Journal of Hazardous Materials 177 (2010) 950955

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Journal of Hazardous Materials
j our nal homepage: www. el sevi er . com/ l ocat e/ j hazmat
Adsorption of Ag, Cu and Hg from aqueous solutions using expanded perlite
Hamid Ghassabzadeh
a,
, Ahmad Mohadespour
b
, Meisam Torab-Mostaedi
c
,
Parisa Zaheri
b
, Mohammad Ghannadi Maragheh
c
, Hossein Taheri
c
a
Department of Chemical Engineering, Tarbiat Modarres University, P.O. Box 14115-143, Tehran, Iran
b
School of Chemical Engineering, University College of Engineering, University of Tehran, P.O. Box 11365-4563, Tehran, Iran
c
Nuclear Fuel Cycle Research School, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran, Iran
a r t i c l e i n f o
Article history:
Received 21 October 2009
Received in revised form 2 January 2010
Accepted 4 January 2010
Available online 11 January 2010
Keywords:
Expanded perlite (EP)
Silver
Copper
Mercury
Adsorption
a b s t r a c t
The aim of the present work was to investigate the ability of expanded perlite (EP) to remove of silver,
copper and mercury ions from aqueous solutions. Batch adsorption experiments were carried out and
the effect of pH, adsorbent dosage, contact time and temperature of solution on the removal process has
been investigated. The optimum pH for the adsorption was found to be 6.5. Adsorption of these metal
ions reached their equilibrium concentration in 120, 240 and 180min for Ag (I), Cu (II) and Hg (II) ions,
respectively. Experimental data were alsoevaluatedinterms of kinetic characteristics of adsorptionandit
was foundthat adsorptionprocess for thesemetal ions followedwell pseudo-second-order kinetics. Using
Langmuir isothermmodel, maximumadsorption capacity of EP was found to be 8.46, 1.95 and 0.35mg/g
for Ag (I), Cu (II) and Hg (II) ions, respectively. Finally, the thermodynamic parameters including, the
change of free energy (G

), enthalpy (H

) and entropy (S

) of adsorption were calculated for each

metal ion. The results showed that the adsorption of these metal ions on EP was feasible and exothermic
at 2050

C.
2010 Elsevier B.V. All rights reserved.
1. Introduction
In the natural aquatic systems, sorption processes play a dom-
inant role in the transport and ultimate fate of pollutants such as
heavy metals [1]. Heavy metals are dened as those metals and
metalloids generally considered to be of sufcient distribution and
abundance as to be in some way environmentally or biologically
signicant as a toxic substance. These include metals such as lead
(Pb), chromium (Cr), copper (Cu), cadmium (Cd), nickel (Ni), silver
(Ag), mercury (Hg), and zinc (Zn) [2].
A number of methods including precipitation and adsorption
have been employed for the removal of copper from industrial
efuents. Precipitation is the most frequently used method. An
adsorption process can be an attractive alternative method for
Cu (II) removal, if a low cost adsorbent that can be regenerated
for repeated use is available [3]. Activated carbon is a commonly
used adsorbent for the removal of pollutants present in water and
wastewaters. Sigworth and Smith [2] showed that the removal of
various heavy metal ions from aqueous solutions can be achieved
using activated carbon. Inspite of its effectiveness inthe removal of
heavy metals from wastewaters, the high cost of activated carbon
has restricted its more widespread use [4]. Hence, an economical

Corresponding author. Tel.: +98 914 410 210 6.

