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International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019
Available at www.ijsred.com
ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 343
Statistical Modelling and Optimization of the
Performance Enhancement of Ubakala Clay for
use as Drilling Mud
---------------------------------------************************----------------------------------
Abstract:
This work studied the performance enhancement of Ubakala clay for use as drilling mud. A clay sample was collected from Ubakala in
Abia State of Nigeria, processed and beneficiated with varying concentrations of soda ash (0-6wt %). Experiments were conducted to
determine the viscosities of the control and clay-soda ash mixture at different curing time intervals (0-8hours), temperatures (30O
C-90O
C) and
speed of agitation (100rpm-600rpm). Response surface methodology, with the aid of MATLAB statistical toolbox was used to perform a
statistical study and optimization of the data obtained from the study. The results revealed that soda ash concentrations, temperature, curing
time and their interactions terms are significant variables in the statistical model with temperature being the most significant term, while time
is the least significant term. The graphical representation of the control showed a decreasing rate in viscosity within the required range of
speed of agitation unlike those of the clay- soda ash mixture. The optimum predicted value of yield stress occurs for a curing time of 8hours,
temperature of 900
C and soda ash concentration of 5.183wt% and this is recommended as the operating parameters for enhancing the
performance of Ubakala clay sample for use as a drilling mud.
Keywords — clay, drilling mud, rheological study, model, viscosity, optimization.
----------------------------------------************************----------------------------------
I INTRODUCTION
Drilling the wellbore is the first and most expensive step in
the oil and gas industry. Expenditure for drilling represents
25% of the total oil field exploitation cost and is concentrated
mostly in exploration cost and development of well drilling
[1]. Drilling fluid which represent about one-fifth of the total
cost of petroleum well drilling, must generally comply with
three important requirements – they should be easy to use,
not too expensive and environmentally friendly. Drilling mud
is important to petroleum and gas production due to its use in
cleaning the rock fragment from beneath the bit to the surface,
sufficient hydrostatic pressure exertion against sub-surface
formations, cool and lubricate the rotating drill string and bit.
When oil and gas operations began in Nigeria in the early
fifties, local clay was used in the preparation of drilling fluids
and cement slurries. The introduction of imported
commercial bentonite in the year 1960 drastically reduced the
use of Nigerian local clay in the petroleum and gas industries
[2]. This also led to a significant reduction in research into
local bentonite clay that could have been used in oil and gas
operations like drilling, cementing, simulation and others.
Prior to the government’s initiative to develop local content,
the cost of importation of bentonite for drilling activities in
Nigeria runs into millions of dollars annually which has been
detrimental to the economy of the country considering that
one-fifth of the cost of drilling a well which ranges between 1
million to 100 million dollars accounts for drilling fluids.
Therefore, it is imperative to locally outsource these clay
materials in order to conserve foreign exchange, create
employment and to enhance Nigerian content development in
the drilling component of oil and gas industry
Nigeria is blessed with abundant reserve of oil, gas and clay
[3], but yet spends millions of dollars yearly importing drilling
mud despite the proven reserve of clay deposits, if these local
deposits are beneficiated and efficiently enhanced, they would
be readily used as drilling mud [4]. Several researchers have
studied some local clay samples [2], [5], [6], [7], [8], [9], [10],
but studies on Ubakala clay, which is one of the abundant
local clays, is not rife in literature, and especially, the authors
did not find any works that considered the effect of
temperature, thus the need for this study.
II METHODOLOGY
The study area chosen for this work was Ubakala town. The
town is located in Umuahia South Local Government Area of
Abia State, south-eastern Nigeria and lies on longitude 70
24’E
and latitude 50
10’N on the geological map of Nigeria.
Materials: Ubakala clay; Sodium Ash; Distilled water.
Equipment: Ostwald viscometer (Model NDJ95N);
Thermometer; Pipette; Weighing balance; Measuring
cylinders; Stopwatch; Mechanical agitator; 200 mesh Tyler
Allison, F.N.*, Nwanekezie, M.N.*, Osoka, E.C.**
*Department of Chemical Eng., Chukwuemeka Odimegwu Ojukwu University, Uli, Nigeria
**Department of Chemical Eng., Federal University of Technology, Owerri, Nigeria
RESEARCH ARTICLE OPEN ACCESS
International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019
Available at www.ijsred.com
ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 344
Sieve (approx. 75 µm size); Hammer mill; Mortar and
pestle/grinder; Plastic buckets
The apparatus consists of an Ostwald viscometer which is a
U-shaped glass tube with two arms and is made of clear
borosilicate and constructed in accordance with the dimension
as shown below. In one arm, N, an upper bulb C is connected
with a fine capillary, R. The lower end of the capillary is
connected with a U-tube, P, provided with bulb A in the
second arm, L. This bulb is necessary to maintain the
hydrostatic pressure during flow of liquid. Through the
capillary tube, the liquid flows with measurable speed. There
are two marks E and F above and below the upper bulb C.
