Journal of Molecular Liquids 219 (2016) 299–305

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Journal of Molecular Liquids

journal homepage: www.elsevier.com/locate/molliq

Removal of methyl orange by copper sulfide nanoparticles loaded

activated carbon: Kinetic and isotherm investigation
P. Mokhtari a, M. Ghaedi a,⁎, K. Dashtian a, M.R. Rahimi b, M.K. Purkait c
a
Department of Chemistry, Yasouj University, Yasouj 75918-74831, Iran
b
Process intensification Laboratory, Chemical Engineering Department, Yasouj University, Yasouj 759418-74831, Iran
c
Department of Chemical Engineering, Indian Institute of Technology Guwahati, Guwahati 781039, Assam, India

a r t i c l e i n f o a b s t r a c t

Article history: This work describes the synthesis of new nanoparticle based adsorbent for the removal of methyl orange (MO)
Received 12 October 2015 from colored waste water. Copper sulfide nanoparticles were synthesized and impregnated on the commercial
Received in revised form 19 November 2015 activated carbon (CuS-NP-AC) and successfully characterized using UV–Vis spectrophotometer, FESEM, XRD
Accepted 6 March 2016
and BET. BET surface area of prepared adsorbent was measured as 1286 m2/g. Effects of various parameters
Available online xxxx
such as pH, initial MO concentration (mg/L), mass of prepared adsorbent dosage (g L−1) and contact time
Keywords:
(min) were studied. The optimization conditions were set as: 4.0 min, 14 mg/L and 25 mg/L for contact time,
Adsorption mass of prepared adsorbent dosage and initial MO concentration, respectively, at pH 5.0. The adsorption
Activated carbon equilibrium data were analyzed using different models and Langmuir model represented the equilibrium data
Copper sulfide nanoparticles well with adsorption capacity of 122 mg/g. Kinetic data revealed that the adsorption of MO dye on the adsorbent
Methyl orange surface followed pseudo-second order model.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction the best candidate for wastewater treatment. On the other hand, extent
of adsorption significantly depends on the presence of active sites on
The extensive application of dyes compound in various industries the surface of adsorbents. Recently M. Ghaedi et al. wildly usemetallic
such as textile, paint, leather, paper and plastics discharges toxic colored nanostructures loaded on activated carbon as adsorbents for the remov-
effluent and contaminates surface and ground water. Dyes are resistant al of pollutants in aqueous environment [6,8,10,15–20]. Carbon-based
to heat, chemical reagent and have ability to generate cancer and muta- materials and their modification by novel nanoscale materials lead to
gens. Presence of dyes in water creates serious impact for different benefits such as high surface area, porous structure, large adsorption ca-
aquatic organism [1–4]. Therefore, their removal from wastewater pacities, fast adsorption kinetics and simultaneously providing easy, low
before the wastewater entered into human bodies is great demand. cost and efficient method for the removal of pollutants from the waste-
Among these pollutants, methyl orange (MO) dye belongs to anionic water [21–23].
category and toxic dye and it has been widely applied in the above in- In this work, CuS nanoparticles were synthesized by green method
dustries. MO leads to health hazards such as difficulties in breathing, and loaded on the surface of commercial activated carbon (CuS-NP-
vomiting, diarrhea and nausea. It is a weak acid–base indicator with po- AC). The prepared CuS-NP-AC was characterized by UV–Vis spectropho-
tential applicability as toxic and carcinogenic agent. Therefore, its re- tometer, field emission scanning electron microscopy (FESEM), X-ray
moval and elimination from various aqueous waste is required. diffraction (XRD) and BET analysis. The dye removal performance of
Generally, coagulation, precipitation, adsorption, electrochemical tech- prepared adsorbent was investigated at various operating conditions.
niques, ozonation and biosorption are suitable candidates for such pur- Kinetics and equilibrium study during adsorption was also performed.
pose [5–11]. These techniques have some limitations that include A calculation procedure is proposed to know the amount of adsorbent
requirement of large amount of supporting material and generation of requirement for known amount of water to be treated.
large amount of secondary waste. Adsorption is one of the most studied
dye removal technique that leads to producing high-quality purified 2. Experimental
water. The adsorption based procedure was widely used due to its
high efficiency, capacity and ability for large scale dye removal applica- 2.1. Materials and instruments
tion [12–15]. The nontoxic, low cost and easily available adsorbents are
MO dye was used for the preparation of colored waste water. pH of the
⁎ Corresponding author. solution was adjusted by HCl and NaOH solution. All the chemicals includ-
E-mail address: m_ghaedi@yahoo.com (M. Ghaedi). ing NaOH, HCl, KCl and Copper (II) acetate (analytical reagent grade)