E-mail address: h.ghassabzadeh@gmail.com (H. Ghassabzadeh).
andeasilyavailableadsorbent wouldcertainlymakeanadsorption-
based process a viable alternative for the treatment of wastewater
containing heavy metals [2].
Silver is a useful raw material in industries due to its excellent
malleability, ductility, electrical and thermal conductivity, pho-
tosensitivity and antimicrobial properties. Signicant amount of
silver are lost in the efuents discharged from such industries and
due to the toxicity of silver to living organisms, the removal of this
element from wastewaters is an important concern [5].
Copper containing waste streams are generated from a vari-
ety of industries including metal nishing, copper electroplating,
and cooling water systems. The concentration of copper in these
streams can be in the range of 202200mg/L. The maximum con-
taminant level goal for copper, as suggested by the US EPA, is
1.3mg/L. Therefore, copper concentration of any industrial efu-
ents should be reduced below 1.3mg/L before discharging to the
environment. Although copper can exist as Cu (0), Cu (I), and Cu
(II), the main species of concern in aqueous solution is Cu (II) [6].
Cu (II) binds easily to organic and inorganic matter in aqueous solu-
tion based on solution pH. These Cu (II) species pose a signicant
threat to aquatic life and render natural water unsuitable for the
public use [3].
Mercury pollution results frommetallurgical industries, chemi-
cal manufacturing and metal nishing industries. Hg in liquid form
in not dangerous and it is used in a number of industries. In vapor
form, Hg becomes very poisonous [7].
0304-3894/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2010.01.010
H. Ghassabzadeh et al. / Journal of Hazardous Materials 177 (2010) 950955 951
Table 1
Chemical composition of expanded perlite.
Constituent Percentage (wt.%)
SiO
2
79.6
Al
2
O
3
11.5
K
2
O 4.8
CaO 0.8
Fe
2
O
3
0.8
Na
2
O 0.5
MgO 0.5
SO
3
0.2
TiO
2
0.1
MnO
2
0.065
Perlite is a natural occurring dense glassy volcanic ryholitic
rock and can be expanded up to 20 times its original volume
when heated rapidly at 8001200

C [8]. Expanded perlite (EP)

acts as an excellent insulator, both thermal and acoustical, resists
re and is classied as ultra-light weight materials. The expanded
perlite is white in color, and has a density of about 32kg/m
3
.
Perlite is generally chemically inert and has a pH of approxi-
mately 7. Perlite is very cheap and easily available in Iran markets.
The cost of expanded perlite is less than US$ 0.2 per kg in Iran.
This could make it a viable candidate as an economical adsorbent
for removing heavy metals such as lead, copper, cadmium and
chromium [911].
In this study, the adsorption potential of expanded perlite in the
removal of Ag (I), Cu (II) and Hg (II) ions fromaqueous solutions has
been studied. The effects of pH, adsorbent dosage, contact time and
temperature on adsorption capacity of EP have been investigated.
Based on these studies, the Langmuir and Freundlich isotherm
models were usedtot the equilibriumdata. Finally, the adsorption
kinetic of these ions was evaluated.
2. Experiments
2.1. Adsorbent characterization
Expanded perlite samples were obtained from Kaneh Azar Co.
(Tabriz, Iran). The expanded perlite was used without any chemical
treatment for the sorption reported here. The chemical composi-
tion of the perlite which was determined by XRF is given in Table 1.
It is mainly composed of silica as SiO
2
(79.6%), aluminum as Al
2
O
3
(11.5), and potassium as K
2
O (4.8%). The specic surface area of
expanded perlite is 1.89m
2
/g. It was measured by BET-N
2
adsorp-
tion.
In the surface hydroxyl groups, the silicon atoms at the
surface tend to maintain their tetrahedral coordination with
oxygen. They complete their coordination at room tempera-
ture by attachment to monovalent hydroxyl groups, forming
silanol groups. The different types of silanol groups are shown as
follows:
The hydrous oxide surface groups in alumina are given as fol-
lows:
It is these groups that give the adsorption property to perlite
[2,12].
2.2. Experimental studies
The solutions containing 1000mg/L of Ag
+
, Cu
2+
and Hg
2+
were
prepared using analytical grade AgNO
3
, CuCl
2
and HgCl
2
salts,
respectively. All other solutions were dilutedfromthese stock solu-
tions.
Several experiments were carried out to identify the optimum
values of pH, contact time and adsorbent dosage. The pH values
were adjusted at 2, 3, 4, 5, 6.5 and 8 using 0.1M NaOH or HNO
3
solution. The effect of adsorbent dosage on removing metal ions
from solutions was studied by using 10mg/L as initial solution in
conjunction with 1, 2, 4, 6, 8, 10, 12, 14, 16 and 18g/L of EP. At
the optimum dosage, other experiments were done. Samples were
collected at 5, 10, 15, 30, 45, 60, 90, 120, 150, 180, 240 and 360min
to determine the optimum value of shaking time. Isotherm studies
were carried out at 5, 10, 20, 30, 40 and 50mg/L as initial solution
concentration and optimum EP dosage and adsorption time. Other
adsorption experiments were also done at 20, 30, 40, and 50