Figure 1: Ostwald Viscometer (Dimensions in mm)
PROCESSING THE CLAY SAMPLES
The collected clay sample is sun-dried to remove moisture and
then pounded with the aid of a mortar and pestle to reduce the
particle size and increase the surface area. The pounded clay
sample is then put in a furnace for further drying to remove
the possible moisture content in sample. After drying, the
sample is taken to mill for further grinding to get the desired
particle size. A hammer mill is mounted vertically and is
designed to have two funnels. The upper funnel serves as the
clay sample inlet while the bottom one serves as the clay
sample outlet. The mill has a hammer at the centre which is
driven by an electric motor part of the mill. The function of
the hammer is to continuously reduce the particles of the clay
to obtain the desired size. Below the hammer is a sieve with
mesh of size 75 µm. The mesh is changeable and the mesh
size used determines the size of the clay particle to be
obtained. After passing through the mill, the clay gotten is
packaged for the experiment.
Sample preparation
Four different samples were prepared and labeled as follows:
• Sample A: 50g of clay/700ml of distilled water.
• Sample B: 50g of clay/700ml of distilled water + 2
wt. % Na2CO3(s)
• Sample C: 50g of clay/700ml of distilled water + 4
wt. % Na2CO3(s)
• Sample D: 50g of clay/700ml of distilled water + 6
wt. % Na2CO3(s)
Procedure:
The viscometer was washed with distilled water
and completely dried. Sample A was heated on heating stirrer
setting the temperature at 30 C and rotor at 100 rpm.
Sample A is then introduced through tube L to slightly above
the mark G, using a long pipette to minimize wetting the tube
above the mark. The tube is clamped vertically and allowed to
stand to maintain equilibrium. The volume of the liquid
sample is adjusted so that the meniscus settles at the mark G.
It is then sucked through arm N about 5 mm above the mark E.
After releasing pressure or suction, the time taken for the
bottom of the meniscus to fall from the top edge of mark E to
the top edge of mark F was taken at curing time intervals of 0,
2, 4, 6, and 8 hours and at temperature of 30 , 60 and
90 . Then, the viscosity was read using Ostwald viscometer.
This was repeated for speed of agitation of 200 rpm, 300 rpm,
400 rpm, 500 rpm and 600 rpm. The above procedure was
repeated for Samples B, C and D.
Mathematical Methodology:
The data of viscosity obtained from the experiment will be
plotted against shear rate and its fit to: Bingham Plastic model,
Power Law model, Herschel-Bulkley model and Casson
model determined and compared based on the adjusted R2
-
squared value. The model that gave the best fit to most or all
of the plots will be used to evaluate the parameters for
statistical study and optimization [11].
The statistical study will be done based on a full factorial
experimental design using the statistical toolbox of MATLAB
software for statistical modeling, response surface study and
optimization. The study will be done for each data using
curing time (x1), temperature (x2) and soda ash concentration
(x3) as factors, with model parameter (yield stress or viscosity)
(y) as response while a-k are constant terms. The value of
selected model parameter will be fit to four response surface
models:
Linear: = + + + (1)
Interaction: = + + + + +
+ (2)
Pure-quadratic: = + + + + + +
(3)
Quadratic: = + + + + + +
+ + + (4)
The model that best fits, based on the adjusted R-squared, will
be considered the statistical model that best describes the
parameter and will be used for optimization to determine
optimum conditions for the parameter.
International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019
Available at www.ijsred.com
ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 345
The value of the R-squared will be used as a measure of
model accuracy and values greater than or equal to 0.90 will
be considered acceptable. The p-value of the F-statistics will
be used as a measure of model adequacy and a value less than
or equal to 0.05 will be acceptable using 95% confidence
interval. The significance of the main effects will be
determined using Analysis of variance (ANOVA) which will
be judged in a similar way to the F-statistics, using the p-value,
while the statistical significance of each element in the model
will be determined using the t-statistics value or its associated
p-value.
The interaction between the factors will be determined using
the surface plots, especially its contour lines, and the
optimization toolbox of MATLAB used for the optimization
of selected model parameter based on the model [12]-[16].
III RESULTS AND DISCUSSION
TABLE 1: DATA FOR STATISTICAL MODELING/OPTIMIZATION
Time Temp. Soda ash
conc.