http://dx.doi.org/10.1016/j.molliq.2016.03.022
0167-7322/© 2016 Elsevier B.V. All rights reserved.
300 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305

were supplied by Merck Company (Darmstadt, Germany). A pH/ion carried out for all the operating variables studied and only the average
meter (Metrohm, Switzerland, Swiss, model 692) was used for the mea- values were taken in to consideration. The average deviation of
surement of pH. MO concentration was determined using an UV–Vis duplicate results in the units of concentration is found to vary within
spectrophotometer (Jasco, model V-530, Japanese) at a wavelength of ± 2.0%. Blank experiments were carried out with dye solution and
465 nm. The morphology of the CuS-NP-AC was observed by field emis- without adsorbent to ensure that no dye was adsorbed onto the walls
sion scanning electron microscopy (FESEM; Hitachi S-4160, China) of the beakers. The amount of dye adsorbed per unit weight of adsor-
under an acceleration voltage of 15 and 20 kV. X-ray diffraction (XRD) bent at time t, qt (mg/g) and percentage dye removal efficiency (R %)
pattern was recorded by X-ray diffractometer (Philips X'Pert, 40 kV and was calculated as follows:
30 mA, American) for 2θ values over 10–80°. A BET surface analyzer
(Quanta chrome NOVA 2000e, Company Quantachrome Instruments, ðC0 −Ct ÞV
qt ¼ ð1Þ
American) was used for examining the nitrogen adsorption–desorption M
isotherm at 77 K. Before each experiment, the samples were degassed
using helium at 553 K for 3 h. According to BET analysis result some useful C0 −Ct
R¼  100 ð2Þ
information about surface properties of adsorbent including surface area, C0
total pore volume and size and porosity was obtained.
where, C0 is the initial dye concentration (mg/L), Ct is the concentration
2.2. Batch experiments methods of dye at any time t, V is the volume of solution (L) and M is the mass of
adsorbent (g) [6,15,18].
Stock solution of MO of concentration 1000 mg/L was prepared by
dissolving an accurately weighed quantity (0.1 g) of solid dye in 2.3. Preparation of copper sulfide nanoparticle
100 mL of deionized water (pH is 6.9). Experimental solutions of desired
concentrations were obtained by successive dilution of the stock CuS nanoparticles were synthesized based on the reaction of the
solution. For studying the effect of solution pH on dye adsorption, mixture of Copper(II) acetate (Cu(CH3COO)2·H2O) with thioacetamide
experiments in different pH (varying from 1 to 8) were conducted for (CH3CSNH2) in aqueous media. In a typical synthesis, 10 mL of a
initial dye concentration of 15 mg/L. To observe the effect of adsorbent 0.1 mol L− 1 (Cu(CH3COO)2·H2O) and 20 mL 0.2 mol L− 1 tri-sodium
dose on dye adsorption, different amounts of adsorbent (varying from citrate as capping and reducing agent were taken in a 100 m L beaker.
2 to 16 mg/L) are used. A common adsorbent dose of 14 mg/L, stirring In the next step, 5.0 mL of 0.4 mol L−1 thioacetamide (TAA) as source
speed of 400 rpm and pH 5.0 was used for all the above experiments. for S2− ions was added to it slowly. Finally, double distilled water was
In order to study the adsorption isotherm, 1.0 mg of adsorbent was added to the solution to make the volume close to 100 mL and the
kept in contact with 100 mL dye solution of different concentrations solution was stirred for 10.0 min for well mixing of the constituents.
at pH 5.0 for 4.0 min with constant shaking at ambient temperature. The resulting mixture was taking place at room temperature and the
After 4 min the solution attains equilibrium and the amount of dye citrate stabilized CuS nanoparticles started to grow slowly. In the next
adsorbed (mg/g) on the surface of the adsorbent was determined by step, 100 mL of the freshly prepared CuS nanoparticles suspension
the difference of the two concentrations. Duplicate experiments were was mixed with 3.0 g of the activated carbon in a 250 mL Erlenmeyer