C to
determine the effect of temperature on the adsorption process and
to evaluate the adsorption thermodynamic parameters.
Experiments were carried out at a 250mL conical ask lled
with 100mL of test solution. Necessary amount of adsorbent
material was added. The ask was then shaken for the desired
contact time in an electrically thermostatic reciprocating shaker at
110rpm. The contents of asks were ltrated through lter paper.
The ltrate was then analyzed for metal concentration by using
inductively coupled plasma-atomic emission spectroscopy (ICP-
AES). The adsorption percentage of metal ions was calculated as
follows:
Adsorption(%) =
C
i
C
f
C
i
100 (1)
where C
i
and C
f
are the initial and nal metal ion concentrations,
respectively.
The amount of metal ions adsorbed per unit mass of adsorbent
(q
e
) was calculated using the following equation:
q
e
=
V
M
(C
i
C
e
) (2)
where C
i
and C
e
represent initial and equilibrium concentrations
(mg/L), respectively. V is the volume of the solution (L) and Mis the
mass of the adsorbent (g).
The average absolute value of relative error, AARE, was used
to compare the predicted results with experimental data. This is
dened as follows:
AARE =
1
NDP
NDP

i=1
|PredictedValue Experimental Value|
Experimental Value
100(3)
in which NDP is the number of data points.
3. Results and discussion
3.1. Effect of pH
The pH of solution has an important role in metal ions adsorp-
tion. This is partly because hydrogen ions themselves are strongly
952 H. Ghassabzadeh et al. / Journal of Hazardous Materials 177 (2010) 950955
Fig. 1. Effect of pH on the adsorption of Ag, Cu and Hg onto EP.
competing with metal ions [11]. The percentage of metal ions
removed from solution versus pH is shown in Fig. 1. At low pH val-
ues (pH<4), the low adsorption observation can be explained due
to increase in positive charge (protons) density on the surface sites
and thus, electrostatic repulsion occurs between the metal ions
and the edge group with positive charge (M-OH
2
+
) on the surface
[2,11,13]:
MOH+HOH
H
+
MOH
2
+
+OH

At higher pH values (4<pH<6), the surface of EP becomes neg-

ative charged and thus electrostatic repulsion decreases with an
increase in pH value. Reduction of positive charge density on the
sorption edges results an increase in metal adsorption, e.g.:
MOH MO

+H
+
MO

+Cu
2+
MOCu
+
More increase in pH values leads to metal precipitation and
metal accumulation on EP surface deteriorated the adsorption
mechanism. Therefore, kinetic studies above pH 7 were not
attempted due to the precipitation of metal ions as hydroxides.
The pH of initial solution of metal ions mixed with EP without
any control is about 6.5 which have the most adsorption percent-
age. Therefore, all experiments were carried out at pH 6.5 without
any pH adjustment.
3.2. Effect of adsorbent dosage
The effect of adsorbent dosage on the adsorption of Ag, Cu and
Hg ions is shown in Fig. 2. These data have been obtained at initial
metal concentration, pHand temperature equal to 10mg/L, 6.5 and
20

