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European Journal of Applied Sciences – Vol. 11, No. 1
Publication Date: February 25, 2023
DOI:10.14738/aivp.111.13941.
Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different
Curing Temperatures. European Journal of Applied Sciences, Vol - 11(1). 637-648.
Services for Science and Education – United Kingdom
Hydration of Palm Oil Fuel Ash Modified Cement Paste at
Different Curing Temperatures
Nkwenti Flavious Tanue
University of Douala,
Post Graduate Training Unit for Engineering Sciences, Douala, Cameroon.
University of Bamenda, National Higher Polytechnic Institute, Bamenda, Cameroon
Laurantine Momoh Bondoh
University of Bamenda, National Higher Polytechnic Institute,
Bamenda, Cameroon
Fokwa Didier
University of Douala, Post Graduate Training Unit for Engineering Sciences,
Douala, Cameroon
Tchemou Gilbert
University of Douala, Post Graduate Training Unit for Engineering Sciences,
Douala, Cameroon
Abstract
As concrete production around the world continuously increases, the high levels of
carbon dioxide emissions from cement manufacture have resulted in growing
interest in the field of supplementary cementitious materials (SCM). Palm oil fuel
ash (POFA) has been proven to be a potential SCM. This study presents the partial
replacement of cement with POFA in four different samples (0%, 5%, 10% and
15%). It is aimed at investigating the influence of POFA to the physical properties
and the hydration rate of cement paste at different temperature conditions (15° C,
28° C and 40° C). The hydration rate of the POFA modified samples was determined
by measuring the amount of hydration water consumed under the different curing
conditions. Physical properties investigated included apparent density, specific
density, fineness, soundness, consistency and setting time test. The results for
physical properties showed that fineness varied from 0.5% for the control sample
through 1.01% for the 5% POFA modified sample to 1.20% for the 15% POFA
modified sample. For soundness, 10% and 15% POFA modified samples are 50%
sounder than both the 5% POFA modified sample and the 0% sample. Meanwhile
both consistency and setting time where proven to be proportional to the increase
in the POFA content of the sample. As for the rate of hydration, globally,
consumption of hydration water was proportional to curing temperature. However,
at 15oC curing temperature, results varied perplexedly: dropping from 0% to 5%
before increasing at 10%, and then dropping from 10% to 15%. At room
temperature, a gradual continuous raise was recorded and a drop witness only for
the 15% sample. At 40° C curing temperature it was instead a continuous drop of
the hydration rate.
Keywords: Cement, POFA, rate of hydration, curing temperature.
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
INTRODUCTION
With the challenge of rapid population growth and evolution in the world leading to rapid
urbanization, environmental sustainability has become a problem in most sectors including the
construction sectors. This is because concrete has become one of is the world’s most widely
used manufactured material and one of the most important construction material before timber
and steel [1]. Unfortunately, the production of cement; the binding element in concrete is
linked to contributing 7% to 10% of global CO2 gas which enhances environmental instability
[2]. By 2025, around 3.5 billion tons of carbon dioxide is foreseen to be released to the
atmosphere during cement production [3]. One solution for more sustainable production
proposed can be the use of Supplementary Cementitious Materials (SCMs).
Supplementary cementitious materials (SCMs) are soluble siliceous, aluminosiliceous, or
calcium aluminosiliceous powders used as partial replacements of clinker in cements or as
partial replacements of Portland cement in concrete mixtures [4]. Industrial solid by-products
such as fly ash, ultrafine fly ash, silica fumes, etc. along with some natural pozzolanic materials
like volcanic tuffs, diatomaceous earth, sugarcane bagasse ash, palm oil fuel ash, rice husk ash,
mine tailings, etc. are good SCMs. In the right proportions, SCMs can improve the fresh
properties of concrete especially the long-term durability [3]. Tay in 1990 began research
studies to see possibilities of using ash as a SCM where he used POFA to replace Portland
cement and showed that it had some pozzolanic properties [5].
Palm oil fuel ash (POFA) is a by-product of palm oil industry, generated from the combustion of
palm oil plant residues. The annual world production of palm kernel shell amounts to about
21,359,000 tons, with about 270,000 tons for Cameroon and about 70% of these shells in
Cameroon are dumped in the wild [6], leading to huge storage problems as it occupies valuable
lands as well as environmental discomfort. The burning of these waste produces POFA which
has been proven to contain cementitious material properties because it contains silica oxide
(SiO2), aluminium oxide (Al2O3) and ferric oxide (Fe2O3).
