Environmental Nanotechnology, Monitoring & Management 9 (2018) 37–41

Contents lists available at ScienceDirect

Environmental Nanotechnology, Monitoring

& Management
journal homepage: www.elsevier.com/locate/enmm

Removal of As(V) from aqueous solution by adsorption onto nanocrystalline T

kaolinite: Equilibrium and thermodynamic aspects of adsorption
⁎
Mohammad W. Amera, Akl M. Awwadb,
a
Department of Chemistry, College of Science, The University of Jordan, Amman, Jordan
b
Department of Materials Science, Royal Scientific Society, Amman, Jordan

A R T I C L E I N F O A B S T R A C T

Keywords: In this paper, a one pot and easy method at room temperature, a modification macro-particles of Jordanian raw
Nano-structured kaolinite kaolin clay by hydrochloric acid and hydrogen peroxide to obtain Nano-crystalline kaolinite as an adsorbent for
Adsorption the removal of As(V) from aqueous solutions. Nano-crystalline kaolinite was characterized by XRD, FT-IR, and
Arsenic ions SEM. The adsorption of As(V) onto Nano-crystalline kaolinite has been investigated. The effects of solution pH,
Thermodynamics
adsorbent dose, initial As(V) concentration, contact time, and temperature were examined. Thermodynamic
analysis revealed that the negative values of ΔGo and the positive value of ΔHo, the adsorption process was
spontaneous and endothermic. The Langmuir isotherm model is the best-fit model to predict the experimental
data and adsorption capacity was found 43.67 mg/g.

1. Introduction
Arsenic is a toxic trace element occurring in natural water and
wastewaters mainly in the inorganic trivalent As(III) and pentavalent
As(V) oxidation states. Toxicity of arsenic depends on its oxidation state
and trivalent As(III) has been reported to be more toxic than pentava-
lent As (Moore and Ramamoorthy, 1984). It has been reported that the
long-term uptake of arsenic-contaminated drinking water produced
gastrointestinal, skin, liver, and nerve tissue injuries. (Choong et al.,
2007). The presence of arsenic in water is mostly due to mining ac-
tivities, arsenic additives, pesticides, and herbicides. Various treatment
methods have been reported for the removal of arsenic from aqueous
solutions such as electrocoagulation (Kumar et al., 2004; Flores et al.,
2014; van Genuchten et al., 2012), Electro-removal by capacitive
deionization (Fan et al., 2016), coagulation and biological treatment
(Pramanik et al., 2016; Bhattacharjee et al., 2015), precipitation
(Tiwari and Pandey, 2013), and reverse osmosis (Ning, 2002). The
adsorption technique is generally considered to be a promising method
and has been studied for arsenic removal from aqueous solutions. So
far, various adsorbents for arsenic removal have been developed which
include red mud (Altundogan et al., 2000), iron oxide coated sand,
(Yang et al., 2015) natural siderite and hematite, (Guo et al., 2007)
calcined iowait (Gao et al., 2016), treated zeolitic tuff (Ahmad and
Awwad, 2010), agricultural wastes (Al-Mamun et al., 2013; Shafiqu
et al., 2012), magnetic nanoparticles (Akin et al., 2012), synthetic Fe7S8
nanoparticles (Cantu et al., 2016), supermagnetic nanomaterial Fe3O4-
TiO2 (Beduk, 2016), nanometric titania (Chiavola et al., 2016), Fe3O4@
SiO2 magnetic composite (Montero-Campos and Puente-Urbina, 2016),
Mox/TiO2 immobilized on quartz (Vaiano et al., 2016), and multiwall
carbon nanotubes (Aranda et al., 2016),
In this work, a new adsorbent, nono-crystalline kaolinite (NCK) was
developed for the adsorption and removal of As(V) from aqueous so-
lutions. The NCK was found to work as an excellent adsorbent for As(V)
from aqueous solutions.
2. Materials and experimental method
2.1. Preparation of As(V) stock solution
An As(V) stock solution of 1000 mg/L was prepared by dissolving
4.2 g of sodium arsenate (NaH2AsO4 ·7H2O, Merck, Germany) in
1000 mL of double-distilled water. A working solution for the experi-
ments was freshly prepared from the stock solution. The working so-
lutions with different concentrations of As(V) ions were prepared by
appropriate dilutions of the stock solution immediately prior to their
use. Standard acid of 0.1 M HNO3 and a base solution of 0.1 M NaOH
were used for pH adjustment. All of the reagents were of analytical
grade and used without further purification.
2.2. Preparation of adsorbent
Kaolinite samples were collected from Batn el ghoul deposits,

