Desalination 256 (2010) 16–21

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Desalination
j o u r n a l h o m e p a g e : w w w. e l s e v i e r. c o m / l o c a t e / d e s a l

Removal of lead(II) from aqueous solution using heartwood of Areca catechu powder
Paresh Chakravarty a,⁎, N. Sen Sarma b, H.P. Sarma c
a
Department of Chemistry, Birjhora Mahavidyalaya, Bongaigaon, Assam, India
b
Material Sciences Division, Polymer Section, IASST, Guwahati, Assam, India
c
Department of Environmental Science, Gauhati University, Guwahati, Assam, India

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

Article history: Removal of lead(II) from aqueous solution was studied using the powder of heartwood of Areca catechu as a
Received 29 October 2009 new biosorbent under batch method at room temperature. Various sorption parameters such as contact time,
Received in revised form 16 February 2010 initial concentration of lead(II) ion, effect of pH and amount of the biomass on the adsorption capacity of the
Accepted 17 February 2010
biosorbent were studied. The adsorbent was effective for the quantitative removal of lead(II) ions in acidic
Available online 12 March 2010
conditions and equilibrium has been achieved in 25 min. The equilibrium adsorption data were fitted to
Keywords:
Langmuir and Freundlich adsorption isotherm models and the model parameters were evaluated. The kinetic
Adsorbent study showed that the pseudo-second order rate equation better described the biosorption process. The FT-IR
Areca catechu powder spectra of the adsorbent before and after treatment with lead(II) solution indicated that hydroxyl, carboxyl,
Lead(II) ion amide and amine groups were major binding sites with the metal. This method is quite feasible, economic, time
Removal saving, and low cost.
Wastewater © 2010 Elsevier B.V. All rights reserved.

1. Introduction
Contamination of the environment by heavy metals is a growing
concern because of health risks on humans and animals [1,2]. Most of the
toxic metal pollutants are waste products of industrial and metallurgical
processes and in particular, the effluents from tanning industries.
According to the WHO, the metals of most immediate concern are Al, As,
Cd, Cr, Co, Cu, Fe, Pb, Mg, Hg, Ni, and Zn.
There are several techniques, which have been utilized to reduce
heavy metal ion content in effluents, namely lime stone precipitation,
ion exchange, adsorption on activated carbon, membrane processing
and electrolytic methods [1]. Most of these methods have been found to
be limited since they often involve high capital and operational cost and
may also be associated with the generation of secondary wastes. Of
these techniques, activated carbon adsorption appears to be particularly
competitive and an effective process for the removal of heavy metals at
trace level [3]. A good number of studies have been reported for metal
ion removal by using different bioadsorbents. In this regard, low cost
biosorbent such as neem-leaf powder [4], phaseolus vulgaris [5],
Canadian albicans [6], macro fungus [7], pine bark [8], ficus religiosa
leaves [9], green algae [10], citrus peel [11], bael leaves [12], moringa
oleifera bark [13] etc. have been utilized for the removal of lead and
other heavy metals from wastewater.
Lead was chosen for biosorption studies with regard to their wide
use in the industry and the potential pollution impact. Lead is released
⁎ Corresponding author. Tel.: +919435122322 (mobile).
E-mail address: pareshchakravarty@gmail.com (P. Chakravarty).
into the aqueous system from paper and pulp industries, lead smelter,
boat and ship fuels, battery manufacturers and ammunition industries.
Lead can contaminate the environment by anthropogenic sources as
well as natural geochemical processes. It can accumulate along the
food chain and is not amenable to biological degradation [14]. Lead
exposure causes weakness in fingers, wrists and ankles. The effects of
lead toxicity are very wide ranging and include impaired blood
synthesis, hypertension, severe stomach-ache, and brain and kidney
damage and even can cause miscarriage in pregnant women. The
consistent pattern of lower IQ values and other neuropsychological
deficits among the children exposed to higher levels of lead pollution
have been reported [15].