X1 X2 X3 τγ
0 30 0 6.921
2 30 0 6.922
4 30 0 6.924
6 30 0 6.935
8 30 0 6.938
0 30 2 6.931
2 30 2 6.931
4 30 2 6.932
6 30 2 6.640
8 30 2 6.940
0 30 4 6.932
2 30 4 6.932
4 30 4 6.936
6 30 4 6.938
8 30 4 6.940
0 30 6 6.933
2 30 6 6.936
4 30 6 6.938
6 30 6 6.939
8 30 6 6.939
0 60 0 7.042
2 60 0 7.050
4 60 0 7.052
6 60 0 7.060
8 60 0 7.065
0 60 2 7.060
2 60 2 7.087
4 60 2 7.081
6 60 2 7.096
8 60 2 7.123
0 60 4 7.060
2 60 4 7.088
4 60 4 7.082
6 60 4 7.097
8 60 4 7.124
0 60 6 7.061
4 60 6 7.090
6 60 6 7.096
8 60 6 7.094
0 90 0 7.128
2 90 0 7.120
4 90 0 7.168
6 90 0 7.208
8 90 0 7.234
0 90 2 7.251
2 90 2 7.121
4 90 2 7.169
6 90 2 7.216
8 90 2 7.237
0 90 4 7.255
2 90 4 7.141
4 90 4 7.173
6 90 4 7.229
8 90 4 7.239
0 90 6 7.142
2 90 6 7.175
4 90 6 7.227
6 90 6 7.240
8 90 6 7.258
RESULT OF RESPONSE SURFACE MODELANALYSIS
The result of the MATLAB programming of the response
surface modelling is presented below.
It can be observed from table 2 using the t-stat value (which
should have a magnitude of ≥2 for significant variables) and
its p-value (which should be ≤ 0.05 at 95% confidence
interval for significant variables), that the most significant
terms appear to be temperature ( ) and soda ash
concentration ( 	). The model is adequate for study Based on
the p-value of the F-stat (which is ≤	0.05) and the three terms
time ( ), soda ash concentration ( 	) and temperature ( )
are all significant based on the analysis of variance (table 3).
The adjusted ! values reveal that the statistical model
explains about 99% of the observed variability in the
experimental data. The model is 99% accurate.
TABLE 2: RESPONSE SURFACE MODEL STATISTICS
Variables Coefficients F -stat
International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019
Available at www.ijsred.com
ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 346
Constants 6.7727 Sse=0.0064742
-0.0036 Dfe=50
0.0053 Dfr=9
0.0073 Ssr=0.77556
2.3917*10#$ F=665.51
1.3333*10#% P val=0
	 1.4167*10#%
-3.6905*10#$
-1.4861*10#%
-8.3750*10#$
Variables t-stat P values
Constants 486.9739 1.4028*10-93
-1.6214 0.1112
12.0931 1.8439*10# &
2.4845 0.0164
11.2795 2.3991*10# %
0.0574 0.9545
	 0.5282 0.5997
-1.6815 0.0989
-4.2920 8.1171*10#%
-2.2804 0.0269
Result of the Analysis using Surface Plots.
Using the programming for the mesh grid, the surface plots
are presented below.
From table 3 it can be deduced that soda ash concentration ( )
is the least significant variable while temperature ( 	) and
time ( ) are the most significant variables. It can be observed
from figure 2, the surface plot of temperature and time, that
temperature shows a progressive colour variation and is more
significant than time and the two factors seem linearly related
to the yield stress.
It can be observed from figure 3, the surface plot of time and
soda ash concentration, that time shows more significant than
soda ash concentration. In addition, time seems to be linearly
related to yield stress while soda ash concentration seems
quadratically related.
Figure 2: Surface Plot Interactions between Temperature (℃) and Time (hr)
Figure 3: Surface Plot Interactions between Soda Ash Conc. (wt %) and Time
(hr)
Figure 4: Surface Plot between Soda Ash Conc. (wt %) and Temperature (℃)
TABLE 3: ANALYSIS OF VARIANCE TABLE
0
2
4
6
8
20
40
60
80
100
6.9
7
7.1
7.2
7.3
7.4
Time (hours)
X: 8
Y: 90
Z: 7.268
Temperature (O
C)
YieldStress(Pa.s)
6.95
7
7.05
7.1
7.15
7.2
7.25
0
2
4
6
8
0
2
4
6
7.02
7.04
7.06
7.08
7.1
7.12
Time (hours)
X: 8
Y: 4.8
Z: 7.12
Soda Ash Conc (%)
YieldStress(Pa.s)
7.04
7.05
7.06
7.07
7.08
7.09
7.1
7.11
20
40
60
80
100
0
2
4
6
6.9
7
7.1
7.2
7.3
7.4
Temperature (O
C)
X: 90
Y: 6
Z: 7.217
Soda Ash Conc (%)
YieldStress(Pa.s)
6.95
7
7.05
7.1
7.15
7.2
International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019
Available at www.ijsred.com
ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 347
source Sum sq. d. f. Mean
sq.
F Prob>F
0.02056 4 0.00714 15.66 0
0.7268 2 0.3634 796.91 0
0.00387 3 0.00129 2.83 0.0476
Error 0.0228 50 0.00046
Total 0.78203 59
It can be observed from figure 4, the surface plot of
temperature and soda ash concentration, that the temperature
seems to be more significant than soda ash concentration.
