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Ruthenium(II)/triphenylphosphine complexes: An effective way to improve the cytotoxicity of lapachol
Journal of Textile Science and Technology, 2024, 10, 64-81
https://www.scirp.org/journal/jtst
ISSN Online: 2379-1551
ISSN Print: 2379-1543
Influence of Solvent onto Chemical
Extraction of America-Type Coconut
(Coco nucifera L.) Fbers: Analysis of
Physicochemical, Mechanical and
Morphological Properties
Delphine Korgai Gandai1, Zara Haman2, Djoda Pagore Frederic1, Memtine Ndong Augustin1,
Abdourhamane Nsangou3, Niraka Blaise1, Hambate Gomdje Valery1*
National Advanced School of Engineering of Maroua, University of Maroua, Maroua, Cameroon
School of Chemical Engineering and Mineral Industries, University of Ngaoundere, Ngaoundere, Cameroon
3
Department of Mechanical Engineering, ENSET, University of Douala, Douala, Cameroon
1
2
How to cite this paper: Gandai, D.K.,
Haman, Z., Frederic, D.P., Augustin, M.N.,
Nsangou, A., Blaise, N. and Valery, H.G.
(2024) Influence of Solvent onto Chemical
Extraction of America-Type Coconut (Coco nucifera L.) Fbers: Analysis of Physicochemical, Mechanical and Morphological
Properties. Journal of Textile Science and
Technology, 10, 64-81.
https://doi.org/10.4236/jtst.2024.103005
Received: June 12, 2024
Accepted: August 13, 2024
Published: August 16, 2024
Copyright © 2024 by author(s) and
Scientific Research Publishing Inc.
This work is licensed under the Creative
Commons Attribution International
License (CC BY 4.0).
http://creativecommons.org/licenses/by/4.0/
Open Access
DOI: 10.4236/jtst.2024.103005
Abstract
In this study, the natural fibers from Coconuts of the species Coco nucifera
L. were Chemically extracted in different solvents such as sodium hydroxide
(SH), acetone (AC) and sodium hydroxide-acetone (SHA) for their applications in the textile industries. Structural, morphological and physico-mechanical characterizations such as X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanned electron microscopy (SEM), measurements
of density, Young’s modulus, water absorption rate and humidity were evaluated. The XRD and FTIR results show that Coco nucifera L. fibers contains
type I cellulose. Mechanical characterizations were also carried out. These
results show that by varying the different solvents used, the physico-chemical,
mechanical and morphological properties of the fibers change, which implies
that the solvent has an influence on the properties of these fibers. The fibers
extracted by the sodium hydroxide-acetone mixture have a linear density of
1.636, the percentage of water absorption is 62.428%, the percentage of moisture absorption 9.605% compared to other values in the literature shows that
this solvent mixture improves the properties of coconut fibers which contain
type I cellulose. The tensile stress is 0.013 GPa, the percentage strain is
49.836% and the Young’s modulus is 0.114 GPa as well as the percentage
elongation show that these fibers are elasto-plastic. The values obtained mean
that these fibers are suitable for use in textiles.
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Keywords
Chemical Extraction, Cellulose, Coco nucifera L. Fibers, Elasto-Plastic,
Textiles
1. Introduction
Natural fibers account for a third of the world’s fiber production [1] [2]. Most of
these fibers are obtained from vegetable plants, animal hair or by chemical synthesis [3]-[7]. The various transformations undergone by these fibers enable
them to be used in a variety of sectors, including the clothing industry [8] [9],
civil engineering [10] [11], transport [12], medicine [13] [14], sport [15] [16],
furniture [17] [18] and agriculture [19].
The design of environmentally friendly materials is nowadays a requirement
of the scientific community, as this helps to protect the environment [20]. The
incorporation of new environmentally friendly materials is an inevitable necessity, along with improved extraction techniques that comply with the increasingly stringent environmental standards. The interesting specific properties of
these materials, their low density, their thermal insulation properties, and their
mechanical properties, particularly their biodegradability, open up promising
prospects [21]-[23]. Traditionally, coir fiber has been used to make rope for
cordage, sparterie (a woven, plaited or braided object), as a source of energy,
fishing nets, canvas, carpets, brushes, brooms or mattress padding. More recently, geotextiles made entirely from coir are being used to combat soil erosion.
