Bioresource Technology 97 (2006) 23502355

Removal of lead from aqueous solutions on palm shell activated carbon

Gulnaziya Issabayeva, Mohamed Kheireddine Aroua *, Nik Meriam Nik Sulaiman
Chemical Engineering Department, University Malaya, 50603 Kuala Lumpur, Malaysia
Received 30 June 2005; received in revised form 7 October 2005; accepted 17 October 2005
Available online 29 November 2005

Abstract
The performance of a commercially available palm shell based activated carbon to remove lead ions from aqueous solutions by
adsorption was evaluated. The adsorption experiments were carried out at pH 3.0 and 5.0. The eect of malonic and boric acid presence
on the adsorption of lead ions was also studied. Palm shell activated carbon showed high adsorption capacity for lead ions, especially at
pH 5 with an ultimate uptake of 95.2 mg/g. This high uptake showed palm shell activated carbon as amongst the best adsorbents for lead
ions. Boric acid presence did not aect signicantly lead uptake, whereas malonic acid decreased it. The diuse layer surface complexation model was applied to predict the extent of adsorption. The model prediction was found to be in concordance with the experimental
values.
2005 Elsevier Ltd. All rights reserved.
Keywords: Adsorption; Lead; Malonic acid; Boric acid; Modeling; Palm shell carbon

1. Introduction
The use of activated carbon to remove heavy metal ions
from wastewater by adsorption is a well-established process. The economics of this process depends mainly on
the cost of the adsorbent material. As such, low cost adsorbents are becoming the focus of many investigations. Low
cost adsorbents could be produced from many raw materials such as agriculture and industrial wastes. In Malaysia,
the palm oil industry generates huge amounts of palm shell.
Some of this solid waste is usually used as fuel to produce
process steam and/or electricity in palm oil mills. However,
a large portion of it is either burned in open air or dumped
in areas adjacent to the mill, which creates huge environmental and disposal problems. In recent years the interest
to palm shell has increased mainly due to the fact that
this material was shown to be an excellent source of high
quality and low cost activated carbon. However, most of
the research on palm shell carbon is focused on the
*

Corresponding author. Tel.: +60(3) 7967 5313; fax: +60(3) 7967 5319.
E-mail address: mk_aroua@um.edu.my (M.K. Aroua).

0960-8524/$ - see front matter 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2005.10.023

processes of carbonization and activation (Hussein et al.,

1996; Lua and Guo, 1998; Guo and Lua, 2000a,b, 2003;
Guo, 2002; Daud et al., 2002; Daud and Ali, 2004). Application of palm shell activated carbon as an adsorbent
oers highly eective technological means dealing with
heavy metals pollution of the aqua-environment with
minimum investment requirements. So far only few studies
focused on the adsorption properties of this material.
Othman et al. (1994) investigated adsorption of cadmium
and lead on the modied oil palm shell. Abu Bakar
(1999) and Salim et al. (2002) examined capacity of the
activated carbons obtained from the dierent parts of oil
palm and the modied palm shell activated carbon to
remove phenols from wastewaters. Chu and Hashim
(2002a,b) reported application of palm oil fuel ash in
removal of chromium and zinc from aqueous solutions.
There is a lack of information on the performance of palm
shell based activated carbon for the adsorption of heavy
metals from aqueous solutions.
In this work, the adsorption capacity of palm shell
activated carbon to remove lead ions from simulated
wastewaters was studied. The eects of solution pH and

G. Issabayeva et al. / Bioresource Technology 97 (2006) 23502355

presence of complexing agents (malonic and boric acids) on

the adsorption of lead were also evaluated.

2351

the speciation diagrams for single lead and lead with complexing agents systems.
3. Results and discussion