C, respectively. This gure shows that adsorbent dosage has an

important role in adsorption process. Increasing adsorbent dosage
has been sharply increased Ag (I), Cu (II) and Hg (II) adsorption to
more than 99, 90 and 30%, respectively.
The increase in the removal efciency may be attributed to the
fact that anincrease inadsorbent dosage means increasing the ratio
of adsorbent weight/solution volume, m(g)/V(L). Then the uptake
is higher because the increased mass of solid phase. The adsorption
percentages of Ag(I), Cu(II) andHg(II) arealmost at highest amount
at 8, 10 and 14g/L adsorbent dosage, respectively. More increase
in adsorbent dosage did not have signicant effect in adsorption
percentage. Therefore, these values have been selected for further
adsorption experiments.
Fig. 2. Effect of adsorbent dosage on the adsorption of Ag (I), Cu (II) and Hg (II) ions
onto EP.
3.3. Effect of contact time and adsorption kinetics
Fig. 3 shows the adsorption percentage of Ag (I), Cu (II) and Hg
(II) metal ions as a function of contact time. As seen in this gure,
adsorption of these metals increased by contact time and reached
to a maximum value. More increase in contact time had no more
sensible changes in adsorption percentage. Hence, adsorption of
Ag (I), Cu (II) and Hg (II) reaches their maximums at 120, 240 and
240min, respectively. These values have been selected as optimum
contact time.
Lagergren rst-order and Ho et al.s pseudo-second-order rate
equations were used to describe the kinetics of these metal ions
adsorption onto EP. The rst-order Lagergren rate equation used
by researchers to study the kinetics of heavy metal adsorption is as
follows [2,11]:
q
t
= q
e
(1 e
k
1
t
) (4)
where k
1
, q
e
and q
t
are Lagergren rate constant of adsorption
(1/min), amount of metal ion adsorbed at equilibrium (mg/g),
and amount of metal ion adsorbed at any given time t (mg/g),
respectively. The adsorption rate constant (k
1
) can be determined
experimentally by tting non-linear Eq. (4). The results are shown
in Fig. 4 and Table 2.
Ho and McKay [14] used a pseudo-second-order rate equation
to study the kinetics of adsorption of heavy metals on peat. The Ho
et al. pseudo-second-order equation is given by:
t
q
t
=
1
k
2
q
2
e
+
t
q
e
(5)
Fig. 3. Effect of contact time on the adsorption of Ag (I), Cu (II) and Hg (II) ions onto
EP.
H. Ghassabzadeh et al. / Journal of Hazardous Materials 177 (2010) 950955 953
Fig. 4. Pseudo-rst-order kinetic model (Points: experimental data; Lines: kinetic
model values).
Table 2
Lagergren rate equation constants and pseudo-second-order rate equation
constants.
k
1
(min
1
) qe (mg/g) r
2
AARE %
Pseudo-rst-order
Ag 0.233 1.154 0.904 9.34
Cu 0.355 0.839 0.973 4.59
Hg 0.03885 0.223 0.819 21.6
k
2
(g/mgmin) qe (mg/g) r
2
AARE %
Pseudo-second-order
Ag 0.117 1.275 0.992 4.39
Cu 0.904 0.853 0.983 3.42
Hg 0.458 0.239 0.956 12.6
where it can be rearranged to:
q
t
=
k
2
q
2
e
t
1 +k
2
q
e
t
(6)
where k
2
is pseudo-second-order rate constant for adsorption
(g/mgmin).
This model is more likely to predict the kinetic behavior of
adsorption with chemical sorption being the rate controlling step
[11,15]. The q
t
versus time for adsorption of Ag, Cu and Hg onto EP
are shown in Fig. 5. The rate constant k
2
, q
e
, correlation coefcient
(r
2
) and AARE % values are given in Table 2.
Comparing the pseudo rst and second-order kinetic models
indicates that the adsorption of Ag, Cu, and Hg ions onto EP follows
Fig. 5. Pseudo-second-order kinetic model (Points: experimental data; Lines:
kinetic model values).
Table 3
Isotherm model parameters for the adsorption onto EP.
qm (mg/g) KL (L/mg) r
2
AARE %
Langmuir isotherm model
Ag 8.46 3.74 0.9998 1.76
Cu 1.946 0.738 0.9822 6.69
Hg 0.346 0.341 0.9863 2.83
1/n K
f
(L/g) r
2
AARE %
Freundlich isotherm model
Ag 0.650 9.08 0.9803 9.74
Cu 0.312 0.746 0.9467 10.1
Hg 0.225 0.137 0.9588 4.67
well the pseudo-second-order kinetics which is same as the results
reported in the literature [2,11,16].
3.4. Adsorption isotherm models
The adsorption isotherms reveal the specic relation between
the concentration of sorbent and its sorption degree onto adsor-
bent surface at constant temperature [11]. Thus, the adsorption
isotherms of these three metal ions were obtained at optimumpH,
adsorbent dosage and contact time by changing the initial concen-
tration of ions in solution in the range of 550mg/L.
The uptake of Ag, Cu and Hg ions increased as their concentra-
tions in the solution increased, and nally reached their saturation
capacity at a higher concentration. Adsorption of metal ions on
expanded perlite may be described by the one-site Langmuir equa-
tion:
1
q
e
=
1
q
m
+

