Arabian Journal of Chemistry (2015) 8, 858864

King Saud University

Arabian Journal of Chemistry

www.ksu.edu.sa
www.sciencedirect.com

ORIGINAL ARTICLE

Dried activated sludge as an appropriate biosorbent

for removal of copper (II) ions
Hossein Zare a, Hamid Heydarzade a, Mosatafa Rahimnejad
Meysam Sey a, Seyed Mohsen Peyghambarzadeh b
a
b

a,*

, Ali Tardast a,

Faculty of Chemical Engineering, Noshirvani University of Technology, Babol, Iran

Department of Chemical Engineering, Mahshahr branch, Islamic Azad University, Mahshahr, Iran

Received 25 July 2012; accepted 13 November 2012

Available online 29 November 2012

KEYWORDS
Dried activated sludge;
Copper ions;
Removal efciency;
Kinetic model;
Adsorption isotherm;
Biosorption

Abstract Removal of Cu (II) from aqueous solution by dried activated sludge (DAS) was investigated. Batch process for the biosorption of Cu (II) ions was performed to determine equilibrium
and adsorption characteristics of DAS. Obtained results by scanning electron microscope showed
DAS pretreated with 1% H2O2 was porous and also it had effective removal for Cu (II) ions from
aqueous solutions. Effects of contact time, temperature, pH and DAS dosage on the biosorption of
Cu (II) were studied. The maximum biosorption of Cu (II) at temperature of 20 C and pH of 5 was
obtained (85%) with the DAS dosage of 3.5 g/L, Cu (II) ion concentration of 100 mg/L and 4 h
contact time. Also removal efciency of Cu (II) decreased with increasing temperature. Langmuir,
Freundlich and DubininRadushkevich (DR) models were employed to study biosorption isotherms for removal of Cu (II). WeberMorris, pseudo rst order and pseudo second order models
were applied to describe the biosorption kinetics.
2012 Production and hosting by Elsevier B.V. on behalf of King Saud University.

1. Introduction
Chemical industries release heavy metals as toxic pollutants
into the environment. Copper (II) is one of the most common
* Corresponding author. Tel.: +98 9111283184; fax: +98 111
3234204.
E-mail addresses: [email protected] (H. Zare), Hamid.heydarzade
@yahoo.com (H. Heydarzade), [email protected], Rahimnejad
[email protected] (M. Rahimnejad), [email protected]
(A. Tardast), [email protected] (M. Sey), peyghambarzadeh
@gmail.com (S.M. Peyghambarzadeh).
Peer review under responsibility of King Saud University.

Production and hosting by Elsevier

heavy metal ions in industrial efuents. Intake of copper

causes mucosal, irritation, hepatic and capillary damage
(Ajmal et al., 1998; Yao et al., 2010). Currently, treatment processes are oxidationreduction, membrane ltration-osmosis,
ion exchange, precipitation, adsorption and biosorption (Fu
and Wang, 2011; Igwe and Abia, 2009; Ko et al., 2000;
Malakootian et al., 2009). Biosorption is one of the most
promising processes for removal of heavy metals from municipal and industrial wastewater (Akar and Tunali, 2006; Mona
et al., 2011). Biosorption of heavy metals has advantages such
as low costs, metal recovery, regeneration of biosorbent and
high efciency in detoxifying very dilute efuents (Mo and
Lian, 2011; Volesky, 2001; Waseem et al., 2014).
Biosorbents are potential inexpensive alternative to conventional adsorbents. In biosorption, both living and dead microbial cells are able to absorb heavy metal ions (Choi et al., 2009;

1878-5352 2012 Production and hosting by Elsevier B.V. on behalf of King Saud University.
http://dx.doi.org/10.1016/j.arabjc.2012.11.019

