Results in Physics 11 (2018) 23–29

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Results in Physics
journal homepage: www.elsevier.com/locate/rinp

Removal of As(V) from aqueous solution by using cement-porous hematite T

composite granules as adsorbent
⁎
Wangyang Xua, Bingqiao Yangb, , Feifei Jiaa,c, Tianxing Chena, Lang Yanga, Shaoxian Songa,c,d
a
School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, 430070 Wuhan, Hubei, China
b
School of Xingfa Mining Engineering, Wuhan Institute of Technology, Xiongchu Road 693, Wuhan 430073, Hubei, China
c
Hubei Key Laboratory of Mineral Resources Processing and Environment, Wuhan University of Technology, Luoshi Road 122, 430070 Wuhan, Hubei, China
d
Hubei Provincial Collaborative Innovation Center for High Efficient Utilization of Vanadium Resources, Wuhan University of Technology, Luoshi Road 122, 430070
Wuhan, Hubei, China

A R T I C LE I N FO A B S T R A C T

Keywords: The potential of using Portland cement-porous hematite composite granules (CHG) as a new adsorbent for the
Porous hematite adsorption of As(V) from aqueous solution was investigated in this study. This research was performed through
Portland cement the measurements of adsorption isotherm, adsorption kinetics, X-ray diffraction (XRD), mercury intrusion por-
Granule osimetry (MIP), scanning electron microscope (SEM) and energy dispersive X-ray detector (EDX). The pore
As(V) adsorption
structure of CHG was extraordinary developed with the porosity, the total pore volume and the average pore
Solid-liquid separation
diameter being 45.48%, 0.3586 mL/g and 62.7 nm, respectively. From the adsorption batch of As(V) on porous
hematite and CHG, CHG exhibited a high adsorption capacity of 9.84 mg/g for As(V), slightly lower than the
porous hematite adsorbent. It was observed that CHG kept greater than 83% adsorption capacity of the porous
hematite. However, CHG was convenient in solid-liquid separation after adsorption benefited from its high
mechanical strength, stability in solutions and big size, which could be separated directly from the water without
any other equipment and technology. As a result, this work provides a theoretical basis for the practical ap-
plication of granular adsorbents to the actual As(V) sewage.

Introduction
Arsenic contamination in natural water has been a worldwide en-
vironmental problem as it provokes toxic effects on biota [1–4]. It has
been implicated in accidents with human disease or death [5,6], con-
tributing to the long-time exposure and consumption [7–10]. Therefore,
the removal of arsenic contamination from aqueous solution is very
crucial. Various technologies have been developed to remove arsenic
from water [11,12], such as coagulation, adsorption [13–15], ion ex-
change, membrane filtration, capacitive deionization (CDI) [16–18]
and bioremediation [19–22]. Among these technologies, adsorption is a
dominant method due to its simple operation, low cost, regeneration
capacity, and no chemical addition [16,23].
To enhance the removal efficiency, miscellaneous adsorbents has
been researched [24,25]. Due to the low cost, strong affinity and high
selectivity for inorganic arsenic species in sorption processes [26], iron
minerals are considered as effective adsorbents for arsenic removal
[27–30]. However, the low surface area and large dosage of the natural
iron minerals limit the arsenic removal efficiency. Therefore, arsenic
adsorption with porous iron oxides has aroused more attentions re-
cently, which can overcome the smaller specific surface and large do-
sage disadvantage of natural iron ore and the complex production
process and high cost shortcoming of synthetic iron ore [31,32].
Thermal modification is one of economical and effective means
[33,34]. It was reported that thermal decomposition of hydrous, hy-
droxy and carbonate minerals (e.g., limonite, goethite and siderite) was
an effective method to produce porous hematite with a large surface
area and uniform pores [35,36]. Nevertheless, much difficulty in ad-
sorption process limited the applications of traditional porous hematite.
As the traditional adsorbents are usually in powders with fine particle
size, they can’t be applied directly in large-scale applications due to
their drawbacks in separation and recycle.
Granular-based adsorption gained impetus for pollutants removal
toward industrial applications in recent years [37,38]. It is obvious that
the adsorption of granule has a simple treatment process, less con-
sumption of power and a convenience in separation when the granular
adsorbents are being applied to the actual treatment, which can de-
crease the cost of its transportation, operation and storage [39].