Also the interaction level is low.
Therefore, time, temperature and soda ash concentration are
significant as variables with only interaction between time and
temperature being significant.
Optimization shows that an optimum predictive value of yield
stress occurs for a curing time of 8 hours, temperature of 90℃
and soda ash concentration of 5.1831. The predicted optimum
(7.2716) only deviates from the experimental value by 0.2%.
The optimization also indicated that the optimum values of
curing time and temperature are local optimum which can be
improved by using higher curing time and temperature values.
The optimum value of soda ash concentration is global
optimum that cannot be improved upon by shifting lower or
upper bounds.
IV CONCLUSION
The surface plots showed that curing time and temperature are
significant variables, but temperature is more significant than
time and both are linearly related to yield stress. The surface
plot of time and soda ash concentration showed that time is
more significant than soda ash concentration. In addition, time
seems to be linearly related to yield stress while soda ash
concentration seems quadratically related. The surface plot of
temperature and soda ash concentration showed that
temperature seems to be more significant than soda ash
concentration and the interaction level is low. Therefore, the
order of decreasing significance is: temperature, curing time,
and soda ash concentration. All variables are however
significant in the analysis of viscosity of clay.
Optimization shows that an optimum predictive value of yield
stress occurs for a curing time of 8 hours, temperature of 90℃
and soda ash concentration of 5.1831. The predicted optimum
(7.2716) only deviates from the experimental value by 0.2%.
The optimization also indicated that the optimum values of
curing time and temperature are local optimum which can be
improved by using higher curing time and temperature values.
The optimum value of soda ash concentration is global
optimum that cannot be improved upon by shifting lower or
upper bounds.
V REFERENCES
[1] T. B. Adam Jr, M. E. Chenevert, K. K. Millheim, F. S. Young Jr.,
“Applied Drilling Engineering”, SPE Textbook Series, Richardson,
TX, Vol.2, Edited by Jack FE and David SP, 1986.
[2] O. Omole, S. Malomo, and S. Akande, “The Suitability of
Nigerian black soil clays as drilling mud clays”, Elsevier Science
Publishers, B. V., Amsterdam, Appl. Clay Sci. 4, pp. 357 –
372,1989.
[3] W. Emofurieta, “Investigation into the rheological and filtration
properties of drilling mud formulated with clays from Northern
Nigeria”, International Conference on Modern Mining
Processing, Abuja Nigeria, 2010. www.nigerianewsdirect.com.
[4] D. C. Agle,, and B. Dwayne, “NASA Rover Finds Conditions
Once Suited for Ancient Life on Mars”. NASA. Retrieved March
12, 2013.
[5] O. A. Falode, O. A. Ehinola and P. C. Nebeife, “Evaluation of
local bentonitic clay as oil well”, Applied Clay Science 39 (1-2),
pp. 19-27, 2008.
[6] C. O. Okogbue and E. Ene, “Geochemical and Geotechnical
Characteristics and the Potential for Use in Drilling Mud of Some
Clay Bodies in South-eastern Nigerioa”, Journal of Mining and
Geology. 44(2), pp. 121-130, 2008.
[7] T. U. Apugo-Nwosu, I. A. Mohammed-Dabo, A. S. Ahmed, G.
Abubakar and S. I. Ayilara,.”Studies on the Suitability of
Ubakala Bentonitic Clay for Oil Well Drilling Mud Formulation”,
British journal of Applied Science and Technology, 1 (4), pp, 152-
171, 2011.
[8] O. M. Nweke, E. O. Igwe and P. N. Nnabo, “Comparative
Evaluation of Clays from Abakaliki Formation with Commercial
Bentonite Clays for the Use as Drilling Mud”, African Journal of
Environmental Science and Technology,9 (6), pp. 508-518, 2015.
[9] B. Dye, “Design Considerations for High Performance Water-
Based Muds”, AADE Paper AADE-04-DF-HO-14, presented
April 2004.
[10] J. D. Exner, and B.C. Craft, “Effects of Temperature on the
Viscosity of Some Gulf Coast Drilling Muds”, Petroleum
Transactions, AIME, Volume 103, Pp. 112-116, 2012.
[11] F. N. Allison, M. N. Nwanekezie, E. C. Osoka,
“Rheological study of performance enhancement of Ubakala clay
for use as drilling mud”, International Journal of Scientific
Research and Engineering Trends, 5(3), pp. 730-734, 2019.
[12] N. Asadi and H. Zilouei, “Optimization of organosoly
pretreatment of rice for enhanced biohydrogen production using
Enterobacter aerogenes”, Bioresource Technology. 227, pp. 335 –
344 , 2017 doi: 10.1016/j.biortech.2016.12.073
[13] R. Battit, B. Mauro and M. Franco, “Reactive Search and
Intelligent Optimization.”, Springer Verlag, 2008. ISBN 978-0-
387-09623-0.