Dried activated sludge as an appropriate biosorbent for removal of copper (II) ions
Filipovic-Kovacevic et al., 2000). Since living cells require
addition of nutrients, the BOD and COD of the wastewater often are increased by using living cells (Rezaei et al., 2011).
Dead cells have been gaining advantage because of toxic ions
that do not affect on stabilized biomass. Besides, dead cells require less maintenance and also are effortlessly regenerated
(Das et al., 2008; Khosravan and Lashkari, 2011).
Activated sludge is an effective biomaterial for biosorption
or bioleaching of the metal ions such as Cd (II), Zn (II), Pb (II)
and Cu (II) from wastewater. The removal of heavy metals
from wastewater using activated sludge is highly efcient and
has low installation and operation and maintenance costs
(Buyukgungor and Gurel, 2009; Gavrilescu, 2004; Hussein
et al., 2005). Activated sludge is a biosorbent with different
functional groups such as carboxylic acid, carboxyl and amine
groups (Gulnaz et al., 2006). It is composed of both live and
dead microbial fractions. Many reports have shown that aldehyde, carboxyl, sulfhydryl, phosphoryl, hydroxyl, amine organic and acidic functional groups in biomass are the most
important functional groups that could eliminate metal ions
from aqueous solutions (Arief et al., 2008; Marandi, 2011;
Zhang and Banks, 2006). The formation of functional groups
in biomass may enhance with the pretreatment method such as
heating, autoclaving, acidic treatment and alkali treatment
(Pereira, 2001; Shroff and Vaidya, 2011).
The aim of the present research was to investigate biosorption of Cu (II) ions by dried activated sludge (DAS). Effects of
contact time, pH, temperature and DAS dosage on biosorption of Cu (II) ions were studied. Langmuir, Freundlich and
DubininRadushkevich (DR) were applied to obtain biosorption isotherms. Also biosorption kinetics was described by
WeberMorris, pseudo rst order and pseudo second order
models.
2. Materials and methods
2.1. Preparation of the biosorbent and stock solution
The activated sludge used in this study was collected from pulp
and paper wastewater treatment plant (Mazandaran Pulp and
Paper plant, Iran). Initially activated sludge was suspended in
500 ml of 1% H2O2 solution in a beaker with a magnetic
stirrer (VELP, SCIENTIFICA, Italy) for 12 h at 25 C. The
suspension was then centrifuged (HERMLE, Germany) at
5000 rpm for 8 min. The resulted cake was washed with deionized water until the pH of the solution decreased to 7. The cake
was dried in oven (Binder, Germany) at 65 C for 48 h. The
dried biomass was grinded and sieved with mesh No. 35 into
particle size smaller than 0.5 mm. Copper stock solution with
concentration of l00 ppm was prepared using analytical grade
of CuSO45H2O (Merck, Darmstadt, Germany). The stock
solution was diluted with double distilled water to obtain desired solutions.
2.2. Batch experiments
Biosorption of Cu (II) onto DAS was carried out by batch
experiments. Biosorption experiments were performed in
250 ml Erlenmeyer asks containing 100 ml of aqueous solution with an initial concentration of 100 ppm Cu (II). For optimization of contact time, pH and adsorbent dosage, batch

859

experiments were carried out at 20 C in incubator shaker

(Excella E24, New Brunswick Scientic, Edison, NJ) at
120 rpm. Batch experiments were performed with contact time
0.5 to 4 h, pH 26, adsorbent dosage 1.53.5 g/L and temperature range from 20 to 50 C. The required pH of aqueous
solution was adjusted by adding 0.2 M HCl and 0.1 M NaOH.
The pH of the solution was measured using a pH meter
(HANA 211, Romania) model glass-electrode. After that, the
biosorption kinetics and isotherm studies were carried out under optimized condition of pH, contact time and adsorbent
dosage. All experiments were carried out twice. Data reported
in this study were the means of the duplicate experimental results. Treated samples were ltered through a paper lter.
2.3. Analytical methods
In order to remove solid particles, the samples were centrifuged
at 10000 rpm for 8 min and then ltered. The concentration of
Cu (II) in the samples was determined using an atomic absorption spectrometer (ATI Unicam 929 AA, England) at 324.8 nm
wavelength according to procedure reported in standard methods (American Public Health Association (APHA), 2005). The
removal efciency and the amount of metal adsorbed per unit
mass of the adsorbent were calculated as 100 (CiCf)/Ci and
(CiCf) V/m (mg/g), respectively; where Ci and Cf (mg/L)
are the initial and nal concentrations of Cu (II) ions, V (L) is
the volume of the solution and m is the amount of adsorbent (g).
The specic surface area and the porosity of the DAS were
determined by BET adsorption isotherm of nitrogen gas in a
micromeritics porosimeter ASAP 2010 V2.00 A (Micrometrics
Instrument Co., USA). The percentage of carbon, nitrogen
and hydrogen in the DAS was analyzed with an element analyzer (Heraeus CHNO, USA) and acetanilide was used as the
standard. Also the ash content of DAS was determined with
the analysis method according to ASTM D2866-94. In order
to investigate on surface morphology of DAS, the sample was
dried and gold coated with a sputtering coater (Emitech
K575X, England). The morphology of DAS was studied by
Scanning Electron Microscope (VEGAnTESCAN, Czech
Republic).
3. Results and discussion
3.1. Properties of DAS
Biosorption capacity and specic surface area of DAS were increased with pretreatment with H2O2. The Characteristics of
DAS used in this work are summarized in Table 1. The

Table 1

Characteristics of the DAS treated by H2O2.