⁎
Corresponding author.
E-mail addresses: akl.awwad@yahoo.com, akl.awwad@rss.jo (A.M. Awwad).

https://doi.org/10.1016/j.enmm.2017.12.001
Received 23 December 2016; Received in revised form 19 November 2017; Accepted 1 December 2017
2215-1532/ © 2017 Elsevier B.V. All rights reserved.
M.W. Amer, A.M. Awwad
located about 280 Km south of Amman, Jordan. Kaolinite rocks was
rolled crushed by a jaw crusher to obtain grains of kaolinite with di-
mensions between 0.08 and 2.5 mm and then sieved to obtain
0.5–2 mm sized fraction. The 0.5–2 mm sized fraction of kaolinite was
washed with distilled water to remove soluble elements and dried at
378 K. Dried kaolinite was treated with concentrated hydrochloric acid
(0.37mass fraction purity) with agitation from time to time and left
overnight. An aqueous colored acid solution which formed was sepa-
rated from grains of kaolinite by decantation and filtration. Afterwards
kaolinite was treated with 50% hydrogen peroxide (H2O2) with agita-
tion from time to time and left overnight and then washed with distilled
water and dried at a temperature of 378 K. The nanocrystalline kaoli-
nite (NCK) samples prepared from raw kaolinite were examined by X-
ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron mi-
croscopy (SEM) and Fourier transform infrared spectroscopy (FTIR).
2.3. Adsorption isotherms
Adsorption equilibrium was obtained by shaking 1 g of dry ad-
sorbent (NSK) in a series of 100 mL flasks containing 20 mL of initial
concentration of As(V) ions ranging from 5 to 100 mg/L for 120 min.
The initial pH value of As(V) ion solutions was adjusted from 1 to 8.0
with either 0.01 M HNO3 or 0.01 M NaOH at four temperatures,
(283.15, 293.15, 303.15, and 313.15) K. Flasks were agitated on a
shaker at a 350 rpm constant shaking rate for 120 min to ensure equi-
librium was reached and filtered through filter paper (Schleicher and
SchÜ ll 589), and the supernatant was analyzed for arsenic by a se-
quential plasma emission spectrometer (ICPS-7510, Shimadizu). Each
experiment was run in triplicate, and mean values are reported. The As
(V) percent removal (%) was calculated using the following equation:
Co − Ce
Removal % = × 100
Co (1)
where Co and Ce are the initial and equilibrium concentrations of the As
(V) ions(mg/L).
The amount of As(V) ions adsorbed at equilibrium qe, which re-
presents As(V) uptake was calculated from the following equation:
Co − Ce
qe = xV
M (2)
where qe is the As(V) adsorbed (mg/g), Co and Ce are the same as above,
V is the volume of the solution (L), and M is the weight of adsorbent (g).
3. Results and discussion
3.1. Characterization of nano-crystalline kaolinite adsorbent
XRF analysis showed that the NCK is rich in SiO2 and Al2O3 with a
percent oxide composition of 63.38 and 24.63, respectively. Moderate
to high SiO2/Al2O3 ratio of 2.57 gives rise to good selectivity.
Mineralogical characterization studies NCK showed that the main
constituents are kaolinite, and traces of anatase and iron oxides. Fig. 1a
showed XRD of NCK and the average size diameter determined by
Debye-Scherr equation equals 20 nm. SEM analysis of prepared na-
noscale kaolinite is shown in Fig. 1b. The SEM image showed the na-
noscale kaolinite particles are in spherical shape and with average size
diameter 5–40 nm. Fig. 1c showed the spectra of raw kaolinite and
nanocrystalline kaolinite.
3.2. Effect of the initial pH
The effect of pH of the As(V) solution on the adsorption capacity of
As(V) onto the NCK is shown in Fig. 2. It can be seen from Fig. 2 that the
removal As(V) percent increases sharply with increasing pH of As(V)
from 1.0 to 8.0 and then decreases to reach pH 9.0. However, a decline