There is also insulation in the form of flexible panels and plywood (fibers and
resins) [24]-[26].
Plant fibers are varied and can be used in a wide range of applications because,
for certain specific applications, they represent materials with technical performances that are sometimes superior to those of traditional materials [26] [27].
These new materials have developed very rapidly in recent decades. Numerous studies have highlighted the advantages and intrinsic limitations of these
materials.
The textile industry is therefore not immune to this requirement, and the various methods of extracting natural fibers, such as chemical extraction using bisulphite [28] [29], acid [30] [31], sodium hydroxide-anthraquinone [32] [33]
and neutral sodium sulphate [34], are often used, but these methods have their
limitations, being difficult and expensive to implement, and the various processes used are often not controlled. The sodium hydroxide and acetone extraction
technique developed in this work have a number of advantages, such as ease of
implementation, and the fibers obtained have good physicochemical and mechanical properties [35]-[37].
The aim of this work is to extract America-type Coconut (Coco nucifera L.)
fibers using sodium hydroxide, acetone to assess the influence of solvent onto
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different extraction methods and the physicochemical, mechanical and morphological properties are analyzed.
2. Materials and Methods
2.1. Sampling
Coconut fibers were extracted from Cocos nucifera L. fruits from Edea (Cameroon), in the Sanaga-Maritime department, in the sampling area with geographical coordinates of 3˚29' longitude North and 10˚06' latitude East. The reagents
used in this work are analytically reliable, therefore have not undergone any prior purification. Sodium hydroxide, acetone, xylene and acetic acid used are purchased from Sisco Research Laboratories pvt. Ltd., India. The extraction of fibers
involves three stages: pre-treatment, extraction and post-treatment.
2.2. Methods
2.2.1. Pre-Treatment
After sampling, Cocos nucifera L. fibers are pre-treated by simple scutching,
which removes impurities from the fibers using a knife. This operation is carried
out in two stages:
The first operation consists of cleaning the outer part of the coconut.
The second operation consists of separating the fibers from the outer part.
2.2.2. Extraction
1) Chemical Extraction with Sodium Hydroxide
For this treatment, 1g of Coco nucifera L. fibers flock was taken, making a total of nine (9) samples which were weighed. Another solution prepared with the
mixture sodium-hydroxide is used. The proportions of 50/50 are used for experimentation. Each of the weighed Coco nucifera L. fibers samples was then
soaked in the different solutions contained in a beaker and sealed with aluminium foil for 72 hours.
After this resting time, the samples are taken and rinsed with distilled water to
remove the residual pectin and hemicelluloses deposited on the fibers surface.
The fibers were then immersed in a neutralization bath containing 5 mL of 0.1
M acetic acid, followed by a second rinse. After these, the fibers were rinsed and
then dried in an oven at 65˚C for 24 hours.
3. Characterization Techniques for Coco nucifera L. Fibers
3.1. Physical Characteristics
3.1.1. Density Measurement
Two methods are used to measure the density and porosity of Coco nucifera L.
fibers.
‐ Pycnometer method
Various density measurements are carried out using a pycnometer (20 cm3).
The fibers were dried for 48 hours in a desiccator containing regenerated silica.
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The fibers are then cut into lengths of 4 to 5 mm and placed in the pycnometer,
which in turn is placed in the desiccators for at least 24 hours. Before weighing
with water, the fibers are impregnated for 2 hours. The micro-bubbles between
the fibers are practically evacuated. Each sample is weighed three times using a
Sartorius balance (1/1000).
The apparent density is expressed by:
(
) M −M[ −M× d − M ]
d e g cm3 =
e
E
E
T
(1)
e
Me: sample mass (alone) (g);
ME: mass of water (20 cm3) (g);
MT: sample mass plus water mass (all 20 cm3) (g);
dE: density of water = 0.997 (g/cm3) at 25˚C.