2. Methods
Commercial granular palm shell activated carbon
(PSAC) was provided by Pacic Activated Carbon a local
manufacturer in Johor Bahru, Malaysia. Activated carbon
granules with particle size ranging from 0.8 to 1.0 mm were
used throughout the experiments. NaNO3 and Pb(NO3)2
from Merck were used as the background electrolyte and
lead ions source, respectively. All solutions were prepared
in deionized water and the pH was adjusted by adding
small amounts of 0.1 M NaOH and HCl solutions. Malonic and boric acids stock solutions of 0.1 M were used to
adjust the proportion of ligand to the metal ion to a value
of 10:1 on a molar basis.
In a typical adsorption run, 500 mg of activated carbon
was equilibrated with 100 ml of lead ion solution at a constant temperature of 27 C. The equilibrated solution was
then subjected to ICP-AES (Varian, Liberty 200) analysis
in order to determine the concentration of residual lead
ion. The amount of lead ion adsorbed was calculated as
the dierence between the initial and nal lead concentration. The adsorption isotherm was obtained by varying
the initial concentration of lead ions from 10 to
700 ppm. The BET surface area of the activated carbon
was determined from N2 adsorption isotherm at 77 K
using BrunauerEmmetTeller equation. The N2 adsorption isotherm was determined using Micrometric ASAP
2010 system. Determination of the total acidity of PSAC
was carried out using Boehm method (Boehm, 1994). pH
of point of zero charge was determined using the pH
drift method (Lopez-Ramon et al., 1999; Mullet et al.,
1999).
The potentiometric titration experiments were carried
out in a glass cell at 25 C, under a OFN gas ow to prevent CO2 dissolution. In these experiments, 500 mg of activated carbon was placed in a ask containing 100 mL of
0.15 M NaNO3, and placed on a shaker at 27 C and
150 rpm for 48 h. Then the solution was titrated with
0.1 M HCl and/or NaOH. The titration was monitored
with a glass electrode paired with an internal Ag/AgCl/
KCl 3 M reference system. The electrode was calibrated
with buers at pH 4, 7 and 10 prior to the potentiometric
measurements. The equipment used included a microprocessor controlled burette and pH meter Metrohm 716
DMS Titrino controlled with a computer using TiNet 2.4
software. The potentiometric titration data were used to
obtain the pKa values of PSAC via application of the computer software Fiteql 4.0 (Herbelin and Westall, 1999).
Modeling on adsorption data was carried out using diffuse layer surface complexation model (Chen et al., 1996;
Faur-Brasquet et al., 2002; Borretzen and Salbu, 2003).
This model is incorporated in the VMinteq 2.15 software
(Gustafsson, 2003). The same software was used to obtain

Most of the studies on adsorption underline strong eect

of pH on adsorption process (Chen et al., 1996). In our
study, two pH values (3 and 5) were selected since this
pH range was a characteristic of industrial wastewaters in
Malaysia (DOE, 2002).
3.1. Characterization data on PSAC
The characterization data on PSAC are shown in Table
1. The data are shown in comparison with activated carbon
cloths (ACC) properties (Faur-Brasquet et al., 2002).
Despite having a surface area lower than ACC, palm shell
activated carbon was characterized by a high concentration
of surface acidic groups. This result indicated that palm
shell activated carbon exhibited higher adsorption capacity
since high acidity was responsible for the higher adsorption
of metal ions on the carbon surface. As reported by Boehm
(1994), the carboxylic acid groups reacted as more or less
weak acids. They exhibited a range of dissociation constants depending on the type of neighbouring groups.
The dissociation of carboxylic surface groups facilitated
the dispersion of the carbon in water by creating a negative
surface charge (Donnet, 1968). The increase of solutions
pH resulted in the increase of negatively charged sites
and the eciency of metal ions removal was, therefore,
higher (Chen et al., 2003). Chen and Wang (2002) emphasized that higher content of carboxylic functional groups
could signicantly improve adsorption of metal due to
the high anity between them.
As for lactones, they are weaker acids than free carboxyl
groups. The other acidic groups namely phenols and carbonyls are very weak acids. However, these last two groups
were not detected in the palm shell activated carbon used
in our experiments. Generally, the acidic groups on oxidized carbon surface produce cation exchange properties,
Table 1
Physico-chemical properties of Pacic palm shell activated carbon
This study

ACCs (Faur-Brasquet
et al., 2002)

PSAC

CS-1501

RS-1301

BET specic surface area (m g )

957.04

1680

1460

Acidic surface groups concentration

Carboxylic functions (meq g1)
Lactones (meq g1)
Phenolic functions (meq g1)
Carbonyl functions (meq g1)
Total number of sites
Surface site density (sites/nm2)
pHpzc
pKa1
pKa2

