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Synthesis and Characterization of Mesoporous Silica Nanoparticles from

Jordanian Glass Sand

Article in Russian Journal of General Chemistry · December 2023

DOI: 10.1134/S1070363223110269

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ISSN 1070-3632, Russian Journal of General Chemistry, 2023, Vol. 93, No. 11, pp. 2941–2947. © Pleiades Publishing, Ltd., 2023.

Synthesis and Characterization

of Mesoporous Silica Nanoparticles from Jordanian Glass Sand
M. Al-Bashabsheha and R. M. A. Q. Jamhoura,*
a Department of Chemistry and Chemical Technology, Tafila Technical University, Tafila, 66110 Jordan
*e-mail: rasheedjamhour@gmail.com

Received September 28, 2023; revised October 30, 2023; accepted November 13, 2023

Abstract—The amorphous mesoporous silica was successfully synthesized from Jordanian desert glass sand
sources. Sodium silicate solution (SSS) was synthesized from glass sand, then silica nanoparticles (SNPs) was
synthesized, using sodium silicate solution as a precursor by sol-gel method. The synthesized mesoporous silica
has a high specific surface area of 50.954 m2/g, pore volume of 0.058 cc/g, average pore diameter in mesoporous
range of 2.89 nm, and relatively acidic surface value with pH point zero charges pHpzc = 6.7. The effect of pH value
in gelation and polymerization colloidal silica was investigated, the synthesized mass of SNPs by this method was
investigated and checked by FTIR and atomic absorption spectrophotometry. The results were excellent in terms
of Si purity. Surface and physical tests for calcinated Jordanian silica nanoparticles (JSNPs) were done, including
SEM EDX imaging, and BET surface analysis.
Keywords: mesoporous silica nanoparticles, sol-gel method, mesoporous silica, glass sand
DOI: 10.1134/S1070363223110269

INTRODUCTION variety of applications because they contain huge surface

Southern Jordan sand contains various important
components such as silica. composition depending on
their geographical location. Utilizing silica-rich desert
sand for producing high-value products can have both
environmental and industrial benefits [1–4]. It can reduce
the need for mining silica from traditional sources, thus
minimizing the environmental impact. Additionally,
it promotes local resource utilization and economic
development. Silica or silicon dioxide has numerous
applications across industries. Their use as adsorbents,
desiccants, filtration technology, and catalyst support-
mesoporous components underscores their importance
in industries ranging from environmental remediation to
chemical manufacturing [5–8]. In general, the prospect of
transforming high-silica-content desert sand into useful
and valuable materials is exciting. It is consistent with
the principles of sustainability, resource efficiency, and
sustainability, and has the potential to progress many
different industries. This material shows great promises in
the adsorbent and catalyst industry if treated or converted
into mesoporous material [9]. The transforming silica-
based materials into mesoporous structures is particularly
interesting. Mesoporous materials are excellent for a
areas and clearly defined pore structures. The material's
functionality and performance can be considerably
improved by this change. Mesoporous structure is
believed to have improved catalytic activity because
it can resolve and prevent the diffusion constraint of
large molecules during the catalytic process [10]. There
are several synthesis methods to achieve mesoporous
silica material, such as hydrothermal, sol-gel, and the
latest sonochemical synthesis [11]. Previous literature
stated that alkaline medium could affect the control of
mesoporous size distribution using sol-gel methods,
hence, making it easier to control the material porosity
[12]. Famous ordered mesoporous silica that is known
for its ordered porosity and exceptional performance in
a range of applications. These materials are commonly
produced using sodium silicate solution or tetraethyl
orthosilicate (TEOS) [13]. These examples demonstrated
silica's enormous adaptability as a catalyst and its
potential for usage in a variety of different applications.
The advancement in nanomaterial technology opened a
wide range of research specially in electronics, photonics,
and energy harvesting and storage, utilizing the silica
nanoparticles SNPs with high demand [14]. Additionally,