‐ Arthur’s method
This method consists of weighing the samples in air, then placing them in a
desiccator to release the air contained in the pores. A pump sucks the air out of
the desiccators for 30 minutes. They were then immersed in xylene for 10
minutes. The xylene-soaked samples are removed and lightly wiped dry. They
were then weighed in air and distilled water. The density and porosity are respectively given by the relationships:
(
) M −M[ −M× d − M ]
(2)
M xa − M e d E
× × 100
M xa − M x d x
(3)
d e g cm3 =
e
E
P=
0 (%)
E
T
e
With:
Me: mass of the sample in air (g);
Mxa: mass of the sample impregnated with xylene in air (g);
Mxe: mass of the sample impregnated with xylene in water (g);
dx: density of xylene = 0.880 (g/cm3).
3.1.2. Measuring the Rate of Water Uptake and Absorption
Knowing the water content of a textile material is very important. From an industrial point of view, this has an influence on the smooth running of the conversion and manufacturing process. From a commercial point of view, this parameter can modify the mass of a good from one environment to another, and
therefore from one country to another, hence the need to understand and control it in order to establish a common reference. And from a structural point of
view, humidity, in parallel with temperature, can alter the physical, chemical and
mechanical properties of the material.
1) The water absorption rate
The water absorption rate is defined as the quantity of water present in the air
that 100 g of dry matter can absorb under well-defined hygrometric conditions.
The gravimetric method is used in accordance with French standard NF G 08DOI: 10.4236/jtst.2024.103005
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001-4. The sample is dehydrated in an oven for 12 hours at 60˚C until it has a
constant anhydrous mass (Ms). The sample is then placed in a room where the
temperature is 22˚C and the relative humidity is 62%. The sample was weighed
every 15 minutes. The measurement is considered complete when two successive
weighing give a difference of less than or equal to 5% of the sample mass.
2) Absorption rate
The moisture content is assessed by the total saturation method, in accordance with the standard (AATCC 20A). The sample is placed in a desiccator for
30 days at a humidity of 65% ± 5% and a temperature of 25˚C. After weighing
(Mm), the sample was dried in an oven at 105˚C ± 5˚C for 15 h. It was then
cooled in desiccators and weighed (Ms). The samples are weighed repeatedly until the weight (Ms) is constant due to drying and cooling. The moisture content
(TH %) of the fiber is calculated by :
=
TH ( % )
Mm − Ms
× 100%
Ms
(4)
With:
Mm: initial mass of the sample.
Ms: mass of the sample after exposure to the humid environment.
3.2. Structural Characterization
Numerous techniques are used to characterize the microstructure of Coco nucifera L. fibers.
3.2.1. X-Ray Diffraction
X-ray diffraction tests are carried out using a Bruker D8 diffractometer. Samples
are dry ground in a ceramic mortar to a size of less than 125 μm. The anticathode is copper (Kα =1.54 Å). The scan angle (2θ) is between 5˚ and 75˚ with a
step size of 0.02˚.
Various physical methods have been proposed in the literature for determining the crystallinity ratio of cellulosic fibers. According to Segal’s method [38]
the crystallinity index Ic, is determined by:
=
I cr
I 002 − I am
× 100
I 002
(5)
I002 is the maximum intensity of the spectrum (amorphous and crystalline).
Iam is the maximum intensity of the amorphous part.
The crystallite size is calculated using Sherrer equation below:
D ( nm ) =
kλ
β cos θ
(6)
where:
k is Sherrer constant, 0.68 to 2.08, 0.94 for spherical crystallites with cubic
symmetry;
λ is the X-ray wavelength equal to 1.5406 Å;
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β is the line broadening at FWHM in radians;
θ is the Bragg’s angle in degrees.
3.2.2. Fourier Transform Infrared Spectrometry (FTIR)
Samples of Coco nucifera L. fibers were ground and dried in an oven to remove
absorbed moisture. These samples are then mixed with potassium bromide (5%
KBr) and pressed into a small pellet approximately 1 mm thick. Infrared spectra
were taken using a Perkin Elmer spectrometer. The samples were scanned at 400
and 4000 cm−1 with a resolution of 2 cm−1.