In the present study, the ability of the heartwood powder of Areca
catechu (betel-nut tree) (HPAC) to eliminate Pb(II) ion from synthetic
wastewater and the effect of various parameters such as contact time
of biosorbent and sorbent, pH of the metal solution, initial metal ion
concentration and different biomass amount have been investigated.
Equilibrium modeling was carried out using Langmuir [16] and
Freundlich [17] adsorption isotherm. The nature of the sorption
process has been evaluated with respect to its kinetic aspects.
2. Materials and methods
2.1. Preparation of the heartwood powder of A. catechu (HPAC)
A healthy and matured A. catechu (betel-nut tree) is collected from
Bakhrapara village of Bongaigaon district of Assam, India and the heart-
wood of the same is carefully separated. The heartwood of A. catechu,
which is soft and spongy, is cut into small pieces and washed with tap

0011-9164/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2010.02.029
 P. Chakravarty et al. / Desalination 256 (2010) 16–21
water and then with double distilled water to remove dust and other
impurities. The small cut pieces of heartwood of A. catechu are sun-dried
for seven days and dried again in an electric oven at 70 °C for 48 h. The
dried materials are grounded in a laboratory blender and made into fine
powder. The finely divided powder of the heartwood of A. catechu is
then shorted in desiccator and used for biosorption studies.
2.2. Metal solution
All chemicals and reagents used for experiments and analyses
were of analytical grade. Stock solution of 1000 mg/L of Pb(II) was
prepared from Pb (NO3)2 (E. Merck, Mumbai, India) in double distilled
water that contained few drops of 0.1 N HNO3 to prevent the
precipitation of Pb(II). The solution was diluted as required to obtain
the working solution. The initial pH of the working solution was
adjusted to 5.0 by an addition of the 0.1 N HNO3 or 0.1 N NaOH
solutions except for the experiment examining the effect of pH. Fresh
dilutions were used for each study.
2.3. Methods of adsorption studies
Batch adsorption experiments were carried out by shaking the flasks
at 120 rmp for a fixed period of time using a mechanical shaker.
Following a systematic process, the adsorption uptake capacity of Pb(II)
in batch system was studied in the present work. The data obtained in
batch mode studies was used to calculate the equilibrium metal
adsorptive quantity by using the following expression:
ðCo −Ce ÞV
qe =
m ion in a monolayer, the metal uptake by the sorbent surface will be
where qe is the amount of heavy metal ion adsorbed onto per unit
weight of the biomass in mg/g, V is the volume of solution treated in
liter, Co is the initial concentration of metal ion in mg/L, Ce is the
equilibrium metal ion concentration in mg/L and m is the biomass in g.
2.3.1. Effect of contact time
Batch biosorption experiments were carried out at different contact
times (5, 10, 15, 20, 25, 30 and 35 min) at an initial concentration of
20 mg/L of Pb(II) ion solution at pH 5.0, the HPAC dose concentration is
0.5 g in 100 ml of solution in 250 ml conical flask at room temperature
(29 °C ± 2 °C). The samples were then agitated in a mechanical shaker
at 120 rmp at a regular time interval and filtered through Whatman 42
filter paper and the filtrates were analyzed using flame atomic
absorption spectrometry (Model: Perkin Elmer 3110). Each determi-
nation is repeated three times and the results given were the average
values.
2.3.2. Effect of initial metal ion concentration
Equilibrium experiments were carried out by contacting 0.5 g of
HPAC with 100 ml of Pb(II) ion solution of different initial concentra-
tions (10 mg/L–70 mg/L) at pH values of 5.0 at room temperature. A
series of such conical flasks were shaken for 25 min at a speed of
120 rpm at room temperature (29 °C ± 2 °C). The samples were
filtered and the filtrates were analyzed as mentioned before.
2.3.3. Effect of biosorbent concentration
Batch adsorption tests were done at a different concentration of
HPAC from 0.1 g to 0.6 g at a 100 ml solution of 20 mg/L of Pb(II) ion at
pH 5.0, for a contact time of 25 min at room temperature (29 °C± 2 °C).
The samples were then agitated and filtered and the filtrates were
analyzed as mentioned before.