2941
2942 AL-BASHABSHEH, JAMHOUR
Table 1. Elemental chemical composition of the prepared silica nanoparticles
Element Oxide
Si SiO2
Al Al2O3
Fe Fe2O3
Mg MgO
Ca CaO
Na Na2O
K K2O
SNPs are more efficient than other nanomaterials at
lowering the viscosity of crude oil [15]. Different ways
are used to produce SNPs depending on the raw materials
used, the process of preparation variables conditions such
temperature, precipitation time, pH, coagulant addition,
and drying processes. These variables directly affect the
size, aggregation, and specific surface area of the SiO2
nanoparticles [16]. Sol-gel techniques are among the
techniques used to produce mesoporous silica MSNs
with a nanoscale particle suitable for the abovementioned
applications. Since water is the most commonly used
solvent to prepare MSNs via the sol-gel reaction [17].
In this study, the silica content in Jordanian desert
sand was used to synthesize silica and mesoporous silica
using the sol-gel method.
RESULTS AND DISCUSSION
Nano silica and xerogel. Jordanian desert sand
samples that were used in this research were collected
from five different locations each sample weighs 200 g.
Sodium silicate solution was prepared by the reaction
between sodium hydroxide and silica to form silicic acid
then crystallization followed by polymerization.
SiO 2(s ) + 2NaOH (aq) → Na 2SiO3(aq) + H 2 O(l) ,
H 2SiO3( aq ) + H 2 O( aq ) → Si ( OH )4 ,
Si ( OH )4 ↔ SiO 2(s) ↓ + 2H 2 O(l) ,
OH OH
n[Si(OH)4 + (OH)4Si] HO−Si−O−Si−OH
OH OH
Element content, wt % Conservation factor
0.4674 2.1393
0.5293 1.8895
0.6994 1.4297
0.6030 1.6583
0.7147 1.3992
0.7419 1.3480
0.8301 1.2046
The elemental composition of each sample was
calculated as follows, %:
SiO
= 2 100 − ∑ (mineral oxide + moisture of sample).
The weight percent of oxides was estimated by
calculating the percent concentration of counter ions
Na+, K+, and Al+3, by AAS, then changing the percent
concentration of counter ions to the percent concentration
of oxides form by multiplying the percent concentration
of each of counter ions by oxide conservation factor
[21]. This approach assumes that all of the counter ions
are present in the sample in the form of the specified
oxides. The conservation factor essentially adjusts for the
difference in molecular weight or equivalents between the
counter ions and the corresponding oxides. It's important
to note that the validity of this conversion relies on the
assumption that the elements are present in the sample
in the specified chemical forms. Additionally, the
conservation factors should be based on the stoichiometry
of the compounds involved, which can be obtained
from the chemical formulas of the oxides as shown in
(Table 1). It can be seen that SiO2 obtained from the
previous calculation step was similar to a commercially
(1) available SiO2. In general, SiO2 is a white, brittle powder,
which makes it easier to grind. AAS analysis was then
(2) carried out on the composition of the powder with the
corresponding statistical analysis. It can be seen that
(3) Jordanian sand can serve as a source for silica with high
purity and potential as silica nanoparticles source.
Moreover, the quantitative chemical analysis of JSNPs
+2nH2O. and the data reflect the high purity of silica. Table 2 shows
the elemental composition of the produced sample with
all possible impurities, moisture and the loss-on-ignition
(4)
(LOI). The silica content is increased due to the formation
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 93 No. 11 2023
 SYNTHESIS AND CHARACTERIZATION OF MESOPOROUS SILICA NANOPARTICLES 2943