Parameter

Values

Size range
Bulk density
Porosity
Specic surface area
Ash
C
N
H

<0.50 mm
0.88 g/cm3
45%
183 m2/g
18%
42%
6.7%
3.5%

860
90

Removal efficiency (%)

activated sludge was suspended in a 1% H2O2 solution for

12 h. The pretreated activated sludge showed better performance for the copper sorption (see Fig. 2). This result may
be explained that some functional groups on the surface of
DAS can be oxidized and activated by H2O2 (Pamukoglu
and Kargi, 2006). In order to investigate the surface morphology of the DAS, scanning electron microscopy (SEM) image
was taken. Fig. 1 shows the pore structure of the DAS which
it can be resulted from pretreatment of DAS by H2O2. According to SEM image, the DAS as an adsorbent was sufciently
porous and can be used for adsorption of Cu (II) ions.

H. Zare et al.

80
70
60
50
40

3.2. Effect of contact time

3.3. Effect of pH
Biosorption of Cu (II) at temperature of 20 C was carried out
with DAS dosage of 3.5 g/L, Cu (II) ion concentration of
100 mg/L and contact time of 4 h. Since at pH higher than 6
hydrate structures of the Cu (II) ions formed and the metal
ions precipitate in the solution, effect of pH was investigated
in the pH range from 2 to 6. Fig. 3 shows the effect of pH value

30
0

t (h)
Figure 2

The effect of contact time on the biosortion.

90

Removal efficiency (%)

The equilibrium contact time is an important parameter for

adsorption process. In order to determine the effect of contact
time, biosorption was performed for 4 h. Fig. 2 demonstrates
contact time effects on biosorption of Cu (II) onto treated
and untreated DAS. For untreated Das, removal efciency
reached to 76% after 4.5 h. For Das treated with H2O2, removal efciency rapidly increased during the initial adsorption
stage and reached to 83.5% when contact time was 3 h. Then
the removal efciency gradually increased with contact time
and equilibrium was reached after 4 h. At equilibrium, removal
efciency was 85% and then it was constant. At initial stage,
adsorption of Cu (II) onto monolayer surface of DAS may explain the rapid increase in removal efciency. After that the
monolayer surface was saturated, the Cu (II) ions were gradually adsorbed into the inner part of DAS with diffusion; therefore lower biosorption rate was obtained.

DAS
DAS treated with H2O2

80
70
60
50
40
30
20
1

pH
Figure 3

Effect of pH on the biosorption.

on biosorption of Cu (II) onto DAS. Removal efciency of Cu

(II) increased with an increase in pH solution, reached at a
maximum value of 85% at pH 5 and then slightly decreased
and reached to 83%. In acidic solution, H+ ions compete with
Cu (II) for the adsorption site, which impedes biosorption of
Cu (II) by DAS.
3.4. Effect of DAS dosage and temperature

Figure 1 Scanning electron microscopy image of the DAS with

magnication of 5000.

Effect of DAS dosage on adsorption isotherm for removal of

Cu (II) at four different temperatures was also investigated
and obtained results are presented. Fig. 4 shows the removal
efciency of Cu (II) at DAS dosage of 13.5 g/L and temperature of 2050 C. Removal efciency increased with an increase in DAS dosage; meanwhile as the temperature was
increased, the removal efciency for the same dosage of
DAS decreased. It is obvious that desorption rate increased
as the temperature was increased, which implies that the
adsorption afnity decreased. In order to evaluate adsorption
isotherm, Langmuir and Freundlich models were tted to
experimental data.

Dried activated sludge as an appropriate biosorbent for removal of copper (II) ions
T = 20 oC
T = 30 oC
T = 40 oC
T = 50 oC

80

T = 20 oC
T = 30 oC
T = 40 oC
T = 50 oC

3.5
3.0

Ce/qe (g/l)

Removal efficiency (%)

100

60

40

861

2.5
2.0
1.5
1.0

20

0.5
0.0

0
0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

10

20

30

40

50

60

70

80

Ce (mg/l)

DAS dosage (g)

Figure 4 The effect of DAS dosage and temperature on the
biosorption.

Figure 5 Langmuir isotherm model for the biosorption of Cu

(II) ions onto DAS.