⁎
Corresponding author.
E-mail address: yanglin538@163.com (B. Yang).

https://doi.org/10.1016/j.rinp.2018.08.031
Received 29 June 2018; Received in revised form 26 July 2018; Accepted 15 August 2018
Available online 22 August 2018
2211-3797/ © 2018 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
W. Xu et al.
However, the common method of granulation for iron ore powder is to
add a certain amount of binder to assemble the power together to form
the grain. The binders can be either inorganic or organic, including
bentonite, various polymeric materials, etc [40]. However, the binder
tends to block the pores of porous hematite and weaken the adsorption
capacity.
In this work, an innovative granulation method was studied to
produce porous hematite granular adsorbents with certain strength and
high specific surface area for arsenic removal. To achieve this purpose,
the batch test including experimental equilibrium adsorption capa-
cities, adsorption isotherm and kinetics studies was conducted in As(V)
solution to compare the adsorption capacity of CHG and the porous
hematite. In order to further understand the As(V) adsorption sites on
porous hematite granular, the SEM-EDX spectra were also investigated.
The research extended the knowledge into providing a new method to
develop the granular adsorbent, reducing the loss of adsorbent capacity.
It had important practical significance and application value for re-
moval of arsenic in water.
Experimental
Materials
The siderite sample used in this work was collected from the
Liupanshui siderite roasting plant located in Guizhou province, China.
It was firstly ground, then purified with high-intensity magnetic se-
paration. The mean particle size (D50) was of 48.63 μm for siderite after
3 min of ball milling. The purities of the samples were of 77.22% FeCO3
for siderite based on chemical analysis. Ordinary Portland cement (P.O
42.5) was used in this work, adhering to Chinese national standard 175-
2007 with a compressive strength of 42.5 MPa at 28 d (SAC, 2007). The
D50 were of 20.95 μm for ordinary Portland cement.
Disodium hydrogen arsenate heptahydrate (Na2HAsO4·7H2O), so-
dium hydroxide (NaOH), hydrochloric acid (HCl) were from Sinopharm
Chemical Reagent Company. All chemicals were of analytical grade. All
the water used in this work was produced from the Millipore Milli-Q
Direct 8/16 water purification system.
Preparation of the granular adsorbents
The preparation scheme of the CHG was presented in Fig. 1. The
siderite concentrate sample was firstly placed in a ceramic crucible, and
Fig. 1. Schematic illustration of preparation of the granular adsorbents.
24
Results in Physics 11 (2018) 23–29
then heated from room temperature to 500 °C at a rate of 5 °C/min in a
muffle furnace (Vulcan3-550PD, UK). Afterwards, the temperature in
the furnace was kept constant for 4 h to prepare the porous hematite
[41,42]. The crucible then was removed from the furnace and cooled to
room temperature.
The disc pelletizer used in this paper was modified with a coater.
After starting the pelletizer inclined to 30°, the porous hematite was
constantly added and water mist was constantly sprayed to obtain a
kind of hematite granules (HG) with certain size. The hematite granules