Recent research endeavour has led to the improvement of new type of concretes by substituting
a percentage of cement, with several supplementary cementitious materials (SCM). As far is
POFA replacement is concerned, most of the researchers have conducted their studies to
improve the compressive strength of concrete containing POFA. For example, Muthusamy and
Zamri [7] concluded that 20% of POFA as cement replacement is the optimum level for
compressive strength of concrete at 28 days. In another study by Islam et al. [8], it was found
that 10% of POFA is the optimum level to replace cement in the concrete mix. In a recent study
by Zeyad et al. [9], it was shown that ultrafine POFA replacing cement can achieve compressive
strength higher than control samples, which may reach more than 90 MPa at 28 days. In 2007,
Tangchirapat et al. [10] used three types of POFA in concrete; the first type was original POFA
called OP, the second type was median particles (15.9 μ) called MP, and the third type was small
particles (7.4 μ) called SP. They reported that the compressive strength of concrete containing
OP was much lower than in case of OPC, while compressive strength of concrete containing
10% MP, and concrete containing 20% SP was better than normal concrete at 90 days.
Concerning fresh properties, Some researchers noted that workability of concrete decreases
with increased amount of POFA percentages in the concrete mortar[8], [11], [12]. Several
studies showed that the use of POFA delays the setting of concrete, and therefore the initial and
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final setting times increase with the increased POFA content[8], [10], [13]. According to Md.
Safiuddin et al., limited studies have been conducted to examine the effects of POFA on the
plastic shrinkage, slump loss, and air content of concrete[14]. Plastic shrinkage causes early- age cracking in concrete, which is responsible for many durability problems.
The accomplishment of an appropriate hydration necessitates the integration of the
surrounding environment temperature to the mixing parameters. Our contribution will be to
monitor the hydration of POFA substituted cement past at various replacement percentages at
different curing temperatures. These temperatures will reflect the mean temperatures of the
various climatic regions of Cameroon at their peak harsh seasons.
EXPERIMENTAL POOL
Materials Studies
Physico-Chemical Features of Cements Used:
The cement that we have used for the test is Portland cement (CPA-CEM II) that is
commercialised by Cimencam; the Cameroonian based cement-producing company.
According to the technical specification paper obtained from the Cimencam Bonaberi Factory,
which is in conformity of the Cameroonian norms: NC 234-2005-06, the characteristics of the
Portland cement used are as consigned in tables 1 and 2.
Table 1: Chemical Constituent of Portland Cement
Table 2: Physical Properties of the Cement
Fusion temperature > 1000°C
Absolute mass density 2.8 - 3.2 g/m3 at 20°C
Apparent mass density 0.9 - 1.2 g/m3 at 20°C
Solubility in water Just 1.5 g/l at 20°C
Granulometry 20 - 30 % of finesse <5μm
Initial setting time 60 - 90 minutes
Source: Cimencam
Obtention of the Palm oil Fuel Ash:
In this study, ash was collected from a local Palm Oil Mill at Souza, Moungo Division in
Cameroon. The collected POFA was oven dried at 105 ̊C for 24 hours and then sieved using an
80 μm size sieve to remove coarse particles and foreign material. After that, the POFA was
grinded in a Deval’s machine with a rotating drum of 100 ± 5 rpm lasting 6 hours to achieve an
improved fineness. After grinding, the POFA passing through 45 μm size sieve was collected.
Chemical Name Chemical Formula Shorthand
Notation
Percent by
Weight
Tricalcium Silicate 3CaO.SiO2 C3S 55 to 70
Dicalcium Silicate 2CaO.SiO2 C2S 10 to 25
Tricalcium Aluminate 3CaO.Al2O3 C3A 5 to 13
Tetracalcium Aluminoferrite 4CaO.Al2O3.Fe2O3 C4AF 1 to 15
Gypsum CaSO4.H2O CSH2 ≤3.5
Source: Cimencam
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
The total amount of POFA passing through the 45 μm was 60%. Figure 1 shows the preparation
of POFA
Figure 1: Preparation of POFA
Sampling:
Three families of POFA modified cement samples were used in this study, in addition to a 100%
pure cement sample. The replacement proportions where 5%, 10% and 15%. These
proportions were motivated by literature. Islam et al. concluded that POFA within 5–15% of
cement replacement gives better results in terms of compressive strength; in contrast,
increased POFA proportions lead to decrease in the splitting and flexural tensile strengths[8].
Experimental Protocol
A series laboratory tests were carried out to determine some physical properties of the
different samples. These tests included the apparent density test, the specific density test by
pycnometer method (IS 4031-11) [15], the fineness test using the sieve method (IS 4031-
1)[15], the soundness test conducted by Le-Chatelier method (BS EN 196-3), the consistency
and setting time test using the vicat method (BS EN 196-3).