3.2.3. Morphological Analysis
Scanning Electron Microscopy (SEM) micrographs of the coir fibers were taken
using a Hitachi (Japan) S-3000H electron microscope with an accelerating voltage of 15 kV. SEM is a widely used technique for investigating surface morphology such as roughness or porosity (from secondary electrons) and chemical
composition (from backscattered electrons) of most solid materials. A beam of
electrons emitted by a cathode bombards a sample, then the interaction between
these electrons and the surface provides signals that are detected, amplified and
used to reconstruct the image seen on the screen.
3.2.4. Fiber Tensile Tests
The fibers were tested on an MTS tensile testing machine in accordance with
ASTM D3379-75 “Standard Tensile Method” [39]. The tensile testing of coir fibers was carried out in accordance with ISO 5079, using a universal testing machine and Test Master software for machine control and data processing.
The diameter of each sample was first measured using a micrometer, and then
recorded in the machine. The samples are then glued to the sample holders and
fixed to the jaws of the testing machine. The edges of the sample holders are cut
so that only the fiber is stressed in tension, and a laying tension is applied to the
fiber. All the machine’s sensors are then set to zero, and a load of 5 kN is applied
to the sample at a speed of 5 mm/min. After the test, the data and all the technical parameters (Young’s modulus, maximum resistance, elastic resistance, deformation, etc.) are recorded.
4. Results and Discussion
4.1. Structural and Functional Characterizations
• X-ray diffraction analysis
Figure 1 shows diffractograms of treated and untreated coco nucifera L. fibers. The major peak is recorded for coco nucifera L. fibers extracted by sodium
hydroxide-acetone at a diffraction angle of 2Ɵ = 22.16˚, which corresponds to
the (002) crystallographic plane. Another peak also appeared in the diffractogram, one at an angle of 2θ = 15.89˚ which corresponds to the (111) crystallographic planes. The (002) crystallographic plane represents the crystalline part of
the cellulose, while the amorphous part appears at 2θ = 15.89˚. According to
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equation (5) the crystallinity index Ic for the higher peak is calculated and equal
to 56.99% which shows that extraction using the sodium hydroxide-acetone
mixture resulted in cellulose with a predominantly crystalline phase. The average
of crystallite size is calculated according to Sherrer equation and is equal to 1.92
x 10−3 Å.
Figure 1. X-ray diffractograms of (a) Untreated Coco nucifera L. fibers and (b) Coco nucifera L. fibers extracted by acetone (c) Coco nucifera L. fibers extracted by sodium hydroxide (d) Coco nucifera L. fibers extracted by sodium hydroxide-acetone.
• Fourier Transform Infrared Spectroscopy (FTIR)
Figure 2 shows the FTIR spectra of untreated and treated Coco nucifera L. fibers. The different absorption bands are characteristic of Coco nucifera L. fibers.
These different spectra do not show any significant differences between the
peaks. The peak observed at a wavelength of 3347 cm−1 corresponds to the O-H
group (stretching of the hydroxyl bond) of the cellulose. The peak at 2925 cm−1
corresponds to the C-H elongation vibrations of the cellulose. The peak at 1597
cm−1 shows the presence of the C-C group in lignin, which has been considerably
reduced. Similarly, the peak at 1231 cm−1, which corresponds to the C-O elongation of the acetyl groups in lignin, underwent a decrease. An intense band at
1032 cm−1 with a shoulder corresponding to the end of the stretching modes of
the C-O acetyl groups increased sharply in intensity; partly because of the increase in the proportion of cellulose in the fibers. The spectra relating to the different IR treatments have a significant influence on the structure of the fibers
treatments. The presence of lignin peaks in the fibers spectra shows that the fibers still contain lignin.