were taken out to weigh the mass of the hematite. A part of the HG was
placed in an oven at 105 °C as the sample to characterize the water
content of HG. The mass of the porous hematite was calculated by using
the mass of HG minus the mass of water.
Then, the remaining HG was returned to the disc pelletizer. By
adding Portland cement and spraying water mist continuously, a ce-
ment layer was attached to the surface of grains to form the Portland
cement-porous hematite composite granules (CHG). Finally, the CHG
should be cured under dripping water at room temperature at every
12 h for 7 d until the CHG reach a certain strength.
Arsenic adsorption
Batch tests of As(V) adsorption on porous hematite and CHG were
carried out in a conical flask. All the tests were carried out in triplicate,
and the average values were given. In the experiments of the porous
hematite, 0.1 g products were added to 100 mL As(V) solutions with
different concentration in the Erlenmeyer flasks for 24 h to investigate
adsorption isotherm. For the adsorption kinetics, 1 g adsorbents were
added into 1 L As(V) solution with an initial concentration of 5 mg/L. In
the experiments of CHG, the CHG contained about 0.1 g of porous he-
matite was added to 100 mL As(V) solutions with different concentra-
tion in the Erlenmeyer flasks for 72 h to investigate adsorption iso-
therm. For the adsorption kinetics of the CHG, the CHG contained about
1 g of porous hematite was added into 1 L As(V) solution with an initial
concentration of 5 mg/L. All the initial pH of the solution was adjusted
to 7.0 by using HCl or NaOH solutions. The adsorption experiments
continued at 25 °C with an agitation rate of 150 rpm.
After the adsorption, the mixture was filtered through a 0.22-μm
membrane filter. The As(V) concentration of filtrate was measured by
molybdenum blue colorimetric method [43,44] at 880 nm (Orion
Aquamate, Thermo Scientific, USA). To achieve a well understanding of
the effect of the innovative granulation method on the adsorption ca-
pacity of the powder adsorbent, a different method was used to cal-
culate the adsorption capacity of CHG. The mass of the porous hematite
contained in CHG took the place of the total mass of CHG to simplify
operations by neglecting the weeny adsorption of the surface of CHG to
calculate:
Vo (Co−Ce )
qCHG =
m
where qCHG was the adsorption capacity on CHG, Vo was the initial
volume of As(V) solution, Co and Ce was the initial and equilibrium
arsenic concentrations of the solution, respectively, m is the porous
hematite weight contained in CHG used in the adsorption test.
Measurement
The particle size distribution of the materials was characterized
with water as the dispersed phase on a Mastersizer Particle Size
Analyzer (Malvern APA 2000). The Brunauer-Emmett-Teller (BET)
specific surface area and pore diameter were determined by using gas
adsorption analyzer. The X-ray diffraction (XRD) patterns of the ma-
terials were obtained on a D8 Advance X-ray diffractometer (Bruker-
AXS) with Cu Kα radiation. The mercury intrusion porosimetry (MIP)
was used to obtain the pore size and specific surface area of CHG on a
mercury pressure meter (AutoPore IV9500). The scanning electron
W. Xu et al. Results in Physics 11 (2018) 23–29