The rate of hydration of POFA modified cement pastes was performed in this study by
monitoring the amount of water consumed by different samples under various curing
temperatures. The different temperatures in this reseach reflect the mean temperatures of the
various climatic regions of Cameroon at their peak harsh seasons. In that light, three curing
temperatures of 15° C, 28° C and 40° C where used.
The procedure for each sample lasted for a period of three days:
Day 1:
Releasing oil was applied inside 12 labelled petri-dishes. These dishes were grouped into sets
of 3. (3 dishes for 0%, 3 dishes for 5%, 3 dishes for 10% and the last 3 dishes for 15% POFA
substituted samples). The empty masses of these dishes in each group were weighed and
recorded. Next, we prepared a fresh cement paste using about 500g of each sample, mixing each
sample at a of water-cement ration of 0.35. For each of the oiled dish per set, the paste was filled
into it to about 1⁄4 full, and the dish vibrated to minimize voids. Then the dish was filled
completely and levelled off at the surface. From here, the masses of each sample were recorded
and the three dishes from each set were regrouped into Ziploc bag as shown on figure 2 to avoid
water evaporation. They were the placed under their respective temperature-controlled
environments for 24 hours.
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Day 2:
The next day, we removed the samples from their respective environments after 24 hours and
massed each dish separately and then recorded their masses. All the dishes containing their
respective samples were then placed in an oven at a temperature of 105 o C in order to
completely dry off the remaining water in the pores of the different samples.
Day 3:
The third day, the samples were removed from the oven and weighed. At this stage, the amount
of water consumed for the 24 hours age of hydration could be computed. The mass of driven
off water in the oven was calculated, as we as the mass of combined water during hydration
and finally, the percentage of water reacted was also calculated.
Calculation
Mass of cement = mass of fresh paste
1+w c
⁄
Mass of original water = mass of cement x w⁄c
Mass of water driven off = day 2 sample mass - day 3 sample mass
Mass of water combined during hydration= original water – water driven off
Percentage of water reacted= mass of driven off water x100
mass of original water
Figure 2: Samples of cement paste in Ziploc bags
RESULTS AND DISCUSSIONS
Physical Properties
The basic physical properties tests conducted on the three POFA modified cement samples and
the control sample (0% POFA modified sample) recoded the following results:
a. Fineness: The values recorded vary from 0.5% for the control sample (pure cement
sample) through 1.01% for the 5% POFA modified sample to 1.20% for the 15% POFA
modified sample (figure 3)
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
The results show that fineness is inversely proportional to the increase in the POFA
content of the sample. A regression model in the form of a second-degree polynomial
equation inscribed on figure 3 bellow can define the situation with a coefficient of
determination of about 98%.
The fineness of cement is the significant factor affecting the rate of hydration, rate of
gain of strength, setting time, and rate of evolution of heat. The rate of strength
development increases with fineness. Since the specific surface area is inversely
proportional to the size of the particle, the surface area is more for finer cement than for
a coarser cement. Therefore, the finer the cement, the higher the surface area for
hydration and hence faster the development of strength. Therefore, it will be evident
that our POFA modified samples present a weaker strength than that of the control
sample as first witness by some researchers[16]–[18]. Though this weakness can be a
question of the poor degree of grounding. Nevertheless, the setting time will be delayed
while its consistency decreases, thereby reducing the early-age shrinkage possibilities.
b. Soundness Test: Results show that, 10% and 15% POFA modified samples are 50%
sounder than both the 5% POFA modified sample and the control sample (figure 4).
Soundness of cement can be defined as its ability to retain its volume after it gets
hardened. This means that a properly sound cement will undergo minimum volume
change in its hardened state. In the soundness test of cement, we determine the amount
of excess lime [15]. As such, the 10% and 15% POFA modified samples will undergo
minimum volume change after hardening than 0% and 5% POFA modified cement.
Hence, the addition of 10% and 15% POFA to cement causes a decrease in undue
expansion of the concrete. This undue expansion results from excess lime (CaO) content
in cement. The EN 196-3 [19] states that the soundness of concrete should not exceed
10 mm. That implies the different cement samples used in this study are within the limit
and contain minimal amounts of lime.
Figure 3: Fineness of cement with different POFA contents.
y = -0.1067x2 + 0.7547x - 0.13
R2 = 0.9782
0
0.2
0.4
0.6
0.8
1
1.2
1.4
0 % POFA 5 % POFA 10 % POFA 15 % POFA
Fineness (%)
Sample type
Fineness (%)
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Figure 4: Soundness of cement with different POFA contents.
c. Consistency Test: As it can be observed on figure 5, the w/c ratios required to obtain
standard consistency increased with increase in POFA content.