Table 2. Statistical and quantitative analysis of the sand com- treated thermally to create a thermodynamically stable
posite oxide, such as SiO2. Calcination degrades sparingly
Chemical composition, wt %a ±SD %RSD thermally soluble oxides as metal carbonates, hydroxides,
Na2O 0.0511 0.00106 2.0728 and oxalates. For ceramic powders, this process is needed
K2O 0.0325 0.00035 1.0817 for purification. The FT-IR spectra shows a disappearance
Al2O3 0.6537 0.00711 1.0883 of the broad band caused by hydroxyls and adsorbed water
Fe2O3 0.0866 0.00165 1.9063 by silica around (3000–3800 cm–1), this indicates that
MgO 0.6123 0.01343 2.1931 water and hydroxyl groups were removed after thermal
CaO 0.5257 0.01704 3.2414 calcination in air furnace at 900°C and a stable SiO2 was
L.O.I 0.0228 0.00025 1.1054 formed.
Moisture 0.0823 0.00296 3.5915 Zeta potential for colloid JSNPs. ζ-Potential
*∑ (Average wt % for 3 trials) = 2.07%. titration was done for synthesized colloidal JSNPs using
ζ-potential analyzer SurPASS 3 (Fig. 1). To investigate
the physical properties of colloidal SNPs, like isoelectric
of silica nano particles during the reaction, while the point (IEP), and their stability behavior. Any particle in
compounds which is considered as impurities presented suspension will display the physical characteristic known
below is decreased, so it is obvious that the chemical as zeta potential, which is the charge that forms at the
sol-gel method is a good example of decreasing the interface between a solid surface and its liquid medium.
impurities. The data below indicate a percentage purity of The most crucial factor for zeta potential is pH value.
97.93% for the SiO2 which was obtained by subtraction Adding acid would cause the pH of the suspension to
the total impurity of 2.07%. drop, increasing the positive charges on the surface of the
FT-IR analysis. The presence of silica was confirmed particles. The zeta potential, also known as the isoelectric
by FT-IR data for the synthesized SNPs without point, is the location where there is no electrophoretic
calcination (dried sample at 108°C). The peaks at 458 mobility. When the zeta potential of a nanoparticle
and 578 cm–1 are caused by bending vibrations with is between –10 and +10 mV, it is said to be neutral
asymmetric stretching vibration for Si–O–Si (siloxane approximately, however, while nanoparticles with zeta
group). The band at 850 cm–1 represents the bending potentials of greater than +30 mV strongly cationic, if
wagging vibration for Si–O–Si, strong infrared bands can zeta less than –30 mV strongly anionic. Zeta potential
be observed one or more in siloxanes Si–O–Si between is a measurement of the potential difference between
850 and 1334 cm–1 with asymmetric stretching vibration the layer of fluid containing the oppositely charged ions
[22]. The Si–O–Si absorption becomes broader and that is connected to the surface of a nanoparticle and the
more complex as the siloxane chains lengthen or branch, bulk fluid in which the particle is dispersed [25]. The pH
resulting in two or more overlapping bands [23]. The of zero charge (pHpzc), for JSNPS was measured using
band at 458 cm–1 and the band at 578 cm–1 associated pH drift method, nine trials of 0.01 M NaCl each trial in
with the Si–O rocking. The broad band at 3500 cm–1 50 mL were prepared. Solutions represent different pH
appeared from the stretching vibration of O–H from value from 3–11 (Fig. 2).
adsorbed water, H–OH. The adsorbed water represents The colloidal silica is extraordinarily stable at
by the bending scissoring vibration for H2O was also pH = 2.7 where the zeta potential is zero and IEP
confirmed with the appearance of a peak at 1640 cm–1, become increasingly sensitive electrolyte at higher pH
which was also assigned to be water that binds to Si–OH. value, this indicate that at pH > 2.7, the surfaces will be
The transmitted peaks at (3000–3900 cm–1) caused by functionalized with negative charge of SiO– groups [26].
Stretching vibration, the appearance of these distinctive The particles in colloidal silica are stable above pH 7
peaks confirms the presence of the Si–O–Si band, the that can be observed for SNPs when pH stands between
Si–OH band, and the H–O–H band in silica, (variant 7 and 10.5.
types of hydroxyls), as well as the residual adsorbed At low pH < 1, complete hydrolysis achieved, slow
water [24]. Spectra in supplementary shows the FT-IR and little polymerization. At pH = 2, full hydrolysis
analysis for synthesized SNPs from Jordanian glass sand achieved, isoelectric charge, no polymerization or
after calcination. By calcination, metal oxide powders are gelation process, with high protonated of orthosilicic acid,
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 93 No. 11 2023
2944 AL-BASHABSHEH, JAMHOUR