1.51
2.63
0
0
4.14
2.605
1.43
7.386
12.24

0.60
0.10
0.40
0
1.10

0.25
0.15
0.40
0
0.80

7.50
6.26
9.33

9.53
3.90
11.90

1

G. Issabayeva et al. / Bioresource Technology 97 (2006) 23502355

100
80
60

C, %

and carbons exhibit an anion exchange capacity due to the

presence of basic surface oxides when carbons are exposed
to the atmosphere. In addition, considerable exchange
capacities may take place despite the comparatively small
concentration of basic surface sites on the carbons surface
(Boehm, 1994).
The pHpzc corresponds to zero surface charge density,
i.e. to equivalent amounts of negative and positive charges
developed by proton equilibria. If no specic adsorption of
ions occurs the point of zero charge coincides with the isoelectric point; whereas specic adsorption of ions causes a
discrepancy between isoelectric and zero charge points.
Determination of these values provides information on
the specicity of adsorption (Mullet et al., 1999). Chen
et al. (1996) and Dastgheib and Rockstraw (2002) outlined
that when the pH of the solution was higher than pHpzc
it promoted higher adsorption rate of metal ions on the
surface. Supposedly, quite low value of pHpzc = 1.43 of
our palm shell carbon suggested higher uptake of metal
ions, especially at higher pH. The above parameters largely
determined the adsorption capacity of the adsorbent material, which was believed to be high for the palm shell activated carbon.

40
20
0
0

3.2.2. Lead with complexing agents

Fig. 2 shows the speciation proles of lead with malonic
acid. The formation of aqueous Pbmalonate started at pH
3.0, and accordingly, concentrations of Pb2+, PbNO3+ and
aqueous Pb(NO3)2 started depleting earlier. However, after
pH 6.3, the same species as for single lead prole were present on the speciation diagram. Speciation diagram of lead

10

12

14

Pb(NO3)2 (aq)

PbNO3+

Pb(OH)2 (aq)

Pb(OH)3-

Pb(OH)2 [s]

PbOH+

Fig. 1. Speciation of single lead.

100
80
60
40
20
0
0

8
pH

10

12

14

Pb2+

PbNO3+

Pb(NO3)2 (aq)

Pb-Malonate (aq)

PbOH+

Pb(OH)2 (aq)

Pb(OH)3-

Pb(OH)2 [s]

16

Fig. 2. Speciation of lead with malonic acid (C[Pb] = 50 mg/L).

with boric acid was identical to the speciation of single lead

(Fig. 3).
3.3. Adsorption results
The Langmuir isotherm given by Eq. (1) was used to
estimate the maximal adsorption capacity of PSAC to
remove lead ions:
y

a  Ce
;
1 b  Ce

where Ce is the equilibrium concentration, y is the amount

of metal adsorbed, a and b are the Langmuirs coecients.

100
80

C, %

3.2.1. Single lead

Fig. 1 shows the speciation proles of single lead species
at a total concentration of 10 ppm in Pb2+. The main species in the pH range 3.05.0 were Pb2+, PbNO3+ and aqueous Pb(NO3)2; their concentrations did not change until
pH 6.0. The formation of solid Pb(OH)2 started at pH
6.3 and that of other soluble hydroxides namely PbOH+,
aq Pb(OH)2, and PbOH3 occurred after pH 7.0.

Pb2+

3.2. Speciation of lead

It is important to outline how aqueous and solid phases
are generally considered and presented by VMinteq software. For example, in the case of Pb(OH)2 precipitation,
when a solid phase starts to form the concentration of
Pb2+ starts proportionally depleting from the aqueous
phase solution. In VMinteq, the concentrations of dissolved species are given in percentage relating to the concentration of available Pb2+. Thus, when precipitated
Pb(OH)2 reaches 99.9% at pH 10, and the diagram shows
presence of PbOH+ at 45%, it actually means that PbOH+
concentration is 0.45% relatively to the total Pb2+ concentration in system. As such, speciation diagrams for both
metals are given in concentrations relatively to a respective
phase, solid or aqueous.

pH

C, %

2352

60
40
20
0
0

10

12

pH
Pb2+

PbNO3+

Pb(NO3)2 (aq)

Pb(OH)2 (aq)

Pb(OH)3-

Pb(OH)2 [s]

PbOH+

Fig. 3. Speciation of lead with boric acid (C[Pb] = 50 mg/L).