The results show that consistency is proportional to the increase in the POFA content of
the sample. A regression model in the form of a second-degree polynomial equation
inscribed on the figure can define the situation with a coefficient of determination of
about 98.5%
The increase in the w/c ratio is because POFA has a high affinity for water because of the
large surface and also because of delayed hydration process. Again, POFA is more porous
compared to cement, and so will tend to absorb more water with increase in its content.
A review done by Safiuddin et al [14] indicates truly that the porosity of POFA particles,
causes it to absorb more water and thus reduce the free water content. In addition, the
water demand of ground POFA becomes greater than that of unground POFA due to
increased specific surface area. The angularity and irregularity of ground POFA with
some porous particles also contribute to increase the water demand of concrete for a
given workability.
d. Setting Time Test: The final setting time test was performed on all the four samples of
0% POFA, 5% POFA, 10% POFA and 15% POFA. It is observed on figure 6 that setting
time evolved with the addition of POFA content in the cement sample.
The reaction of OPC clinker compounds like C3S and C3A with water is often slowed
down by the presence of gypsum, which lead to the early formation of ettringites
(Calcium aluminium sulphate, Ca6All2(SO4)3(OH)12. 26H2O.Addition of POFA further
again slows down the normal process. Increase in the content of POFA in substituting
the quantity of cement indicates an increase in the setting time. As recorded by
Tangchirapat et al [10] the long setting times of POFA concrete are due to the pozzolanic
reaction (reaction between POFA and calcium hydroxide evolved from cement
hydration), which is usually slower than the hydration reaction of cement.
1 1
0.5 0.5
0
0.2
0.4
0.6
0.8
1
1.2
0% pofa cement 5% pofa cement 10% pofa cement 15% pofa cement
Soundness(mm)
pofa cement type
Soundness of POFA modified cement
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
There is no standard value for the setting time of cement. Though literature holds that
according to the British Standard and the ASTM requirement (ASTM C150/C150M-09
2009), the maximum final setting time of cement is 10 hour [20].
In this study, the setting time of the control sample was recorded to be 140 minutes. The
addition of 5% POFA increased this time by 36%. Subsequent POFA addition then only
recorded a gradually increment of the setting time. A regression model in the form of a
second-degree polynomial equation inscribed on figure 6 can define the situation with a
coefficient of determination of about 96.4%.
Figure 5: Consistency of cement with different POFA contents.
Figure 6: Final setting time of cement with different POFA contents.
y = 0.0025x2 + 0.004x + 0.2725
R2 = 0.9858
0.25
0.26
0.27
0.28
0.29
0.3
0.31
0.32
0.33
0.34
0 5 10 15
Consistency(mm)
Consistency(mm) Poly. (Consistency(mm))
y = -7.5x2 + 62.5x + 87.5
R2 = 0.964
120
140
160
180
200
220
240
0 5 10 15
Time (min)
POFA %
Setting time
Setting time Poly. (Setting time)
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Table 3: Physical Properties of POFA modified Cement samples
POFA content Consistency
w/c ratio
Fineness
(Sieve method)
Soundness
(Le-Chatelier
method)
Setting time
(Vicat)
0% 0.28 99.5% 1 mm 140 minutes
5% 0.29 98.99% 1 mm 190 minutes
10% 0.31 98.88% 0.5 mm 200 minutes
15% 0.33 98.80% 0.5 mm 220 minutes
Table 3 above presents the summary of the different physical properties for the four cement
samples discussed above.
Rate of Hydration
The rate of hydration in this study measured to the amount of water consumed during the
hydration process. Cement paste samples were prepared with an optimal w/c ratio of 0.35 for
all the four cement samples, subjected to curing under the three temperature ranges used in
this study (15° C, 28° C and 40° C). The curing period lasted 24 hours and the various data
collected were computed in an Excel sheet as stated in paragraph II.2 above to obtain the
percentage of consumed water during hydration.
A total of 36 samples were studied: 3 for each of the four cement samples and at each curing
temperature. The major reason for the repeatability of the tests was to confirm trustworthiness
of the first readings. The values of the recoded masses and the calculations are consigned in
table 4 below.
Table 4: Rate of hydration test data
CURING
TEMPERATURE
15° C 28° C 40° C
CEMENT
SAMPLE
0% 5% 10
%
15
%
0% 5% 10
%
15
%
0% 5% 10
%
15
%
Day one
Mass of paste 191
.74
177
.91
206
.81
179
.72
199
.95
204
.54
243
.57
235
.93
271
.18
280
.27
210
.55
237
.08
Mass of
cement
142
.03
131
.79
153
.19
133
.13
148
.11
151
.51
180
.42
174
.76
200
.87
207
.61
155
.96
175
.61
Mass of water 49.