10
pH pH = 2.7 Isocritical point (IEP)
0
0 2 4 6 8 10
–10 Unstable
ζ-Potential

–20 ty

–30

–40
± 40 to 60 Stable
–50
ty Si(OH)4 neutral
–60
pH
60

40

stability reference
20
ζ-Potential

ζ-Potential
0

–20

–40

–60
2 4 6 8 10 12

Fig. 1. Zeta potentiometric titration result for synthesized JNSPs, calcinated form.

no negative charge, no nucleophilic attack on Si atom, no
polymerization or gelation. This explains why NSPS has
high solubility in acidic media. When the pH increased
to 4–6, condensation reaction occurs due to nucleophilic
attacking, polymerization and gelation processes.
The negatively charged silicates would increase the
condensation rate because of the favored nucleophilic
attack [27]. At higher pH = 9–10.5 negative charge
increases, so nucleophilic attack appeared, decreasing
of OH group which linked with Si atom, siloxane bonds
Si–O–Si for certain monomeric silanols are hydrolyzed
very slowly from silica supports.
Pore size examination for calcinated JSNPs. The
synthesized silica was analyzed by Quantachrome gas
sorption analyzer (GSA). To determine their porosity
character [28]. The isotherm graph and specific surface
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 93 No. 11 2023
area were determined using the BET equation. Pore
volume, average pore diameter, and pore size distribution
were determined and found to be: pore volume =
0.058 cc/g, surface area = 50.954 m2/g, and pore width
2.89 nm, respectively for calcinated JNSPs. The pore size
distribution was relatively homogenous.
Scanning electron microscopic (SEM) analysis
for silica nanoparticles. Characterization of JNSPs
with SEM-EDX was done to reveal the morphology of
synthesized silica structure. SEM imaging was necessary
to characterize the 3D surface morphology of colloid
silica shown in Fig. 3a. It can be seen that the morphology
of colloidal JNSPs had homogeneity in size and spherical
shape, with a diameter of 90.8 nm; on the other hand,
some spherical particles attached to each other due to
 SYNTHESIS AND CHARACTERIZATION OF MESOPOROUS SILICA NANOPARTICLES 2945

Fig. 2. pHpzc (point zero charge) for JSNP. 1 – linear relation between initial and final pH values, 2 – pH value for NaCl and silica
nanoparticles.

Fig. 3. SEM for synthesized JSNPs: (a) colloid form, (b) calcinated form.