• Morphological analysis
According to the images obtained by scanning electron microscopy (SEM) in
Figure 3(a), Coco nucifera L. fibers has a very clean, smooth surface, free of
non-cellulosic matter. Several authors [40] [41] have shown that treating fibers
with basic solutions cleans the surface by degrading amorphous constituents
such as lignins, hemicelluloses, waxes and fats, since they are soluble in an
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aqueous NaOH solution. This treatment cleaned the micropores in the fibers
and made the surface smoother with a reduction in diameter. Figure 3(b), Figure 3(c) and Figure 3(d), on the other hand, show the presence of debris with a
rough surface. This always explains the presence of other bodies such as lignins,
hemicelluloses or pectins, waxes and fats. Removal of the hemicellulose gives the
cellulose fibrils freedom of movement in the direction of tensile deformation,
which increases the tensile strength and surface roughness of the fiber.
Figure 2. IR spectra of (a) Untreated Coco nucifera L. fibers and (b) Coco nucifera L. fibers extracted by sodium hydroxide (c) Coco nucifera L. fibers extracted by acetone (d)
Coco nucifera L. fibers extracted by sodium hydroxide-acetone.
Figure 3. SEM analysis of (a) Untreated Coco nucifera L. fibers and (b) Coco nucifera L.
fibers extracted by sodium hydroxide (c) Coco nucifera L. fibers extracted by acetone (d)
Coco nucifera L. fibers extracted by sodium hydroxide-acetone.
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4.2. Physical Characteristics
• Density
Figure 4 shows the different densities of fibers treated with different solvents. These density values of between 1.636 and 1.066 are not too far removed
from the densities of other plant fibers such as cotton = 1.55, flax = 1.33, sisal
= 1.53, alfa = 1.51, jute = 1.44, coir = 1.2, hemp = 1.07 [42]. When lignin, pectins and hemicelluloses are less present in the sample, its density is higher. This
density measurement is therefore also a means of verifying the elimination of
non-cellulosic matter. Comparison of the values obtained with those for plant
fibers shows that the density of coconut fibers is within the average range for this
type of fiber. It should be noted that these fibers show interesting results due to
the absence of lignin, pectins and hemicelluloses.
Figure 4. Density of different coco nucifera L. fibers.
• Measurement of water absorption percentage
Figure 5 below shows the histograms of the water absorption percentages of
the fibers treated with the different solvents. These results show that the water
absorption rate is 62.428% which can be explained by the fact that during this
chemical extraction based on the sodium hydroxide-acetone mixture, these two
solvents being polar favoured a better extraction of the fibers allowing the cellulose contained in these fibers to be less encumbered and thus to easily absorb
water.
• Measurement of moisture uptake
The histograms presented in Figure 6 below show the moisture content of the
different fibers after extraction in different solvents. These results show that the
moisture content varies from 9.605 to 7.793, which are values close to those
found in the literature [43]-[45]. The values found indicate that a product made
from these fibers will offer a fairly good feeling of comfort, since it will absorb
up to 9% moisture, a value very close to that of cotton (7% - 8%) and jute (12%).
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Figure 5. Water absorption percentage of different coco nucifera L. fibers.
Figure 6. Moisture absorption of different coco nucifera L. fibers.
4.3. Mechanical Characterization of Coconut Fibers
Figure 7 shows the values for mechanical strength of untreated and treated of
coco nucifera L. fibers. Sodium hydroxide-Acetone (SHA) extraction of coco
nucifera L. fibers increases their mechanical strength.
As for fiber deformation, the difference between these values means that the
treatment has effect on fiber deformation (see Figure 8).
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Figure 7. Mechanical strength of different coco nucifera L. fibers.
Figure 8. Deformation of coco nucifera L. fibers.
Young’s modulus, which is the fibers resistance to deformation, shows a significant difference in the values obtained between the different treated fibers (see
Figure 9). This reflects the beneficial effect of the treatment, which makes the
fibers more resistant to deformation. This is undoubtedly due to the presence of
hydroxyl groups on the surface areas of these fibers, as shown by the FTIR analyses. These groups are responsible for the formation of strong bonds and Van
Der Valls bonds, and favour the establishment of mechanical bonds.
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Figure 9. Young’s modulus differents coco nucifera L. fibers.
The force required to break the fiber is known as its tensile strength. The
more resistant a fiber is before breaking, the higher its tensile strength. The mechanical tests carried out on the coconut fibers are tensile tests which gave the
result of the tensile force and the elongation of the fiber during traction. These
results are expressed by curves giving force as a function of elongation as shown
in Figure 10. The slopes of these curves enabled us to determine the different
Young’s moduli of each type of fiber extracted.