[14] F. Boylu,. “Optimization of foundry sand characteristics of
soda-activated calcium bentonite, Applied Clay Science 52, pp.
104-108, 2011.
[15] G. E. P. Box and K. B. Wilson, “On the Experimental
Attainment of Optimum Conditions (with discussion)”. Journal of
the Royal Statistical Society Series B13 (1), pp.1- 45, 1951.
[16] A. Gelman,. “Analysis of Variance? Why it is more important
than ever”. The Annals of Statistics 33: 1 – 53, 2005.
.

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IJSRED-V2I3P36

  • 1. International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019 Available at www.ijsred.com ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 343 Statistical Modelling and Optimization of the Performance Enhancement of Ubakala Clay for use as Drilling Mud ---------------------------------------************************---------------------------------- Abstract: This work studied the performance enhancement of Ubakala clay for use as drilling mud. A clay sample was collected from Ubakala in Abia State of Nigeria, processed and beneficiated with varying concentrations of soda ash (0-6wt %). Experiments were conducted to determine the viscosities of the control and clay-soda ash mixture at different curing time intervals (0-8hours), temperatures (30O C-90O C) and speed of agitation (100rpm-600rpm). Response surface methodology, with the aid of MATLAB statistical toolbox was used to perform a statistical study and optimization of the data obtained from the study. The results revealed that soda ash concentrations, temperature, curing time and their interactions terms are significant variables in the statistical model with temperature being the most significant term, while time is the least significant term. The graphical representation of the control showed a decreasing rate in viscosity within the required range of speed of agitation unlike those of the clay- soda ash mixture. The optimum predicted value of yield stress occurs for a curing time of 8hours, temperature of 900 C and soda ash concentration of 5.183wt% and this is recommended as the operating parameters for enhancing the performance of Ubakala clay sample for use as a drilling mud. Keywords — clay, drilling mud, rheological study, model, viscosity, optimization. ----------------------------------------************************---------------------------------- I INTRODUCTION Drilling the wellbore is the first and most expensive step in the oil and gas industry. Expenditure for drilling represents 25% of the total oil field exploitation cost and is concentrated mostly in exploration cost and development of well drilling [1]. Drilling fluid which represent about one-fifth of the total cost of petroleum well drilling, must generally comply with three important requirements – they should be easy to use, not too expensive and environmentally friendly. Drilling mud is important to petroleum and gas production due to its use in cleaning the rock fragment from beneath the bit to the surface, sufficient hydrostatic pressure exertion against sub-surface formations, cool and lubricate the rotating drill string and bit. When oil and gas operations began in Nigeria in the early fifties, local clay was used in the preparation of drilling fluids and cement slurries. The introduction of imported commercial bentonite in the year 1960 drastically reduced the use of Nigerian local clay in the petroleum and gas industries [2]. This also led to a significant reduction in research into local bentonite clay that could have been used in oil and gas operations like drilling, cementing, simulation and others. Prior to the government’s initiative to develop local content, the cost of importation of bentonite for drilling activities in Nigeria runs into millions of dollars annually which has been detrimental to the economy of the country considering that one-fifth of the cost of drilling a well which ranges between 1 million to 100 million dollars accounts for drilling fluids. Therefore, it is imperative to locally outsource these clay materials in order to conserve foreign exchange, create employment and to enhance Nigerian content development in the drilling component of oil and gas industry Nigeria is blessed with abundant reserve of oil, gas and clay [3], but yet spends millions of dollars yearly importing drilling mud despite the proven reserve of clay deposits, if these local deposits are beneficiated and efficiently enhanced, they would be readily used as drilling mud [4]. Several researchers have studied some local clay samples [2], [5], [6], [7], [8], [9], [10], but studies on Ubakala clay, which is one of the abundant local clays, is not rife in literature, and especially, the authors did not find any works that considered the effect of temperature, thus the need for this study. II METHODOLOGY The study area chosen for this work was Ubakala town. The town is located in Umuahia South Local Government Area of Abia State, south-eastern Nigeria and lies on longitude 70 24’E and latitude 50 10’N on the geological map of Nigeria. Materials: Ubakala clay; Sodium Ash; Distilled water. Equipment: Ostwald viscometer (Model NDJ95N); Thermometer; Pipette; Weighing balance; Measuring cylinders; Stopwatch; Mechanical agitator; 200 mesh Tyler Allison, F.N.*, Nwanekezie, M.N.*, Osoka, E.C.** *Department of Chemical Eng., Chukwuemeka Odimegwu Ojukwu University, Uli, Nigeria **Department of Chemical Eng., Federal University of Technology, Owerri, Nigeria RESEARCH ARTICLE OPEN ACCESS