Fig. 2. The typical morphology appearance of CHG. (a) The cross-section of

CHG; (b) The appearance of CHG.

microscope (SEM, Zeiss Merlin Compact) was used to analyze the

morphology of the particles, while the arsenic distribution after ad-
sorption on the materials was recorded with energy dispersive X-ray
detector (EDX, Oxford X-MAX).

Results and discussion

Characterization of CHG

The typical morphology appearance of CHG was shown in Fig. 2. As

can be seen from Fig. 2(a), there was obvious boundary to divide CHG
into the interior of CHG and the external of CHG. The interior of CHG
was composed by porous hematite. The interior of CHG performed
powder after drying, because porous hematite was only temporarily
granulated due to the capillary force of water and mechanical force in
the granulating process. Meanwhile, the external of CHG represented a
stable layer to enwrap the interior of CHG, which indicated Portland
cement reacted with water in hydration and hardening process. Then,
the CHG had a certain strength and stability to keep granular in room
temperature (Fig. 2(b)).
Fig. 3(a) showed the XRD patterns of the siderite concentrate and
the interior of CHG, in which S and H labeled on the characteristic
peaks represented siderite and hematite respectively. At 500 °C, it was Fig. 3. X-ray diffraction patterns of the siderite and the interior of CHG (a) and
obvious that there was no siderite peak but hematite peaks, indicating the Portland cement and the external of CHG (b). Indexes: H-Hematite; S-
that the siderite had completely transformed into hematite at the cal- Siderite; P-Portlandite; Hy-Calicium silicate hydrate; T-Tricalcium silicate; C-
Calcite; D-Dicalcium silicate.
cining temperature. The siderite decomposed into porous hematite for
the reaction that the ferrous carbonate reacted with oxygen at 500 °C
and decomposed to produce iron oxide and carbon dioxide gas [45,46]. diffraction peaks of C-S-H was identified. From the above analysis, it
The reaction is: concluded that a considerable degree of cement hydration reaction took
500oC
place during the preparation process of CHG.
FeCO3 + O2 → Fe2 O3 + CO2 Fig. 4(a) showed the SEM image of the interior of CHG, indicating
that the porous hematite was featured by micron-scale granular struc-
The decomposition removed CO2 and CO from siderite crystal
tures. Due to the fact that the particle size didn’t change during calci-
structure, forming hematite with uniform pores and large surface area,
nation, the granular structures could be considered to be porous he-
which was customarily referred to as the porous hematite.
matite crystals. And, it could be seen that the surface of the particle was
The XRD patterns of the Portland cement and the external of CHG
uneven with a large amount of voids. This observation was attributed to
was demonstrated in Fig. 3(b). Compared with the XRD curve of Port-
the elimination of carbon oxide in the siderite crystals, leaving a well-
land cement powder, the XRD curve of the external of CHG showed that
developed pore construction.
the intensity of the diffraction peak of P (portlandite) increased ob-
For the external of the CHG presented in Fig. 4(b), various hydration
viously, indicating great amount of portlandite was produced after
products in the shape of coral reefs had rich developed pores. It con-
granulation. Moreover, the intensity of diffraction peak of T (tricalcium
sidered that the capillary pressure and mechanical force weakened the
silicate: the most principal constituent of Portland cement) decreased
adhesion between cement powder during the pelleting process, which
distinctly, implying that a considerable tricalcium silicate was involved
made the cement particles not close tightly. Because of the fact, the C-S-
in reaction as reactant during granulation. Cement was highly complex
H gel formed by hydration was loose and tended to present a porous
material whose constituents reacted with water to form various hy-
structure after hardening. This was critical for the cement layer of CHG
dration products such as C-S-H (calcium silicate hydrate), portlandite
to have good permeability.
[47]. The main reaction is:
The mercury intrusion-extrusion curve of CHG shown in Fig. 5.
3CaO∙SiO2 + nH2 O → xCaO∙SiO2 ∙ (n−3 + x ) H2 O + (3−x ) Ca (OH )2 Mercury began to intrude into the sample in the low pressure, in-
dicating that there was an amount of pores with prodigious aperture. As
As the C-S-H generated was amorphous, there was no new