Figure 10. Tensile curves for coco nucifera L. fiber(CNF), coco nucifera L. fiber extracted
by Sodium Hydroxyde (SH), coco nucifera L. fiber extracted by Acetone (AC) and coco
nucifera L. fiber extracted by mixture Sodium Hydroxyde-Acetone (SHA).
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The results of the tensile test showed that the tensile strength of coconut fibers
(see Figure 10) is 0.006 Gpa, 0.012 Gpa, 0.011 Gpa, and 0.013 GPa respectively
for coco nucifera L. fibers (CNF), coco nucifera L. fiber extracted by Sodium
Hydroxyde (SH), coco nucifera L. fibers extracted by Acetone (AC) and coco
nucifera L. fibers extracted by mixture Sodium Hydroxyde-Acetone (SHA
(Table 1). These values are much lower than those of the other fibers presented
in Table 1, obtained from the literature, such as cotton, kenaf, sisal and hemp,
whose tensile strength is 0.287 - 0.597 GPa, 0.7 GPa, 0.6 GPa, 0.69 GPa and GPa
respectively. On the other hand, the elasticity of coconut fibers was higher compared with the same fibers. Coconut fibers appear to be more flexible although
they have a low tensile strength. Mechanical properties are directly related to
molecular structure properties, fiber length, microfibrillar angle, cellulose content, fiber orientation and cellulose crystallinity. The mechanical characterization carried out is tensile strength to better understand the behaviour of different
fibers. It was found that the best extraction of Coco nucifera L. fibers was
achieved with sodium hydroxide (0.1 mol/L) diluted with acetone in proportions
of 50/50, while the best.
Table 1. Mechanical properties of coconut fibers obtained by different treatments and some vegetable fibers.
Fibers
Tensile Stress (GPa)
Elongation (%)
Young’s Modulus (GPa)
References
Cotton
0.287 - 0.597
7-8
0.005 - 0.012
[46]
Kenaf
0.7
3
0.055
[47]
Linen
0.345 - 1.035
1.3 - 3.3
0.027
[48]
Sisal
0.6
3
0.012
[49]
Jute
0.396 - 0.773
1.5 - 1.8
0.026
[50]
Hemp
0.690
1.6
0.03 - 0.06
[48]
SHA
0.013
49.84
0.114
Present work
SH
0.012
46.70
0.100
Present work
AC
0.011
39.44
0.090
Present work
CNF
0.006
22.03
0.052
Present work
5. Conclusion
The chemical extraction of coconut fibers has been carried out. However, the
experiments focused on chemical extraction with the aim of proposing an appropriate method for this fiber. The work involved cleaning the outer part of the
coconut fiber flock, then separating the fibers from the inner part. The fibers extracted by the sodium hydroxide-acetone mixture present a linear density of
1.636, the percentage of water absorption of 62.428%, the percentage of moisture
absorption of 9.605% compared to other values in the literature shows that this
solvent mixture improves the properties of coconut fibers which contains type I
cellulose. The tensile stress is 0.013 GPa, the percentage of deformation is
49.836% and the Young’s modulus is 0.114 GPa as well as the percentage of
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elongation show that these fibers are elasto-plastic. After physical, structural and
mechanical characterization, the results show that these fibers can be used in
textiles and in other applications as composite materials. The perspectives of this
work can be focused on the reaction mechanism of chemical extraction, carry
out a thermodynamic and kinetic study.
Conflicts of Interest
The authors unanimously declare that they have no known competitive financial
interests or personal connections likely to influence the work reported in this article.
Acknowledgements
The outcome of this work finds satisfaction in the financial support granted by
the Council for Scientific and Industrial Research (CSIR), by the World Academy of Sciences for the Advancement of Science in Developing Countries
(TWAS) in the Analysis Center of the Faculty of Sciences and Techniques of the
Sultan Moulay Slimane University of Beni-Mellal (Morocco).
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DOI: 10.4236/jtst.2024.103005
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