the result gotten from the model developed
and experimental result gotten from the laboratory with. The developed model gave a correlation coefficient of 0.9998 and standard error of
0.08838. The model is simple and can readily be used to sensitize on thickening time by varying one or more of the factors considered.

Evaluation of Thickening Time of Oil Field Class G Cement Slurry at High Temperature and Pressure Using Experimental Design

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Internat ional Jour nal of Engineeri ng Science s, 2(8) Au gust 2013

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