in removal As(V) percent occurred when the pH was lower than 8.0.
38
Environmental Nanotechnology, Monitoring & Management 9 (2018) 37–41
The maximum adsorption was observed around pH 8.0 at all tem-
peratures. However, a decrease in the removal As(V) percent from
aqueous solution at low pH = 7 to 1. The maximum adsorption was
observed around pH 8.0 at all temperatures.
3.3. Effect of adsorbent dose
The effect of adsorbent dose of NCK on the As(V) removal percent is
shown in Fig. 3, which shows that the removal percent of As(V) in-
creased very rapidly with an increase in dosage of NCK from (0.1–0.9)
g/L and a marginal increase was observed on further increase in the
adsorbent dose. At an adsorbent dose of 0.5 g/L NCK, maximum re-
moval efficiencies of 98.45% were observed at 303.15 K. The increase
in efficiency of As(V) removal may be attributed to the fact that, with
an increase in the adsorbent dose, more adsorbent surface or more
adsorption sites were available for the metal ions to be adsorbed.
3.4. Effect of contact time and temperature
The effect of contact time and temperature on the adsorption of As
(V) onto NSK is shown in Fig. 4. It can be seen from Fig. 4 that the
removal percent of As(V) increases with contact time until equilibrium
is attained between the amount of As(V) on NSK and the remaining As
in solution. Fig. 4 shows that the removal percent of As(V) increases
with contact time from (0–60) min and then becomes almost constant
up to the end of the experiment. It can be concluded that the binding of
As(V) with NSK is high at initial stages and becomes almost constant
after an optimum contact time of 100 min. As temperature increases
from (283–313) K, As(V) removal percent increase from (70.0–98.4)%
for an initial concentration of 40 mg/L at pH 8.0. Similar trends were
observed for other concentrations. This indicated that the adsorption
process is endothermic in nature. The As(V) removal percent versus
time curves are smooth and continuous leading to saturation, sug-
gesting possible monolayer coverage of As(V) ions on the surface of the
NCK.
3.5. Adsorption isotherms
An adsorption isotherm describes the fraction of sorbate molecules
that are partitioned between liquid and solid phases at equilibrium.
Adsorption of As(V), ions onto NSK was modeled using two adsorption
isotherms: Langmuir, and Freundlich isotherms.
3.5.1. Langmuir isotherm
The Langmuir isotherm assumes monolayer adsorption on a uniform
surface with a finite number of adsorption sites. Once a site is filled, no
further sorption can take place at that site. As such the surface will
eventually reach a saturation point where the maximum adsorption of
the surface will be achieved. The linear form of the Langmuir isotherm
model is described as (Langmuir, 1918):
Ce 1 1
= + Ce
qe KL qmax qmax (3)
where KL is the Langmuir constant related to the energy of adsorption
and qmax is the maximum adsorption capacity (mg/g). Values of
Langmuir parameters, qmax and KL were calculated from the slope and
intercept of the linear plot of Ce/qe versus Ce as shown in Fig. 5. Values
of qmax, KL and regression coefficient R2 are 43.67 mg/g, 0.0134 L/mg,
and 0.9998, respectively. These values for NCK adsorbent indicated that
Langmuir model describes the adsorption phenomena as favorable. The
essential characteristics of the Langmuir isotherm parameters can be
used to predict the affinity between the sorbate and sorbent using se-
paration factor or dimensionless equilibrium parameter, RL, expressed
as in the following Equation:
M.W. Amer, A.M. Awwad Environmental Nanotechnology, Monitoring & Management 9 (2018) 37–41

Fig. 1. (a) XRD pattern, (b) FT-IR, and (c) SEM of prepared nanocrystalline kaolinite.