Fig. 1. Absorption spectra of the CuS nanoparticles taken at 5 min (a), X-ray diffraction (XRD) pattern of the CuS nanoparticles (b), FESEM images of activated carbon (c) and FESEM images
of CuS nanoparticles deposited on activated carbon (d).
 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305 301

Fig. 2. Pore size distribution of CuS-NP-AC.

flask under magnetic stirring for up to 1.0 h, resulting in deposition of Fig. 1b shows the XRD pattern obtained by scanning 2θ in the range
the CuS nanoparticles on the activated carbon. The carbon-supported 30–75°, for the powder of CuS-NP at room temperature. It exhibits
CuS nanoparticles were then filtered and extensively washed with seven major diffraction peaks related to the diffraction angles 32.33°
double distilled water. The carbon-supported CuS nanoparticles were (101), 34.25° (102), 37.13° (103), 38.20° (006), 56.37° (110), 62.23°
generally dried at 80 °C in an oven for 10 h. (108), and 70.20° (116). This pattern confirmed the formation of a
hexagonal covellite phase of CuS, which is in good agreement with the
standard XRD pattern (Joint Committee for Powder Diffraction
3. Results and discussion Standards, JCPDS card No. 24-0060) [24].
The FE-SEM images of the activated carbon surface and the CuS
3.1. Characterization of adsorbent nanoparticles loaded on activated carbon are shown in Fig. 1c and d,
respectively. As shown in Fig. 1c the surface morphology of the activated
Absorption spectra of CuS-NP in range of 5.0–30 min are shown in carbon is homogeneous and relatively smooth. Fig. 1d shows the
Fig. 1a. The CuS-NP suspension shows a well-resolved absorption morphologies of the CuS-NP deposited on the activated carbon which
maximum of the first electronic transition indicating a sufficiently are composed of a large quantity of well-dispersed spherical nanoparti-
narrow size distribution of the CuS-NP, which shifts to shorter cles and relatively uniform in shape and size distribution. The size of
wavelengths with decreasing size of the nanoparticles as a consequence each CuS-NP is in the range of 100–200 nm. The particle size measured
of quantum confinement. As Fig. 1a exhibits, the citrate-capped CuS-NP
have absorption edges in the range of 390–416 nm.

Table 1
Summary report of prepared adsorbent.

Physical properties Values

Surface area (m2/g)

BET surface area: 1286
Langmuir surface area: 1276
BJH desorption cumulative surface area of pores 787
between 17,000 Å and 3,000,000 Å width:

Pore volume (m3/g)

BJH desorption cumulative volume of pores between 545 × 10−6
17,000 Å and 3000,000 Å width:

Pore size (Å)

Adsorption average pore width (4 V/A by BET): 28.4 Å
BJH adsorption average pore width (4 V/A): 31.1 Å
BJH desorption average pore width (4 V/A): 53.1 Å
Fig. 3. Chemical structure of MO molecule in acidic and basic pH.
302 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305

Fig. 4. Effect of pH on the removal of MO by CuS-NP-AC. Adsorbent dosage: 14 mg/L; Fig. 6. Effects of contact time on the amount of MO adsorption. pH: 5; contact time: 4 min;
contact time: 4 min; initial dye concentration: 15 mg/L; temperature: 25 °C. initial dye concentration: 15 mg/L; temperature: 25 °C.