3.5. Biosorption isotherms

Table 2 Langmuir isotherm model parameters for biosorption of Cu (II) ions onto DAS.

The Langmuir model is valid for monolayer adsorption containing nite number of identical biosorption sites. In this case
interaction between adsorbate particles is negligible. The
Langmuir model is given by the following equation (Langmuir,
1918):

Temperature (C)

qm KL Ce
1 KL Ce

where Ce (mg/L) is the equilibrium concentration of the

solution, qm (mg/g) is the maximum amount of metal ions required to form monolayer, K (L/mg) is the adsorption equilibrium constant related to the sorption energy between the
adsorbate and adsorbent and qe (mg/g) is the amount of metal
adsorbed per specic amount of adsorbent. In order to conveniently determine Langmuir constants, Eq. (1) can be rearranged to a linear form as follows (Mo and Lian, 2011):
Ce
1
Ce

qe KL qm qm

The equilibrium data were analyzed using the linearized

form of Langmuir adsorption isotherm Eq. (2). Langmuir constants, KL and monolayer biosorption capacity, qm were calculated from the slope and intercept of the plot Ce/qe versus Ce
(Fig. 5). The maximum copper sorption capacity of DAS
was obtained (91 mg/g) at 20 C. The qm was one and a half
times higher than that was obtained (62.5 mg/g) by Benaissa
and Elouchdi (2011). The Langmuir isotherm constants are
shown in Table 2.
The Freundlich isotherm model is employed to describe heterogeneous surfaces that represents the binding sites are not
equivalent and/or independent. This model considers repulsive
interactions between adsorbed solute particles (Freundlich,
1906; Sinha et al., 2012). Freundlich equation is given as follows:
qe KF Ce 1=n

20
30
40
50

logqe logKF

qm (mg/g)

KL (L/mg)

R2

91
67
45
27

0.024
0.027
0.033
0.068

0.975
0.989
0.997
0.994

 
1
log Ce
n

As shown in Fig. 6, the plot of log qe versus log Ce was tted linearly for Freundlich isotherm model. Freundlich isotherm parameters, KF and 1/n were calculated from the slope
and intercept of linear plots of log qe and log Ce. The Freundlich parameters for adsorption of Cu (II) ions on DAS at different temperatures are summarized in Table 3.

2.0
T = 20 oC
T = 30 oC
T = 40 oC
T = 50 oC

1.8

log (q e)

qe

Langmuir isotherm constants

1.6
1.4
1.2
1.0

where n is the adsorption intensity and KF is the adsorption

capacity (mg/g)(L/mg)1/n. Freundlich equation can be linearized in logarithmic form for the convenience of plotting and
determining Freundlich isotherm parameters (Eq. (4)):

1.0

1.2

1.4

1.6

1.8

2.0

log (Ce )
Figure 6 Freundlich isotherm model for the biosorption of Cu
(II) ions onto DAS.

862

H. Zare et al.

The DR isotherm model was employed to determine the

nature of the biosorption process. Linearization of this model
is presented in Eq. (5) (Dubinin et al., 1947):
lnQe lnQm  be2

-7.0

-7.5

where Qm (mol/g) is the monolayer capacity, and b (mol /J ) is

the activity coefcient related to biosorption energy, Qe (mol/g)
is the amount of copper ions adsorbed per unit mass of the
adsorbent and e is the Polanyi potential given as follows:

 
1
6
e RT ln 1
Ce

ln (Qe)

-8.0

The mean free energy E (J/mol) of biosorption for the transfer

of adsorbate from the innity to the adsorbent surface is given
as follows:
1
E p
2b

-8.5
2

2 108

the E values below 8 kJ/mol indicate, physisorption mechanism is the dominant mechanism of adsorption, and the values
between 8 and 16 kJ/mol show the chemisorption mechanism
of adsorption (Sari and Tuzen, 2008). A representative plot
of DR isotherm model is shown in Fig. 7. The DR isotherm
parameters are summarized in Table 4. Obtained results based
on E values indicated that chemisorption is the dominant
mechanism of biosorption.
3.6. Kinetics models
Kinetics models of biosorption were investigated by Weber
Morris, pseudo-rst-order and pseudo-second-order models.
With the purpose of kinetic study of Cu (II) ions biosorption
on DAS, variation in the concentration of adsorbate on
biosorbent with mixing time was described by the following
equation (Weber and Morris, 1963):
qt Rid t1=2 C