2.3.4. Effect of solution pH on biosorption
The effect of pH on the adsorption capacity of HPAC was
investigated using a 100 ml solution of 20 mg/L of Pb(II) ion for a
17
pH range of 2.0 to 7.0 at 29 °C. Experiments could not be performed at
higher pH value due to hydrolysis and precipitation of lead ions. Flasks
were agitated on a shaker for 25 min to ensure that the equilibrium
was reached. The mixtures were then filtered and the concentration of
metal in the filtrates was measured.
2.4. FT-IR measurements
FT-IR spectra for both free HACP and Pb(II) loaded HPAC were
obtained by KBr pellets methods operated on FT-IR spectrophotometer
(Brucker, Vector 22) to investigate the functional groups present in
the biomass and to look into possible Pb(II) binding sites.
3. Result and discussion
3.1. Effect of contact time
The effect of contact time on Pb(II) biosorption on HPAC was
studied and the results were shown in Fig. 1. From Fig. 1, it was found
that the adsorption quantity of Pb(II) ion on HPAC increases as the
contact time increased. The biosorption of lead onto HPAC was rapid
for the first 5 min (88%) and equilibrium was nearly reached after
25 min (97%). Hence, in the present study, 25 min was chosen as the
equilibrium time. Basically the removal rate of sorbate is rapid, but it
gradually decreases with time until it reaches equilibrium. The rate in
percent of metal removal is higher in the beginning due to the larger
surface area of the adsorbent being available for the adsorption of the
metals [18]. It is also relevant that, since active sorption sites in a
system have a fixed number and each active site can adsorb only one
rapid initially, slowing down as the competition for the decreasing
availability of active sites intensifies by the metal ions remaining in
the solution [19].
3.2. Effect of initial metal ion concentration
Biosorption experiments with HPAC were conducted for solutions
containing 10 mg/L to 70 mg/L Pb(II) ion. As seen in Fig. 2, at lower
concentrations of Pb(II) ion (10 mg/L–40 mg/L), biosorption was
completed in about 5 min, but at higher concentrations it took about
25 min. At lower concentrations, all metal ions present in the solution
would interact with binding sites and then facilitated about 99%
adsorption. At higher concentration, more Pb(II) ions are left
unabsorbed in the solution due to the saturation of binding sites.
This appears due to the increase in the number of ions competing for
available binding sites in the biomass [20].
Fig. 1. Effect of contact time on Pb(II) adsorption on the heartwood powder of Areca
catechu (HPAC), 100 ml single metal solution, pH = 5.0, initial metal ion concentration
(Co) = 20 mg/L, biosorbent amount = 0.5 g, and temperature = 29 °C.
18 P. Chakravarty et al. / Desalination 256 (2010) 16–21
Fig. 2. Effect of Pb(II) ion concentration on HPAC; initial metal ion concentration = 10 mg/L,
20 mg/L, 30 mg/L, 40 mg/L, 50 mg/L, 60 mg/L and 70 mg/L; 100 ml of single metal solution;
contact time=25 min; amount of HPAC= 0.5 g; temperature = 30 °C, and pH = 5.0.
3.3. Effect of biosorbent concentration
The influence of biosorbent concentration in equilibrium uptake
was shown in Fig. 3. It can be observed that the percentage removal of
Pb(II) ion increases with the increase in HPAC doses from 0.1 g to
0.5 g. There was a non-significant increase in the removal of
percentages of Pb(II) when the adsorbent dose increases beyond
0.5 g. A similarity in metal uptake with variation in biosorbent
concentration has been reported for lead biosorption from its
synthetic aqueous solutions by Spirulina maxima [21] and Cr {VI}
removal from industrial effluent using Saccharomyces Cerevisiae
immobilised in chitosan [22]. This suggests that after a certain dose
of biosorbent, the maximum adsorption is attained and hence the
amount of ions remains constant even with further addition of dose of
adsorbent. The increase in Pb(II) removal percentage with increase in
adsorbent dose is due to the greater availability of the exchangeable
sites or surface area at a higher concentration of the adsorbent.