1
q
m
K
L

1
C
e
(7)
where q
e
, q
m
and K
L
are adsorption capacity corresponding to
metal ion concentration C
e
, maximumadsorption amount of metal
ions (mg/L) andLangmuir adsorptionconstant (L/mg), respectively.
Experimental data correlated with non-linear Langmuir model.
Obtainedq
m
andK
L
parameters andalso correlationcoefcient (r
2
),
and AARE % values are reported in Table 3.
Furthermore, the Freundlich model which can be applied for
non-ideal sorption on heterogeneous surfaces and multilayer sorp-
tion has been used for adsorption isotherm data. The Freundlich
model in linear form is given as follows [13]:
log q
e
= log K
f
+
1
n
log C
e
(8)
where K
f
is a constant related to the adsorption capacity and 1/n is
an empirical parameter related to the adsorption intensity, which
varies with the heterogeneity of material. The values of Freundlich
model are also reported in Table 3. The q
e
curves versus C
e
are
shown in Figs. 68 for experimental equilibrium data and both
Langmuir and Freundlich models for Ag, Cu and Hg ions, respec-
tively.
The correlationcoefcient (r
2
) andAARE%whichare reportedin
Table 3 for bothLangmuir andFreundlichisothermmodels indicate
that both models are able to adequately describe the relationship
between q
e
and C
e
values. However, comparing the results demon-
strates that Langmuir isotherm model ts equilibrium data better
than Freundlich model.
The shape of the isotherm may also be considered to predict if
an adsorption system is favorable or unfavorable. The essential
characteristic of a Langmuir isotherm can be expressed in terms of
a dimensionless separation factor or an equilibrium parameter R,
which is dened by the following equation [9]:
R =
1
1 +K
L
C
e
(9)
954 H. Ghassabzadeh et al. / Journal of Hazardous Materials 177 (2010) 950955
Fig. 6. Isotherms models of Ag ion adsorption onto EP.
Fig. 7. Isotherms models of Cu ion adsorption onto EP.
According to the value of R, the isotherm shape may be inter-
preted as follows:

R>1: Unfavorable adsorption.

R=1: Linear adsorption.

0<R<1: Favorable adsorption.

R=0: Irreversible adsorption.

The values of R for Ag, Cu and Hg have been calculated
as 0.270.93, 0.030.47 and 0.060.52, respectively. Hence, the
adsorption of Ag, Cu and Hg ions onto EP is favorable.
Fig. 8. Isotherms models of Hg ion adsorption onto EP.
Table 4
Comparison EP adsorption capacity with other adsorbents.
Adsorbent Adsorption capacity (mg/g) Reference
Ag (I) Cu (II) Hg (II)
Zeolite 33.2 [5]
Coke 4.9 3.1 [17]
Peat 10.8 6.2 [17]
Bituminous coal 6.4 1.37 [17]
Multisorb 36.1 8.3 [17]
Low-rank Turkish coals 1.87 [18]
Low-rank Turkish coals 1.6 [19]
Peat 12.1 [20]
Red mud 5.3 [21]
Expanded perlite 8.62 [11]
Expanded perlite 0.18 [22]
Unexpanded perlite 0.26 [22]
Expanded perlite 0.51 [9]
Unexpanded perlite 1.01 [9]
Clay 12.84 [23]
Shells of lentil 9.59 [24]
Shells of wheat 17.42 [24]
Shells of rice 2.95 [24]
Turkish bentonite 2.62 [25]
Fullers earth 1.14 [26]
Activated Carbon 69.4 [26]
Eucalyptus bark 34.6 [27]
Activated carbon (walnut shell) 151.5 [28]
Expanded perlite (EP) 8.46 1.95 0.35 This study
In Table 4 the maximum adsorption capacity of expanded per-
lite has been compared to other adsorbents. From this table, it
can be concluded that the adsorption of silver (I) and copper (II)
onto expanded perlite is effective as much as other adsorbents. The
results illustrate that the adsorption of mercury (II) onto EP has not
favorable efciency. However from economical aspect, the cost of
adsorbent is also one important issue must be considered when
selecting an adsorbent. The regeneration and reuse of perlite may
also play an important role in making this a practical process. The
cost of regeneration/disposal of the spent adsorbent would have to
consider in any detailed economic analysis required to determine
the most economical adsorbent.
3.5. Adsorption thermodynamics
The adsorption isotherms obtained at various temperatures
were used to gain a better understanding of the adsorption mecha-
nism. Fromthe variations of K
d
with temperature, the integral heat
of adsorption can be calculated using the Vant Hoff equation [29]:
lnK
d
=
S