Fig. 3. Effect of adsorbent dose on the percent removal of As(V) by NCK

(T = 303 K; Co = 30 mg/L; pH = 8.0).
Fig. 2. Effect of pH solution on the percent removal As(V) by NCK.
T = 303 K; Co = 30 mg/L; pH = 8.0.
provides important information about the nature of adsorption. The
value of RL indicated the type of Langmuir isotherm to be irreversible
1 (RL = 0), favorable (0 < RL ˂ 1), linear (RL = 1) or unfavorable
RL =
1 + KL Co (4) (RL ˂ 1). The RL for As(V) ions adsorption by NCK was found to be
0.43–0.88 for concentration of 10–100 mg/L of metal ions. They are in
where KL is the Langmuir constant and Co is the maximum initial
the range of 0–1 which indicates the favorable adsorption. Langmuir
concentration of As(V) ions. The value of separation parameter RL

39
M.W. Amer, A.M. Awwad Environmental Nanotechnology, Monitoring & Management 9 (2018) 37–41

Fig. 7. log Ka vs 1/T for the adsorption of As(V) by NCK.

Fig. 4. Effect of contact time and temperature on percent removal of As(V) by NCK.
Table 1
Thermodynamic Parameters of NCK for As(V) Adsorption.

T(K) Ka ΔGo (kJ/Mol) ΔHo (kJ/Mol) ΔSo (J/K Mol)

293 4.45 −3.64 22.94 90.72

303 6.11 −4.56
313 8.12 −5.45

Table 2
Comparision of various adsorbents for the removal of As(V).

Adsorbent qmax (mg/g) References

Fe7S8 nanoparticles 31.30 Cantu et al. (2016)

Treated zeolitic tuff 18.35 Ahmad and Awwad (2010)
Red mud 0.51 Altundogan et al. (2000)
Natural siderite and hematite 0.16 Guo et al. (2007)
Fig. 5. Langmuir isotherm for As(V) ions onto NCK. Alumina 25.00 Wasay et al. (1996)
Magnetite 46.70 Yean et al. (2005)
Maghemite nanoparticles 50.00 Tuutijärvi et al. (2009)
Nanoscale zero valent iron 29.04 Wang et al. (2014)
Nanoscale zero valent iron 14.00 Mosaferi et al. (2014)
Nano-crystalline kaolinie 43.67 This work

1
l nqe = l nkF + lnCe
n (5)

where KF is the Freundlich constant related to the bonding energy. 1/n

Fig. 6. Freundlich isotherm for As(V) ions onto NSK.
qmax and KL values increased with temperature, showing that the ad-
sorption capacity and intensity of adsorption are enhanced at higher
temperatures
3.5.2. Freundlich isotherm
Freundlich isotherm model is the well-known earliest relationship
describing the adsorption process. This model applies to adsorption on
heterogeneous surfaces with the interaction between adsorbed mole-
cules and the application of the Freundlich equation also suggests that
sorption energy exponentially decreases on completion of the sorption
centers of an adsorbent. This isotherm is an empirical equation and can
be employed to describe heterogeneous systems and is expressed as
follows in linear form (Freundlich and Hellen, 1939):
is the heterogeneity factor and n (g/L) is a measure of the deviation
from linearity of adsorption. Freundlich equilibrium constants were
determined from the plot of lnqe versus lnCe, Fig. 6. The n value in-
dicates the degree of non-linearity between solution concentration and
adsorption as follows: if n = 1, then adsorption is linear; if n < 1, then
adsorption is a chemical process; if n > 1, then adsorption is a physical
process. The n value in Freundlich equation was found to be 1.58 for As
(V) ions, Since n lie between 1 and 10, this indicates the physical ad-
sorption of As (V) ions onto NCK. The value of regression coefficients
R2 = 0.8903, which is regarded as a measure of goodness of fit of the
experimental data to the isotherm models. The Langmuir model is more
suitable than the Freundlich model for the representation of the ad-
sorption data because it has higher R2 values.
3.6. Thermodynamics
The thermodynamic behavior of the adsorption of As(V) ions onto
NCK is evaluated as follows. The changes in Gibbs energy, ΔGo, of the
adsorption process is related to the equilibrium constant by the fol-
lowing equation:
ΔGo = −RT ln Ka (6)
where Ka is the equilibrium constant calculated from the following