25
W. Xu et al.
Fig. 4. Scanning electron microscopy image of the CHG: (a) the interior of CHG;
(b) the external of CHG.
Fig. 5. The mercury intrusion-extrusion curve of the MIP of the CHG.
the test was governed by the Washburn-Laplace equation in which the
size of intruded pore accesses, assimilated to cylindrical capillaries,
were inversely proportional to the applied pressure:
4γcosθ
P=
d
where P was the mercury injection pressure (Pa), γ was the surface
tension of mercury (N/m), θ was the contact angle between solid and
mercury (o), and d was the pore access diameter (m) [48]. Moreover,
the cumulative intrusion volume of mercury increased rapidly to ap-
proximate the maximum under low pressure, inferring that pore dia-
meter of pores were very high. Meanwhile, the mercury extrusion curve
obviously lagged and the end point didn’t return to zero point, showing
26
Results in Physics 11 (2018) 23–29
Table 1
The specific surface area, pore volume and pore dimension of the CHG mea-
sured by MIP.
Sample Total Total Median Median Average Porosity (%)
Intrusion Pore Pore Pore Pore
Volume Area Diameter Diameter Diameter
(mL/g) (m2/ (Volume) (Area) (4 V/A)
g) (nm) (nm) (nm)
CHG 0.36 22.86 5108.1 6.1 62.7 45.48
that there were a large number of bottleneck holes in CHG. The ex-
istence of the bottleneck hole indicated that the actual pore size dis-
tribution would be larger than the measured pore size distribution.
It was inferred from the data of Table 1 that the pores of the samples
were well developed with the porosity up to 45.48%. This was sup-
ported by the SEM image of the surface of the CHG given in Fig. 4. The
total pore volume was 0.36 mL/g and the median pore diameter cal-
culated by volume datum was up to 5108.1 nm, which was consistent
with the observation from the mercury intrusion-extrusion curve in
Fig. 5 with the low pressure. Studies demonstrated that the median pore
diameter calculated by volume was close to the median pore diameter
calculated by area for homogeneous matter. Taking into account that
CHG was made up of internal porous hematite and external cement
hydration layer, it was easy to explain the great difference between the
median pore diameter calculated by volume and the median pore dia-
meter calculated by area in Table 1, being 5108.1 nm and 6.1 nm re-
spectively. On the basis of these results, it concluded that CHG was a
macroporous material with good permeability, having the average pore
diameter in Table 1 with the value of 62.7 nm.
The schematic illustration of solid-liquid separation for the CHG was
exhibited in Fig. 6. Although many kinds of powder materials were
proven to be effective adsorbents, they couldn’t be used directly in
large-scale applications due to the difficulty of solid-liquid separation.
CHG had good stability and maintained complete morphology after the
adsorption of 72 h in the solution. And the mixed solution was basically
clarified without powder dispersion and would be convenient in solid-
liquid separation. Unlike the CHG, the porous hematite powder was
sufficiently dispersed in solution before and after adsorption and diffi-
cult for solid-liquid separation.
Arsenic adsorption
Fig. 7 illustrated the adsorption kinetics of As(V) on the porous
hematite powder and the CHG. The adsorption capacity reached 85% in
about 10 h with the porous hematite as adsorbent, whereas it reached
80% in nearly 30 h with the CHG. These results revealed that As(V)
adsorption was slower on the CHG. This was in anticipation and con-
formity with the theory that the adsorption rate of granular adsorbent
was slower than that of powder adsorbent. Compared with the powder,
the granular adsorbents had less contact with the solution, which must
lead to more times to reach adsorption equilibrium. Nevertheless, the
adsorption equilibrium time of CHG was only double times that of the
Fig. 6. The morphologies diagram of the CHG and the porous hematite powders
in the As (V) initial solution and after the adsorption for 72 h.
W. Xu et al. Results in Physics 11 (2018) 23–29

constant of the first-order kinetic model (h−1), k2 was the rate constant
of the second-order kinetic model (g·h−1·g−1). As it was expected, the
rate constants of As(V) adsorption on the CHG were slower than on the
porous hematite for the two models.
The adsorption isotherm of As(V) on the porous hematite and the
CHG were illustrated in Fig. 8. It was evident that the adsorption ca-
pacity increased with increasing As(V) equilibrium concentration for
CHG and porous hematite. Moreover, the adsorption capacity didn’t
reach the maximum at a considerable concentration.
The data was further simulated with the Langmuir and Freundlich
models. The results displayed that the adsorption fitted the Langmuir
isotherm, shown in Table 3. Theoretically, the value of the constant K
was related to the adsorption energy of the adsorbate on adsorbent
surfaces. The larger the K value, the stronger the adsorption [41].
Therefore, the results shown in Table 3 suggested that adsorption of As
(V) species on the CHG was approximate as strongly as porous hematite
powder. At the same time, the qm of CHG was close to that of porous
hematite, being 9.84 mg/g and 11.81 mg/g, respectively. The result
indicated that CHG retained the most of adsorption capacity of internal
Fig. 7. Adsorption kinetics of As(V) on minerals: the porous hematite and the porous hematite, which showed the innovative granulation method to
CHG. produce CHG was rational.