directly from this FE-SEM image agrees with that determined by the pH, both adsorbent and adsorbate became positively charged after
XRD analysis. The pore size distribution and surface area of adsorbent adsorption of additional H+ molecule and hence adsorption reduces.
were studied by BET studies and the results were shown in Fig. 2 and
summarized in Table 1. It can be seen that high surface area and very po- 3.3. Adsorbent mass influence on MO removal
rous structure make possible this novel adsorbent as more reactive sites
for external and internal adsorption of MO. The effect of adsorbent dosage (varying from 2.0 mg/L to 16 mg/L)
on the percentage removal of MO at initial dye concentration of
3.2. Effect of pH 15 mg/L is shown in Fig. 5. It is observed that the MO removal increases
with increase in adsorbent dose up to a certain limit (14 mg/L) and then
The molecular structure of MO (Fig. 3) in acidic and basic medium, the rate of increase is slowed down. Initially, rapid increase in adsorp-
reveals that functional groups with reactive atoms are present in MO tion with the increase in adsorbent dose can be attributed to greater
structure. The ionic charge of both MO and CuS-NP is greatly affected surface area and availability of more adsorption sites. After this critical
by pH of the solution and extent of adsorption thereon. It is expected dosage (14 mg/L) the extent of adsorption is increasingly slowed
that high solubility of copper in acidic media strongly reduced at down due to the fact that although there is increasing number of active
alkaline pH and improved the loading and impregnation onto activated sites but there is shortage of dye in the solution. The increase in MO
carbon. Effects of initial solution pH on the MO adsorption over Cu-NP- removal percentage at higher adsorbent dosage is due to the very fast
AC surface were investigated and the result is shown in Fig. 4. It may be superficial adsorption onto the adsorbent surface that produces a
seen, that the percentage removals of MO increase with pH range of 1.0 lower solute concentration in the solution than when adsorbent dosage
to 5.0. The maximum removal was observed at pH of 5.0 and at higher is lower.
values of 5.0 the removal percentage decreases with increase in pH.
The nature of adsorption of MO as anionic dye on CuS-NP-AC surface 3.4. Effects of contact time
is a combination of various mechanism and binding pathways such as
hydrogen bonding, electrostatic (dye anion and positive AC support or The variation in percentage removal of MO with contact time at
adsorbent surface), soft–soft and dipole–ion interaction. The decrease initial MO concentration of 15 mg/L is presented in Fig. 6. It may be
in dye adsorption beyond pH 5.0 was due to the inter-ionic repulsion observed from the figure that the maximum amount of dye adsorption
of negatively charged dye molecule and adsorbent surface. At acidic taking place within the contact time of 4.0 min attains equilibrium

Fig. 5. Effect of CuS-NP-AC dosage on the percentage removal of MO. pH: 5; contact time: Fig. 7. Effect of initial dye concentration on the removal of MO. Adsorbent dosage:
4 min; initial dye concentration: 15 mg/L; temperature: 25 °C. 14 mg/L; contact time: 4 min; pH: 5; temperature: 25 °C.
 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305 303

Table 2
Various kinetic parameters for the adsorption of MO on to CuS-NP-AC.

Model Equation Plot Parameters Value

First-order kinetic Log(qe− qt) = log(qe) − k1/2.303 t Plot the values of log (qe − qt) versus t to give a linear relationship k1 0.13
from which k1 and qe can be calculated from the slope and intercept, qe (calc) 105
respectively. R2 0.92
k2 0.03
Plot the values of (t/qt) versus t to give a linear relationship from which k1 qe (calc) 119
Second-order kinetic (t/qt ) = 1/(k2q2e ) + 1/qe(t)
and qe can be calculated from the slope and intercept, respectively. R2 0.99
h 104.2
Kdiff 11.4
The values of Kdif and C were calculated from the slope and intercept of the
Intraparticle diffusion qt = Kdif t1/2 + C C 31.3
plot of qt versus t1/2, respectively.
R2 0.90
β 0.1
Plot the values of (qt) versus ln(t) to give a linear relationship from
Elovich qt = 1/β ln(αβ) + 1/β ln(t) α 447.91
which α and β can be determined from the slope and intercept, respectively.
R2 0.90
qe (exp) 122