1/2

where Rid (h
) is the rate constant for the intra-particle diffusion and C (mg/g) is the intercept constant of the plot that is related to the boundary layer thickness, qt (mg/g) is the adsorbed
concentration of Cu (II) ions with respect to the time t. The
WeberMorris model represents multi linearity which indicates
that adsorption may occur in two or more steps. As shown in
Fig. 8a, in the rst stage, the sharp slope of the line was attributed to the diffusion of Cu (II) ions through the solution to
the external surface of the adsorbent. In the second stage, the
low slope of the line was caused by a low diffusion rate of Cu
(II) adsorption onto internal pore surface of DAS.
The intra-particle diffusion rate constants were calculated
from the slope of the linear plots. The WeberMorris constants

Table 3 Freundlich isotherm model parameters for biosorption of Cu (II) ions onto DAS.
Temperature (C)

20
30
40
50

T = 20 oC
T = 30 oC
T = 40 oC
T = 50 oC

Freundlich isotherm parameters

n

KF

R2

1.74
2.02
2.48
4.3

5
5.37
5.65
8.20

0.995
0.998
0.986
0.896

Figure 7 DR isotherm model for the biosorption of Cu (II) ions

onto DAS.

Table 4 DR isotherm model parameters for biosorption of

Cu (II) ions onto DAS.
Temperature (C)

DR isotherm parameters
b (mol2/J2)

20
30
40
50

9

5.12 10
4.55 109
3.84 109
2.28 109

Qm (mg/g)

R2

E (kJ/mol)

149
103
65
41

0.994
0.997
0.989
0.905

9.88
10.48
11.41
14.80

(Rid, C) for the rst and second stages were Rid = 11.8 h1/2,
C = 5.09 mg/g and Rid = 2.39 h1/2, C = 19.59 mg/g,
respectively.
Also the kinetic modeling of Cu (II) adsorption onto DAS
was studied by two common models which are pseudo-rst-order and pseudo-second-order kinetic equations. Lagergren
pseudo-rst-order rate is given as follows (Lagergren, 1989;
Zhou et al., 2007):
logqe  qt log qe 

k:t
2:303

where k (h1) is the rst order rate constant and qe (mg/g) is

the sorbed concentration at equilibrium. As shown in
Fig. 8b, the linear plot of log(qeqt) versus time t (h) demonstrates the applicability of the pseudo-second-order model
for Cu (II) adsorption onto DAS. The pseudo-rst-order rate
constant and the correlation coefcient were k = 0.671 h1
and R2 = 0.96, respectively.
The kinetic data for Cu (II) ions adsorption onto DAS was
subjected to pseudo-second-order model given by the following equation (Ho and McKay, 1999; Wang and Guo, 2011):
t
1
t

qt Kq2e qe

10

where K (g/mg h) is the second order rate constant and qe (mg/

g) is the adsorbed concentration at equilibrium. The pseudosecond-order rate constant was from the slope and intercept
of the line drawn based on obtained experimental data
(Fig. 8c). The rate constant and correlation coefcient were
K = 0.058 g/mg h and R2 = 0.99, respectively.

Dried activated sludge as an appropriate biosorbent for removal of copper (II) ions

(a) 0.18

concentration of 100 mg/L, DAS dosage of 3.5 g/L and contact time of 4 h. Also it was found that the increase of temperature had a negative impact on biosorption of Cu (II) onto
DAS.

t/qt (mg.h/g)

0.15
0.12

Acknowledgment
0.09

The authors wish to acknowledge the Noshirvani University of

Technology, Babol, Iran and Islamic Azad University,
Mahshahr, Iran for the facilities provided to accomplish this
research.

0.06
0.03
0.00
0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

t (h)

(b)

1.5

log (qe -qt)

1.0
0.5
0.0
-0.5
-1.0
-1.5
0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

t (h)

(c)

30
25

qt (mg/g)

863

20
15
10
5
0
0.0

0.5

1.0

1/2

1.5

2.0

2.5

1/2

(h )

Figure 8 Kinetic models for the biosorption of Cu (II) ions onto

DAS, (a) WeberMorris, (b) pseudo-rst-order and (c) pseudosecond-order.

4. Conclusions
In this research, the DAS showed effective removal of Cu (II)
from synthetic aqueous solutions. Langmuir, Freundlich and
DR isotherm models were well tted to experimental data.
Biosorption kinetics was studied by WeberMorris, pseudo
second order and pseudo second order models. The Maximum
removal efciency of Cu (II) was 85% at temperature of 20 C
and pH of 5; this result was obtained with the Cu (II) initial

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