R

H

RT
(10a)
lnK
d
T
=
H

RT
2
(10b)
where K
d
, H

, S

, R, and T are distribution coefcient (L/g),

enthalpy change (J/mol), entropy change (J/mol), universal gas con-
stant (8.314J/mol K), and temperature (K), respectively.
According to Eq. (10a), (H

) and (S

) parameters can be indi-

vidually calculated from the slope and intercept of the plot of lnK
d
versus 1/T (Fig. 9). Gibbs free energy (G

) may be written in terms

of entropy and enthalpy:
G

= H

T S

(11)
The H

for the adsorption of Ag (I), Cu (II) and Hg (II) ions

are equal to 85.43, 18.63 and 6.28kJ/mol, respectively. These
negative values indicate the exothermic nature of the adsorption
of all metal ions onto EP in temperature range of 2050

C. The
values of S

are found to be 246.2, 45.18 and 27.30J/mol K

for the adsorption of Ag (I), Cu (II) and Hg (II), respectively. The
H. Ghassabzadeh et al. / Journal of Hazardous Materials 177 (2010) 950955 955
Fig. 9. lnK
d
vs. 1/T for estimation of H

and S

.
Fig. 10. Gibbs free energy (G

) vs. temperature.
negative values of S

suggest a decrease in the randomness at

solid/solution interface during the adsorption of ions onto EP [11].
The values of Gibbs free energy (G

) can be calculated directly

from Eq. (11). The G

versus temperature has been shown in

Fig. 10. The negative G

values indicate adsorption of Ag (I) and

Cu (II) are thermodynamically feasible and naturally spontaneous
at 2050

C. The positive and weak values of G

indicate that the

process is feasible but not spontaneous for the adsorption of Hg
(II) onto EP. Furthermore, the G

increased to a positive value

by increasing the temperature. Hence, the feasibility of adsorp-
tion is lower at higher temperature. Finally, as shown in Fig. 10,
the adsorption of Ag (I) onto EP is more sensitive than Cu (II) and
Hg (II) to temperature variance because it has a greater adsorption
enthalpy (H

) compared to the other metal ions.

4. Conclusions
The adsorption behavior of Ag (I), Cu (II) and Hg (II) onto
expanded perlite was investigated in the batch experiments. The
adsorption was found to be drastically dependent on pH, adsor-
bent dosage, and contact time. The optimum pH for adsorption
of all metal ions was found to be 6.5. The rate of these metal
ions adsorption was rapid. The silverperlite, copperperlite and
mercuryperlite systems attained equilibrium in 120, 240 and
180min, respectively. Isotherm analysis of the data showed that
the adsorption pattern of all three metal ions onto EP followed well
the Langmuir model. Using the Langmuir model equation, the max-
imum capacity of EP was found to be 8.46, 1.95 and 0.35mg/g for
Ag (I), Cu (II) and Hg (II) ions, respectively. The pseudo-second-
order rate equation described best the kinetic data of all metal
ions. Thermodynamic parameters depicted the exothermic nature
of adsorption and the process was favorable.
Finally, theresults showedthat EPhas ahighadsorptioncapacity
for silver which is comparable with other adsorbents. The copper
adsorptionontoEPwas fairlyhigh. Finally, EPcouldadsorbmercury
ions partially from aqueous solution (below 50% adsorption).
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