siloxane bond formation, Si–O–Si, and the release of CONCLUSION

water (condensation reaction) [29].
Figure 3b shows flat sheets shape for JSNPs calcinated
powder form, as shown, the use of thermal treatment
by calcination at 900°C to remove impurities and
purification, and to increase decomposition and water
removing. By viewing EDX data, in supplementary
information, JSNPs sand contains quarts’ silicon (SiO2) as
a major mineral that might be found in Jordanian desert.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 93 No. 11 2023
Jordanian desert sand was successfully used as a
silica source for mesoporous silica synthesis with high
porosity properties. JSNPs has a specific surface area
of 50.954 m2/g, a total pore volume of 0.058 cc/g, and
an average pore diameter of 2.89 nm. The presence of
silica formation and subsequent characterization was
supported by absorption spectroscopy, FT-IR, SEM and
2946 AL-BASHABSHEH, JAMHOUR
EDX imaging. This study also found the pH of zero charge
and zeta potential for the synthesized mesoporous silica.
In summary, the desert silica sand can be utilized by an
efficient sol-gel synthesis and be an alternative source to
synthesize silica nanoparticles that can be used not only
as super hydrophobic material but also in many other
important industrial applications as reported in this study.
EXPERIMENTAL
The desert sand was collected from Ras En Naqb 70
km northeast of Aqaba in south Jordan. All chemicals
used in this work are analytical grade without any
purification and were purchased from Sigma-Aldrich,
Merck company. Perchloric acid (70%), hydrochloric
acid (37%), sodium hydroxide (≥ 99%), EDTA (99.9%),
silver nitrate, pyridine (Sigma Aldrich), buffer solutions
(pH = 2, 4, 8, 10, and 12), multi-element standard solution
(Na, K, Fe, Al, and Ti) 1000 ppm, silica standard solution
1000 ppm, and finally, lead standard solution Pb(II)
1000 ppm were used.
Mesoporous silica synthesis. Mesoporous silica
was synthesized from desert sand that is rich with SiO2.
The sand was washed several times with distilled water
and with 0.5 M HCl to remove organic and insoluble
impurities and then washed again with water to remove
excess HCl, before air dried. The composite sand sample
was screened in Tyler screen sieves (325 microns) to
reduce the size of silica sand and increase the surface area
of the sand particle. A 100 g of the sample was transferred
to a round bottom flask, with 500 mL of 10 M NaOH to
reaction mixture then condensed at a temperature adjusted
to 300°C for 3 h. Followed by room temperature cooling.
To eliminate unreacted sand particles, the filtrate was
first separated from the solid using filter paper by simple
filtering. It was then moved to a sonicator with an ice
bath, a pH electrode was added to monitor the filtrate
pH. Concentrated HCl (6 M) was applied gradually and
dropwise until pH = 7. The solution mixture was sonicated
for 30 min. Silicic acid, a white slurry, was formed. To
speed up drying and polymerization, the reaction mixture
was left to stand overnight at room temperature [18].
Synthesis of a pure nano silica particle (NSP) by
calcination of an xerogel. After settling down, the white
gel was separated from the solution by simple filtration
with care to prevent gel damage as mentioned above.
The white gel was transferred in a Porcelain container
and thermally dried in the oven at 108°C. The xerogel
formed then transferred into the centrifuge tube then
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 93 No. 11 2023
distilled water added, and the solution centrifuged for
10 min in 5 circles at 5000 rpm at room temperature.
Water was decanted from the tube. This was repeated
twice to remove all sodium and other impurities. Decanted
water was checked by using dilute AgNO3 solution, to
ensure full removal for NaCl. The white transparent gel
was transferred from the tube and placed in a Platinum
crucible, then dried at 108°C in the oven, then placed at
900°C in a furnace for calcination [19].
Characterization of mesoporous silica. The
chemical composition of the mesoporous silica was
analyzed by qualitative identification of functional groups
presence and/ or disappearance of the main characteristics
peaks on silica, using FTIR spectrometer with KBr disc
technique. Pore size and volume were analyzed using
N2 gas sorption analysis which was carried out using
Quanthachrome NOVA touch. Adsorption and desorption
isotherms were calculated by the multipoint method. The
total surface areas were measured by the BET method.
Quantachrome desorption model was used to provide pore
size distribution. Morphology of mesoporous silica was
characterized using scanning electron microscope and
transmission electron microscope to analyze its pore’s
structure [20]. Atomic absorption spectrophotometer
ContrAA 800 F (Analytik Jena, Germany) with xenon
lamp for all element was used. The acidity of sand, and
mesoporous silica was analyzed using ζ-potential analyzer
SurPASS 3 (Anton Paar, Austria).
FUNDING
This work was supported by ongoing institutional funding.
No additional grants to carry out or direct this particular
research were obtained.
CONFLICT OF INTEREST
The authors declare no conflict of interest.
SUPPLEMENTARY INFORMATION
The online version contains supplementary material
available at https://doi.org/10.1134/S1070363223110269.
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