14

G. Issabayeva et al. / Bioresource Technology 97 (2006) 23502355

2353

Table 2
Langmuir parameters for the adsorption of lead
pH

Variant

qm (mg/g)

qm (mmol/g)

SSE

R2

5
5
5

Pb
Pb + MA
Pb + BA

10.6
8.9
9.1

1.12
0.28
0.08

95.2
31.5
22.0

0.46
0.15
0.59

0.19
0.48
0.13

0.99
0.99
0.99

3
3
3

Pb
Pb + BA
Pb + MA

13.3
15.9
0.34

0.16
0.24
0.02

82.0
67.1
16.0

0.39
0.32
0.08

0.17
0.05
0.33

0.99
0.99
0.99

Table 2 shows adsorption data for single lead and lead

with complexing agents systems at both pH values. The
results indicated that pH 5.0 was more favorable for the
uptake of lead than pH 3.0 in all systems under investigation. Similar observations have been reported by many
researchers (Corapcioglu and Huang, 1987; Ravat et al.,
2000; Chen and Lin, 2001; Chen et al., 2002) and were
explained by the competition between metal ions and protons for the adsorption sites on the carbon surface, which is
lower at higher pH.
The presence of boric acid resulted in higher uptake of
lead compared to single lead at pH 5.0. Although the speciation diagram for lead with boric acid did not identify
any dierent species than in single lead speciation, the eect
of boric acid could be such that it inuenced chemical
course of lead ions in the solution promoting certain favorable conditions for accommodation of higher amount of
lead on the carbon surface. The same result was observed
by Rajakovic and Ristic (1996). They suggested that boric
acid in solution aected the optical orientation of the
organic molecules to form more complexes. However, it
was acknowledged that at the time no detailed understanding of such eect could be provided.
However, at pH 3.0 the uptake of lead in the system
with boric acid was lower relatively to single lead system.
Such relative decrease of lead uptake was probably associated with partial adsorption of boric acid on the carbon
surface decreasing the number of sites occupied by lead.

This was possible in view of the reported ndings of Rajakovic and Ristic (1996) who determined that 1.4 mg/g of
boric acid from potable water was adsorbed on the activated carbon. Rajakovic and Ristic (1996) also showed
that activated carbon had higher sorption anity towards
monomeric, univalent ions than towards polyvalent structures of boric acid that were present in aqueous solutions.
The activated carbon maintained its adsorptive functions
in the presence of boric acid and the principal ion
BOH
4 in borax solution did not demonstrate anity
towards complex formation (Rajakovic and Ristic, 1996).
Furthermore, the ineectiveness of boric acid on adsorption of lead at pH 3.0 could be associated with its weak
electrolytic properties and slow dissociation, especially in
the acidic aqueous solutions (Cotton and Wilkinson,
1966).
Malonic acid had a deteriorating aect on the adsorption of lead compared to the two previous systems. The
uptake of lead was signicantly lower: 31.5 and 16.0 mg
Pb2+/g AC at pH 5.0 and 3.0, respectively, compared to
95.2 and 82.0 mg Pb2+/g AC for single lead system. However, the same trend was observed with the eect of pH as
the amount of lead removed at pH 5.0 was higher than at
pH 3.0. The speciation diagram for lead with malonic acid
identied formation of leadmalonate (aq) complex in pH
range 310, with a peak concentration at pH 6.5. The formation of this complex could be responsible for the substantial decrease of lead adsorption on PSAC.

Table 3
Adsorption capacities (mg/g) of lead by various adsorbents
Adsorbent
Natural ferric oxide
Tea leaves
Clay
Groundnut husk
Sphagnum moss peat
Olive mill residue
Sago waste
ACC
Carex peat
Cocoa shells
Bone powder
Active carbon
Nile rose plant powder
Commercial carbon
Palm shell activated carbon

pH

Lead (II)

References

5.6
25.5
210
7.8
2
3 and
3 and
3 and
3 and
3 and

230.0
78.7
0.12
39.3
30.7
21.56
46.64
30.45
83%
6.2
29.5 and 55.3
32.7 and 41
19.7 and 27.4
9.8 and 27.3
82.0 and 95.2

Srivastava et al. (1988)

Tan and Kian (1988)
Srivastava et al. (1989)
Okieimen et al. (1991)
Ho et al. (1996)
Gharajbeh et al. (1998)
Quek et al. (1998)
Faur-Brasquet et al. (2002)
Ringqvist et al. (2002)
Meunier et al. (2003)
Abdel-Halim et al. (2003)
Abdel-Halim et al. (2003)
Abdel-Halim et al. (2003)
Abdel-Halim et al. (2003)
This study