thereafter. This indicates that the rate of adsorption is very fast. Data has with initial dye concentration was due to the increase in the ratio of
been taken up-to 20 min of operation (not shown in Figure) which is dye molecule to the surface area available for adsorption [10,25].
more than sufficient to attain equilibrium. After 4.5 min no significant
change in the extent of adsorption is observed. For the initial concentra- 3.6. Adsorption kinetic modeling
tion of 15 mg/L, more than 99% adsorption has been observed. From the
above observation, it is evident that initial adsorption is very fast. The kinetics of MO adsorption onto Cu-NP-AC surface was evaluated
using different models such as pseudo-first-order, pseudo-second-order,
Elovich model and intraparticle diffusion models [16,26,27]. The various
3.5. Effect of initial dye concentration parameters were calculated from the plots of the kinetic model equations
and summarized in Table 2. Among these models the criterion for their
The influence of initial MO concentration in the range of 5–40 mg/L applicability is based on judgment on the respective correlation
on its removal percentage was investigated and the result is shown in coefficient (R2) and agreement between experimental and calculated
Fig. 7. It may be found that MO removal percentage was decreased value of qe. The high values of R2 (~1) and good agreement between
with increasing initial dye concentration, while the actual amount of two qe values indicate that the understudy adsorption system follows
adsorbed MO significantly increased. Some decrease in percentage pseudo-second-order kinetic model (Table 2). Another alternative
adsorption (~22%) was found when initial dye concentration increases method for kinetic evaluation of an adsorption process is intra-particle-
from 5.0 mg/L to 40 mg/L. The decrease in the extent of adsorption diffusion model. According to conditions and equation presented in
Table 2, it is seen that respective plot (plot of qt versus t1/2) gives only
one line and the rate constant ki was evaluated from the slope of the
Table 3 line. Since the line did not pass through the origin, it indicates that the
Various isotherm constants and their correlation coefficients calculated for the adsorption intraparticle diffusion was not the rate-controlling step.
of MO onto CuS-NP-AC.

Isotherm Equation Parameters Value of 3.7. Adsorption equilibrium study

parameters

Langmuir qe = qmbCe/(1 + bCe) Qm (mg/g) 120.4 The experimental adsorption equilibrium data provides some
Ka (L/mg) 0.845 insight into the adsorption mechanism, the surface properties and
R2 0.99
affinity of the adsorbent for adsorbate. Among different isotherm
Freundlich ln qe = ln KF + (1/n) ln Ce 1/n 0.42
KF (L/mg) 51.60 models, Langmuir, Freundlich, Temkin, Dubinin–Radushkevich,
R2 0.93 Harkins–Jura, Halsey, Jovanovic, Henderson and Frumkin equations
Temkin qe = B1 ln KT + B1 ln Ce B1 26.586
KT (L/mg) 2.01
R2 0.98
Dubinin–Radushkevich ln qe = ln Qs –Bε2 Qs (mg.g) 98.3
(DR) B 0.002
E (kj/mol) 15.81
R2 0.98
Harkins–Jura 1/q2e = (B/A)-(1/A) logCe A 1666
B 0.833
R2 0.76
Halsey lnqe = ((1/n)lnKH)-(1/n)lnCe KH 3 × 10−6
n −3.142
R2 0.76
Jovanovic qe = qmax(1-e (K·Ce)
) K 3 × 10−6
qm 45.1
R2 0.75
Henderson ln (−In(1-Ce)) = n ln qe + ln k K 0.024
n 0.397
R2 0.94
Frumkin ln(((θ/(1-θ))(1/Ce)) = lnK + K 0.56
2aθ a 0.88
R2 0.98
Fig. 8. A single-stage batch adsorbed.
304 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305