40
M.W. Amer, A.M. Awwad
equation
C
Ka = a
Ce (7)
where Ca and Ce are the equilibrium concentration of As(V) (mg/L) on
NSK adsorbent and in solution, respectively.
The enthalpy change, ΔHo, and entropy change, ΔSo, were obtained
from the van’t Hoff equation:
ΔS o ΔH o
log K a = − by adsorption on red mud. Waste Manage. 20, 761.
2.303R 2.303RT (8)
where T is the absolute temperature (K); R is the gas constant (8.314 J/
mol/ K). ΔHo (kJ/mol) and ΔSo (J/ mol/K) were calculated from the
slope and intercept of a linear plot of log Ka versus 1/T. The plot shown
in Fig. 7 is linear over the entire range of temperatures investigated.
The thermodynamic parameters were evaluated at three operating
temperatures, (293, 303, and 313) K, at an initial As(V) concentration
of 40 mg/L. The values of Ka, ΔHo, ΔSo, and ΔGo at the investigated
temperatures are listed in Table 1. The obtained negative values of ΔGo
at all temperatures studied revealed the fact that the adsorption process
was spontaneous. Positive values of ΔHo indicate the endothermic
nature of the adsorption process. The positive value of ΔSo suggests
increased randomness of the solid-solution interface during the ad-
sorption of As(V) ions onto NCK adsorbent.
3.7. Comparison of NCK powder with other adsorbents
A comparative of the maximum adsorbent capacity, qmax of NCK
with those of some other adsorbents reported in literature is given in
Table 2. Differences in qmax are due to the nature and properties of each
adsorbent such as surface area, particle sizes and the main functional
groups in the structure of the adsorbent. A comparison with other ad-
sorbents indicated a high As(V) ion adsorption capacity of Nano-crys-
talline kaolinite.
4. Conclusion
The results obtained in this research work demonstrated the effi-
ciency of Nano-crystalline kaolinite (NCK) as an effective and eco-
friendly adsorbent for removal As(V) from aqueous solutions. The
thermodynamic parameters ΔHo, ΔGo, and ΔSo values of As(V) ions
adsorption onto NCK show the endothermic heat of adsorption, favored
at high temperatures. The positive value of ΔSo revealed an increase in
randomness of the solid-solution interface during the adsorption of As
(V) ions. Regression coefficients R2 were found to be more than 0.9998,
0.8903 revealing the best fit for the adsorption data by the Langmuir
isotherm model over the Freundlich isotherm model. Compared to
various adsorbents reported in the literature, the Nano-crystalline
kaolinite showed good promise for its use in wastewater treatment.
Funding
Authors thank Industrial Research and Development Fund (iR&Df),
Jordan for financial support No. 1/18/340.
Novelty statement
A new natural adsorbent in Nano-structured used for the first time
in removal toxic arsenic ions from aqueous solutions.
Acknowledgments
Authors are thankful to the Royal Scientific Society and the
University of Jordan for giving all facilities to carry out this research
work. Also authors thank University of Science and Technology, Irbid,
Jordan for SEM and XRD analysis.
41
Environmental Nanotechnology, Monitoring & Management 9 (2018) 37–41
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