5
5
5
5
5

G. Issabayeva et al. / Bioresource Technology 97 (2006) 23502355

In order to assess the performance of palm shell activated carbon as adsorbent for lead ions, a comparison with
other types of adsorbents was made (Table 3). All adsorbents showed lower lead uptake than PSAC, except the
natural mineral ferric oxide, which was characterized by
a capacity three times higher than PSAC. Such high uptake
for ferric oxide was expected since this solid was characterized by high number of surface hydroxide groups that
exhibited high anity for heavy metals. The capacities of
other carbonaceous materials of plant origins were considerably lower compared to the PSAC capacity. This could
be due to the smaller surface area that these adsorbents
possessed. Due to the lack of information on the surface
areas of most of these adsorbents, it was dicult to conrm
the eect of the surface area on the adsorption capacity.
Nevertheless, a rigorous comparison could be made with
ACC. As shown in Table 3, PSAC was characterized by
a capacity, which was more than a double of that of
ACC despite the higher surface area of the later. This result
indicated that the concentration of surface acidic groups
was more important in this adsorption process than the
overall surface area.

Table 4
Surface complexation constants values calculated for PSAC using DLM
Initial conc. Pb2+

Log K int
SOM

Initial conc. Pb2+ (mg/L)

Log K int
SOM

128.7
153.6
229.2
258.7
273.8
294.0

6.4
6.2
5.8
5.7
5.6
5.5

315.8
337.0
394.4
424.7
485.0
511.0
541.6

5.5
5.4
5.3
5.2
5.0
5.0
4.9

100

80

mod %

2354

60

40

20

0
0

3.4. Modeling on adsorption of lead

4.00E-02
exp

model

3.00E-02

[H+]

2.50E-02
2.00E-02
1.50E-02
1.00E-02
5.00E-03
0.00E+00
0

40

60

80

100

exp %

For modeling of experimental data on adsorption, a

diuse layer model was used. This model is amongst the
simplest surface complexation models and has four adjustable parameters. Details pertaining to this model can be
found elsewhere (Chen et al., 1996; Faur-Brasquet et al.,
2002; Borretzen and Salbu, 2003; Gustafsson, 2003).
Fig. 4 shows potentiometric curve of the PSAC titration.
These data were used to determine the intrinsic surface
acidity constants of the carbon using a tting procedure
in Fiteql 4.0 software (Herbelin and Westall, 1999). The
obtained constants values were used for calculations of
complex formation constants for every initial metal concentration (Table 4). The modeling results are presented
in percentage of metal adsorbed over a range of initial
concentrations at pH 3.0 and 5.0. Fig. 5 shows parity
graph (80% sectors) of the modeled and experimental
adsorption data. This model could predict fairly well the
percentage of lead adsorbed.

3.50E-02

20

10

pH

Fig. 4. Acidbase titration curves for Pacic palm shell activated carbon.

Fig. 5. Modeling results on adsorption of lead (80% parity). (s)pH 3;

(m)pH 5.

The estimated values of complexation constants (Table

4) for lead were relatively high, suggesting higher complexation anity between lead ions and palm shell carbon surface groups. Also, higher values of complexation constants
for lead were correlated with the high molecular weight of
the metal and its lower initial molar concentrations in the
solution leading to faster saturation of adsorption sites
(Faur-Brasquet et al., 2002).
4. Conclusion
Results on adsorption of lead on palm shell activated
carbon showed that this material exhibited high adsorption
capacity and could be successfully applied in the wastewater treatment technologies to remove heavy metals.
The adsorption capacity of lead was higher at pH 5.0 than
at pH 3.0, which was explained by the lower competition
between protons and lead ions at higher pH. Addition of
boric acid to the solution of lead improved total metal
uptake especially at pH 5.0; whereas malonic acid presence
resulted in the substantial decrease of metal uptake at both
pH due to formation of (aq) Pbmalonate complex. Data
on adsorption modeling using diuse layer model showed
good agreement between experimental and modeled
adsorption uptakes. It would be worth to note that palm
shell activated carbon used in this study did not undergo
any chemical or physical pre-treatment, which enhances
its scope for heavy metal removal application from industrial wastes.

G. Issabayeva et al. / Bioresource Technology 97 (2006) 23502355

Acknowledgements
We would like to thank the Ministry of Science, Technology and Innovation, Malaysia for the IRPA Research
Grant; the Institute for Postgraduate Studies and Research
(IPSP), University Malaya for nancing VotF 159/2003A
research project; and Pacic Activated Carbon Company,
Johor Baru, Malaysia for the generous provision of palm
shell activated carbon for our research.
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