Fig. 9. Adsorbent mass (W) against volume of effluent (V) treated for different percentages of MO removal (C0 = 15 mg/L).

are useful methods are presented in Table 3 [16,27–31]. All the model It was reported in the equilibrium study that the MO removal by
constants are evaluated from the slopes and intercepts of the respective CuS-NP-AC followed Langmuir model. The above-mentioned equation
model equations and summarized in Table 3. Fitting the experimental can be rearranged as follow:
data in these isotherm models and considering the higher values of cor-
relation coefficients (R2 ~ 1) it is concluded that Langmuir isotherm
W=V ¼ ðC0 −C1 Þ=qe ¼ ðC0 −Ce Þð1 þ bC0 Þ=ðq0 bCe Þ ð5Þ
model is the best model to explain the MO adsorption over CuS-NP-AC.

3.8. Design of batch sorption based on the equilibrium data Except for 100 percentage removal conditions, Eq. (5) can be used to
calculate the amount of adsorbent dose required for the essential
It is quite difficult to design properly the adsorber size and perfor- percentage removal of MO from aqueous solution. Fig. 9 showed the
mance until and unless all experimental data and rate controlling amount of CuS-NP-AC required for a desired percentage removal of
steps are available. Therefore, empirical design procedures based on MO for different solution volumes. This study will give an idea to design
sorption equilibrium conditions are the most common method for an adsorption column. Finally, a comparative analysis of MO adsorption
predicting the amount of adsorbent and performance. A diagram of capacity of different adsorbent was done and reported in Table 4. The
batch removal process is illustrated in Fig. 8. In this model, V (L) is the adsorption capacity of CuS-NP loaded on activated carbon considered
volume of wastewater, C0 is the initial MO concentration, W (g) is the in this work is also reported in Table 4 and compared with various
mass of adsorbent and C1 is the final dye concentration after adsorption. adsorbents. From the table, it might be concluded that CuS-NP loaded
The actual adsorbed dye on the adsorbent changes from q0 = 0 on activated carbon is a prospective adsorbent over others for MO
(initially) to q1 after adsorption. The mass balance equation may be removal [24,32–35].
written as
4. Conclusion
VðC0 −C1 Þ ¼ Wðq0 −q1 Þ ð3Þ
İn this work, the copper sulfide nanoparticles loaded on activated
At equilibrium, C1 → Ce and q1 → qe. The following equation may be carbon was synthesized and fully characterized using UV–Vis, FE-SEM,
obtained XRD and BET analysis. BET surface area of prepared adsorbent was
measured as 1286 m2/g. Subsequently, this adsorbent was used for
VC0 þ Wq0 ¼ VCe þ Wqe ð4Þ the removal of MO from aqueous medium. It was observed that batch
sorption of MO onto CuS-NP-AC depends largely on pH and maximum
removal was achieved at pH 5.0. CuS-NP-AC is an efficient adsorbent
for removal of high amount of MO in a short time (4.0 min). The
sorption of MO was found to decrease with the increase in initial MO
Table 4
Comparison of methyl orange adsorption capacity of copper sulfide nanoparticles loaded
concentration and increase with the increase in adsorbent dosage.
on activated carbon with some reported literatures. Equilibrium sorption data showed good fit to Langmuir isotherm
model and maximum MO sorption capacity of the sorbent was found
Adsorbent Adsorption capacity References
to be 122 mg/g. The pseudo second-order kinetic model was found to
(mg/g)
be best correlated to the experimental data for MO sorption.
Protonated cross-linked chitosan 89 [11]
Multiwalled carbon nanotubes 42–78 [36]
Carbon coated monolith 47–23 [37] Acknowledgment
Ammonium-functionalized silica 105 [13]
nanoparticle The authors express their appreciation to the Graduate School and
Copper sulfide nanoparticles loaded 122 Present work Research Council of the University of Yasouj for the financial support
on activated carbon
of this work.
 P. Mokhtari et al. / Journal of Molecular Liquids 219 (2016) 299–305 305

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