Table 2 Distribution of arsenic on CHG

The parameter of adsorption kinetics models for As(V) adsorption on the porous
and the CHG. To figure out the adsorption sites of the As(V) on CHG, SEM-EDX
Sample qm(mg/g) k1(h−1) R12 k2(g h−1g−1) R22 spectra was adopted to present the difference of elemental distribution
outside the external of CHG (cement hydration layer) and the interior of
Porous hematite 4.75 0.35 0.82 0.108 0.92 CHG (porous hematite), respectively.
CHG 2.23 0.05 0.99 0.015 0.99
Fig. 9 showed the SEM images and EDX spectra of the external of
CHG and the interior of CHG respectively after As(V) adsorption at
initial arsenic concentration of 50 mg/L. Here, EDX spectrum was used
to identify if there was any arsenic on the surfaces of the two compo-
nents of CHG. As it was shown, there were several peaks attributed to
arsenic in the EDX spectrum for the interior of CHG, indicating that
there was much arsenic adsorbed on the interior of CHG. However,
there was no peak corresponding to arsenic in the case of the external of
CHG, indicating that the concentration of arsenic might be lower than
the limitation of the EDX or negligible arsenic was adsorbed on the
external of CHG, which assumed that cement was only served as a
matrix coating outside the iron-oxide [49]. These results suggested that
the As(V) adsorption capacity of the CHG came from the interior porous
hematite. According to the results above in the test analysis, it could
assume that the cement hydration layer with developed pore con-
struction had no adsorption on arsenic, which only acted as a frame-
work to immobilize porous hematite powder.
Compared with the SEM-EDX spectra, SEM-EDX elemental mapping
could be more intuitive to perform the distribution of several elements,
especially for the elements required special attention. Fig. 10 showed
the morphological image of the interior of CHG, EDX elemental map-
Fig. 8. Adsorption isotherm of As(V) on minerals: the porous hematite and the
ping of As and Fe on the surfaces respectively after As(V) adsorption at
CHG.
initial arsenic concentration of 50 mg/L. It was distinct that a good deal
of As elements distributed in the internal of CHG, indicating a good
Table 3 adsorption of As(V) in the internal of CHG. Meantime, it exhibited that
The parameter of Langmuir isotherm for As(V) adsorption on the porous and the distribution of arsenic and iron had considerable overlap, which
the CHG. could speculate the aqueous arsenic oxyanions such as H2AsO4- and
Sample qm(mg/g) K(L/g) R2 HAsO42- undergo a ligand exchange reaction with iron species and form
an inner-sphere surface complex [42,50,51].
Porous hematite 11.81 0.18 0.94
CHG 9.84 0.12 0.95
Conclusion

porous hematite powder, also showing the developed pore structure
and good permeability of CHG from the side.
The data shown in Table 2 were further simulated with the Pseudo-
first-order kinetics and Pseudo-second-order kinetics models, where qm
was the mass of As(V) adsorbed at equilibrium (mg/g), k1 was the rate
CHG exhibited excellent adsorption capacity of As(V) (9.84 mg/g),
which was main attributed to the good affinity of porous hematite to As
(V). Meantime, the cement hydration layer on the external of CHG
performed negligible adsorption, which only acted as a framework to
immobilize porous hematite. Simultaneously, the high mechanical
strength stability in solutions and millimeter size brought the easy

27
W. Xu et al.
Fig. 9. SEM images and EDX spectrum of the different components of the CHG with As(V) adsorption. (a) the interior of CHG; (b) the external of CHG.
solid-liquid separation after adsorption, which gave a prospect for the
practical application of adsorbents in the As(V) sewage.
Acknowledgements
The financial supports for this work from the National Natural
Science Foundation of China (51704220, 51674183 and 51704212),
Natural Science Foundation of Hubei Province (2017CFB280), and
China Postdoctoral Science Foundation (2016M600621) are gratefully
acknowledged.
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in the
online version, at https://doi.org/10.1016/j.rinp.2018.08.031.
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