71
46.
12
53.
62
46.
59
51.
84
53.
03
63.
15
61.
17
70.
31
72.
66
54.
59
61.
47
Day two
Mass of
sample
190
.96
177
.71
206
.63
179
.70
199
.53
204
.28
243
.53
235
.44
270
.41
279
.56
209
.38
236
.19
Day 3
Mass of dry
sample
157
.05
144
.32
169
.71
145
.14
163
.00
170
.32
206
.13
198
.08
230
.26
237
.07
176
.00
199
.69
Mass of
driven off
water
33.
91
33.
39
36.
92
34.
56
36.
53
33.
96
37.
40
37.
36
40.
15
42.
49
33.
38
36.
50
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
Mass of water
combined in
reaction
15.
80
12.
73
16.
70
12.
03
15.
31
19.
07
25.
75
23.
81
30.
16
30.
17
21.
21
24.
97
% of water
reacted
31.
78
27.
61
31.
14
25.
83
29.
53
35.
96
40.
77
38.
92
42.
89
41.
52
38.
85
40.
62
Figure 7: Hydration rate at different curing temperatures
Results obtained reveal that, globally as shown on figure 7, the rate of hydration is proportional
to curing temperature though the behaviour of the POFA content at each curing temperature is
perplexing. At the lowest curing temperature (15oC), a drop in the consumption of water during
hydration from 0% to 5% before recording an increase at 10%, and then a drop-in hydration
rate from 10% to 15% was experienced. Meanwhile, at room temperature, a gradual continuous
raise in the hydration rate was recorded and a drop witness only for the 15% sample. On its
part, the highest curing temperature (40° C) contrary to the previous, instead recorded a
continuous drop of the hydration rate.
0.0
10.0
20.0
30.0
40.0
50.0
15° C 28° C 40° C
% of hydrated water
Curing temperature
Hydration rate
0% 5% 10% 15%
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Figure 8: Hydration rate at different curing temperatures
From the trends observed, it can be concluded that the amount of water used up during
hydration increases with increase in temperature for all the samples. But it is only at the 28° C
curing temperature that hydration water consumption increased with the increase in POFA
content (Figure 8). This affects the microstructure development of the cement paste. The initial
hydration products at elevated temperatures are distributed heterogeneously and is thus
detrimental to the compacity of the sample and thereby reducing its strength. A similar
situation was witnessed by Deschner and al. when they modified cement with siliceous fly ash
[21].
CONCLUSION
This work was focused on investigating the influence of POFA to the physical properties and
the hydration rate of cement paste. The major influencing parameters for this study were the
POFA content and the curing temperature conditions (15° C, 28° C and 40° C).
Results of physical properties showed the though fineness of the cement samples was inversely
proportional to the increase in the POFA content of the sample, the lime content of the samples
were rather better equilibrated with this POFA addition. That is why the 10% and 15% POFA
modified samples were 50% sounder than both the 5% POFA modified sample and the control
sample. This leaded to the proportional increase of the consistency and the setting time of the
samples with more POFA addition. As such, the 10% and 15% POFA samples will undergo lesser
volumetric deformation than the later.
As regards the hydration, globally, the rate of hydration is proportional to curing temperature
though the behaviour of the POFA content at each curing temperature is bewildering. While at
28° C, an ascending behaviour was recorded, it was the contrary at 40° C. Meanwhile that at 15°
20
25
30
35
40
45
0% 5% 10% 15%
% OF HYDRATED WATER
POFA CONTENT
HYDRATION RATE
28° C 15° C 40° C
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Tanue, N. F., Bondoh, L. M., Didier, F., & Gilbert. T (2023). Hydration of Palm Oil Fuel Ash Modified Cement Paste at Different Curing Temperatures.
European Journal of Applied Sciences, Vol - 11(1). 637-648.
URL: http://dx.doi.org/10.14738/aivp.111.13941
C was simply sinusoidal form. In this light, it is necessary to reduce the intervals of both
parameters (POFA content and curing temperature) and also integrate the variation of the
composition of the cement samples in subsequent researches.
Acknowledgement
Gratitude to Mr. ASHU WYATT AGBOR-ENOH for his assistance during the experimentations
carried out in the GEOSTRUCT laboratory.
Conflicts of Interest
The authors declare no conflicts of interest regarding the publication of this paper.
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