  • 2. International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019 Available at www.ijsred.com ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 344 Sieve (approx. 75 µm size); Hammer mill; Mortar and pestle/grinder; Plastic buckets The apparatus consists of an Ostwald viscometer which is a U-shaped glass tube with two arms and is made of clear borosilicate and constructed in accordance with the dimension as shown below. In one arm, N, an upper bulb C is connected with a fine capillary, R. The lower end of the capillary is connected with a U-tube, P, provided with bulb A in the second arm, L. This bulb is necessary to maintain the hydrostatic pressure during flow of liquid. Through the capillary tube, the liquid flows with measurable speed. There are two marks E and F above and below the upper bulb C. Figure 1: Ostwald Viscometer (Dimensions in mm) PROCESSING THE CLAY SAMPLES The collected clay sample is sun-dried to remove moisture and then pounded with the aid of a mortar and pestle to reduce the particle size and increase the surface area. The pounded clay sample is then put in a furnace for further drying to remove the possible moisture content in sample. After drying, the sample is taken to mill for further grinding to get the desired particle size. A hammer mill is mounted vertically and is designed to have two funnels. The upper funnel serves as the clay sample inlet while the bottom one serves as the clay sample outlet. The mill has a hammer at the centre which is driven by an electric motor part of the mill. The function of the hammer is to continuously reduce the particles of the clay to obtain the desired size. Below the hammer is a sieve with mesh of size 75 µm. The mesh is changeable and the mesh size used determines the size of the clay particle to be obtained. After passing through the mill, the clay gotten is packaged for the experiment. Sample preparation Four different samples were prepared and labeled as follows: • Sample A: 50g of clay/700ml of distilled water. • Sample B: 50g of clay/700ml of distilled water + 2 wt. % Na2CO3(s) • Sample C: 50g of clay/700ml of distilled water + 4 wt. % Na2CO3(s) • Sample D: 50g of clay/700ml of distilled water + 6 wt. % Na2CO3(s) Procedure: The viscometer was washed with distilled water and completely dried. Sample A was heated on heating stirrer setting the temperature at 30 C and rotor at 100 rpm. Sample A is then introduced through tube L to slightly above the mark G, using a long pipette to minimize wetting the tube above the mark. The tube is clamped vertically and allowed to stand to maintain equilibrium. The volume of the liquid sample is adjusted so that the meniscus settles at the mark G. It is then sucked through arm N about 5 mm above the mark E. After releasing pressure or suction, the time taken for the bottom of the meniscus to fall from the top edge of mark E to the top edge of mark F was taken at curing time intervals of 0, 2, 4, 6, and 8 hours and at temperature of 30 , 60 and 90 . Then, the viscosity was read using Ostwald viscometer. This was repeated for speed of agitation of 200 rpm, 300 rpm, 400 rpm, 500 rpm and 600 rpm. The above procedure was repeated for Samples B, C and D. Mathematical Methodology: The data of viscosity obtained from the experiment will be plotted against shear rate and its fit to: Bingham Plastic model, Power Law model, Herschel-Bulkley model and Casson model determined and compared based on the adjusted R2 - squared value. The model that gave the best fit to most or all of the plots will be used to evaluate the parameters for statistical study and optimization [11]. The statistical study will be done based on a full factorial experimental design using the statistical toolbox of MATLAB software for statistical modeling, response surface study and optimization. The study will be done for each data using curing time (x1), temperature (x2) and soda ash concentration (x3) as factors, with model parameter (yield stress or viscosity) (y) as response while a-k are constant terms. The value of selected model parameter will be fit to four response surface models: Linear: = + + + (1) Interaction: = + + + + + + (2) Pure-quadratic: = + + + + + + (3) Quadratic: = + + + + + + + + + (4) The model that best fits, based on the adjusted R-squared, will be considered the statistical model that best describes the parameter and will be used for optimization to determine optimum conditions for the parameter.
  • 3. International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019 Available at www.ijsred.com ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 345 The value of the R-squared will be used as a measure of model accuracy and values greater than or equal to 0.90 will be considered acceptable. The p-value of the F-statistics will be used as a measure of model adequacy and a value less than or equal to 0.05 will be acceptable using 95% confidence interval. The significance of the main effects will be determined using Analysis of variance (ANOVA) which will be judged in a similar way to the F-statistics, using the p-value, while the statistical significance of each element in the model will be determined using the t-statistics value or its associated p-value. The interaction between the factors will be determined using the surface plots, especially its contour lines, and the optimization toolbox of MATLAB used for the optimization of selected model parameter based on the model [12]-[16]. III RESULTS AND DISCUSSION TABLE 1: DATA FOR STATISTICAL MODELING/OPTIMIZATION Time Temp. Soda ash conc. X1 X2 X3 τγ 0 30 0 6.921 2 30 0 6.922 4 30 0 6.924 6 30 0 6.935 8 30 0 6.938 0 30 2 6.931 2 30 2 6.931 4 30 2 6.932 6 30 2 6.640 8 30 2 6.940 0 30 4 6.932 2 30 4 6.932 4 30 4 6.936 6 30 4 6.938 8 30 4 6.940 0 30 6 6.933 2 30 6 6.936 4 30 6 6.938 6 30 6 6.939 8 30 6 6.939 0 60 0 7.042 2 60 0 7.050 4 60 0 7.052 6 60 0 7.060 8 60 0 7.065 0 60 2 7.060 2 60 2 7.087 4 60 2 7.081 6 60 2 7.096 8 60 2 7.123 0 60 4 7.060 2 60 4 7.088 4 60 4 7.082 6 60 4 7.097 8 60 4 7.124 0 60 6 7.061 4 60 6 7.090 6 60 6 7.096 8 60 6 7.094 0 90 0 7.128 2 90 0 7.120 4 90 0 7.168 6 90 0 7.208 8 90 0 7.234 0 90 2 7.251 2 90 2 7.121 4 90 2 7.169 6 90 2 7.216 8 90 2 7.237 0 90 4 7.255 2 90 4 7.141 4 90 4 7.173 6 90 4 7.229 8 90 4 7.239 0 90 6 7.142 2 90 6 7.175 4 90 6 7.227 6 90 6 7.240 8 90 6 7.258 RESULT OF RESPONSE SURFACE MODELANALYSIS The result of the MATLAB programming of the response surface modelling is presented below. It can be observed from table 2 using the t-stat value (which should have a magnitude of ≥2 for significant variables) and its p-value (which should be ≤ 0.05 at 95% confidence interval for significant variables), that the most significant terms appear to be temperature ( ) and soda ash concentration ( ). The model is adequate for study Based on the p-value of the F-stat (which is ≤ 0.05) and the three terms time ( ), soda ash concentration ( ) and temperature ( ) are all significant based on the analysis of variance (table 3). The adjusted ! values reveal that the statistical model explains about 99% of the observed variability in the experimental data. The model is 99% accurate. TABLE 2: RESPONSE SURFACE MODEL STATISTICS Variables Coefficients F -stat
  • 4. International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019 Available at www.ijsred.com ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 346 Constants 6.7727 Sse=0.0064742 -0.0036 Dfe=50 0.0053 Dfr=9 0.0073 Ssr=0.77556 2.3917*10#$ F=665.51 1.3333*10#% P val=0 1.4167*10#% -3.6905*10#$ -1.4861*10#% -8.3750*10#$ Variables t-stat P values Constants 486.9739 1.4028*10-93 -1.6214 0.1112 12.0931 1.8439*10# & 2.4845 0.0164 11.2795 2.3991*10# % 0.0574 0.9545 0.5282 0.5997 -1.6815 0.0989 -4.2920 8.1171*10#% -2.2804 0.0269 Result of the Analysis using Surface Plots. Using the programming for the mesh grid, the surface plots are presented below. From table 3 it can be deduced that soda ash concentration ( ) is the least significant variable while temperature ( ) and time ( ) are the most significant variables. It can be observed from figure 2, the surface plot of temperature and time, that temperature shows a progressive colour variation and is more significant than time and the two factors seem linearly related to the yield stress. It can be observed from figure 3, the surface plot of time and soda ash concentration, that time shows more significant than soda ash concentration. In addition, time seems to be linearly related to yield stress while soda ash concentration seems quadratically related. Figure 2: Surface Plot Interactions between Temperature (℃) and Time (hr) Figure 3: Surface Plot Interactions between Soda Ash Conc. (wt %) and Time (hr) Figure 4: Surface Plot between Soda Ash Conc. (wt %) and Temperature (℃) TABLE 3: ANALYSIS OF VARIANCE TABLE 0 2 4 6 8 20 40 60 80 100 6.9 7 7.1 7.2 7.3 7.4 Time (hours) X: 8 Y: 90 Z: 7.268 Temperature (O C) YieldStress(Pa.s) 6.95 7 7.05 7.1 7.15 7.2 7.25 0 2 4 6 8 0 2 4 6 7.02 7.04 7.06 7.08 7.1 7.12 Time (hours) X: 8 Y: 4.8 Z: 7.12 Soda Ash Conc (%) YieldStress(Pa.s) 7.04 7.05 7.06 7.07 7.08 7.09 7.1 7.11 20 40 60 80 100 0 2 4 6 6.9 7 7.1 7.2 7.3 7.4 Temperature (O C) X: 90 Y: 6 Z: 7.217 Soda Ash Conc (%) YieldStress(Pa.s) 6.95 7 7.05 7.1 7.15 7.2
  • 5. International Journal of Scientific Research and Engineering Development-– Volume 2 Issue 3, May –June 2019 Available at www.ijsred.com ISSN : 2581-7175 ©IJSRED: All Rights are Reserved Page 347 source Sum sq. d. f. Mean sq. F Prob>F 0.02056 4 0.00714 15.66 0 0.7268 2 0.3634 796.91 0 0.00387 3 0.00129 2.83 0.0476 Error 0.0228 50 0.00046 Total 0.78203 59 It can be observed from figure 4, the surface plot of temperature and soda ash concentration, that the temperature seems to be more significant than soda ash concentration. Also the interaction level is low. Therefore, time, temperature and soda ash concentration are significant as variables with only interaction between time and temperature being significant. Optimization shows that an optimum predictive value of yield stress occurs for a curing time of 8 hours, temperature of 90℃ and soda ash concentration of 5.1831. The predicted optimum (7.2716) only deviates from the experimental value by 0.2%. The optimization also indicated that the optimum values of curing time and temperature are local optimum which can be improved by using higher curing time and temperature values. The optimum value of soda ash concentration is global optimum that cannot be improved upon by shifting lower or upper bounds. IV CONCLUSION The surface plots showed that curing time and temperature are significant variables, but temperature is more significant than time and both are linearly related to yield stress. The surface plot of time and soda ash concentration showed that time is more significant than soda ash concentration. In addition, time seems to be linearly related to yield stress while soda ash concentration seems quadratically related. The surface plot of temperature and soda ash concentration showed that temperature seems to be more significant than soda ash concentration and the interaction level is low. Therefore, the order of decreasing significance is: temperature, curing time, and soda ash concentration. All variables are however significant in the analysis of viscosity of clay. Optimization shows that an optimum predictive value of yield stress occurs for a curing time of 8 hours, temperature of 90℃ and soda ash concentration of 5.1831. The predicted optimum (7.2716) only deviates from the experimental value by 0.2%. The optimization also indicated that the optimum values of curing time and temperature are local optimum which can be improved by using higher curing time and temperature values. The optimum value of soda ash concentration is global optimum that cannot be improved upon by shifting lower or upper bounds. V REFERENCES [1] T. B. Adam Jr, M. E. Chenevert, K. K. Millheim, F. S. Young Jr., “Applied Drilling Engineering”, SPE Textbook Series, Richardson, TX, Vol.2, Edited by Jack FE and David SP, 1986. [2] O. Omole, S. Malomo, and S. Akande, “The Suitability of Nigerian black soil clays as drilling mud clays”, Elsevier Science Publishers, B. V., Amsterdam, Appl. Clay Sci. 4, pp. 357 – 372,1989. [3] W. Emofurieta, “Investigation into the rheological and filtration properties of drilling mud formulated with clays from Northern Nigeria”, International Conference on Modern Mining Processing, Abuja Nigeria, 2010. www.nigerianewsdirect.com. [4] D. C. Agle,, and B. Dwayne, “NASA Rover Finds Conditions Once Suited for Ancient Life on Mars”. NASA. Retrieved March 12, 2013. [5] O. A. Falode, O. A. Ehinola and P. C. Nebeife, “Evaluation of local bentonitic clay as oil well”, Applied Clay Science 39 (1-2), pp. 19-27, 2008. [6] C. O. Okogbue and E. Ene, “Geochemical and Geotechnical Characteristics and the Potential for Use in Drilling Mud of Some Clay Bodies in South-eastern Nigerioa”, Journal of Mining and Geology. 44(2), pp. 121-130, 2008. [7] T. U. Apugo-Nwosu, I. A. Mohammed-Dabo, A. S. Ahmed, G. Abubakar and S. I. Ayilara,.”Studies on the Suitability of Ubakala Bentonitic Clay for Oil Well Drilling Mud Formulation”, British journal of Applied Science and Technology, 1 (4), pp, 152- 171, 2011. [8] O. M. Nweke, E. O. Igwe and P. N. Nnabo, “Comparative Evaluation of Clays from Abakaliki Formation with Commercial Bentonite Clays for the Use as Drilling Mud”, African Journal of Environmental Science and Technology,9 (6), pp. 508-518, 2015. [9] B. Dye, “Design Considerations for High Performance Water- Based Muds”, AADE Paper AADE-04-DF-HO-14, presented April 2004. [10] J. D. Exner, and B.C. Craft, “Effects of Temperature on the Viscosity of Some Gulf Coast Drilling Muds”, Petroleum Transactions, AIME, Volume 103, Pp. 112-116, 2012. [11] F. N. Allison, M. N. Nwanekezie, E. C. Osoka, “Rheological study of performance enhancement of Ubakala clay for use as drilling mud”, International Journal of Scientific Research and Engineering Trends, 5(3), pp. 730-734, 2019. [12] N. Asadi and H. 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