3.4. Effect of solution pH
The pH of the solution is perhaps the most important parameter
for adsorption. To understand the adsorption mechanism, the
adsorption of Pb(II) as a function of pH was measured and the result
is shown in Fig. 4. Lead removal recorded its minimum values at pH
2.0. There was an increase in the biosorption capacity of the biomass
with an increase in pH from 2.0 to 5.0 and showed marginal
Fig. 3. Effect of biosorbent concentration on Pb(II) on HPAC; 100 ml of single metal
solution; contact time = 25 min, pH = 5.0; initial metal ion concentration = 20 mg/L,
and temperature = 30 °C.
Fig. 4. Effect of pH on Pb(II) adsorption on HPAC; 100 ml of single metal solution; contact
time = 25 min, pH= 2.0, 3.0, 4.0, 5.0, 6.0 and 7.0; initial metal ion concentration= 20 mg/L,
amount of HACP= 0.5 g and temperature = 31 °C.
downward trend from pH 6.0. In lower pH values, occupation of the
negative sites of the adsorbent by H+ and H3O+ ions leads to
reduction of vacancies for metal ion and consequently causes a
decrease in metal ion biosorption [23]. As the pH was raised, the
ability of the metal ions for competition with H+ and H3O+ ions was
also increased. Although the sorption of metal ions raised by growing
pH, further increment of pH caused declining in adsorption due to the
precipitation of metal hydroxides.
3.5. FT-IR analysis
Numerous chemical functional groups such as carbonyl, hydroxyl,
amine, amide, etc. have been identified as potential adsorption sites to
be responsible for binding metallic ions to the biomass. The FT-IR
spectroscopy is an important analytical technique, which detects the
vibration characteristics of chemical functional groups present on
adsorbent surfaces. The FT-IR spectra of both the adsorbents (fresh as
well as lead loaded) are shown in Fig. 5.
FT-IR spectra of fresh HPAC show peaks between the regions 3500
and 3200 cm−1 which represent the overlapping peaks of stretching
vibrations of O–H and N–H groups. The strong absorption peak
at 2919 cm−1 could be assigned to –CH stretching vibrations of –CH3
and –CH2 functional groups. The distinct peak observed between
1749 cm−1 and 1627 cm−1 characterizes carbonyl groups stretching from
aldehyde and ketones. The adsorption peaks at 1627–1421 cm−1
correspond to the primary and secondary amide bands, respectively.
1421–1392 cm−1 was the deformation stretching of C–H, –CH3 and –CH2
Fig. 5. FT-IR spectra of fresh-dried (A) HPAC and (B) Pb(II) loaded HPAC.
 P. Chakravarty et al. / Desalination 256 (2010) 16–21
functional groups. The strong band within 1100–1000 cm−1 is due to
the C–O group, which are characteristic peaks of polysaccharides.
Changes in intensity and shift in position of the peaks could be
observed in FT-IR spectrum after Pb(II) adsorption in HPAC. The
first change was the enhancement of the intensity at the regions
3500–3200 cm−1, indicating an increase of the free hydroxyl group on
the biomass. The shifting of peak at 1749 to 1737 cm−1 and 1627 to
1629 cm−1 indicates the involvement of C O of carboxyl group, N–H of
amine and C–O of amides in the adsorption process. The minor shift of
the peak from 1033 to 1031 cm−1 also suggests the involvement of
the C–O group in binding Pb(II). It is clear from the FT-IR analysis that
the possible mechanism of adsorption of Pb(II) on the biomass HPAC
may be due to physical adsorption, ion exchange, surface precipita-
tion, complexation with functional groups and chemical reactions
with surface sites [10,24].
3.6. SEM and EDX analysis
Scanning electron microscopy (LEO, Model 1430VP) along with
energy dispersive X-ray (EDX) analysis has been used by many
researchers for the characterization of the adsorbent as well as the
elucidation of the probable mechanism of biosorption. SEM micro-
graphs and EDX spectra obtained from fresh HPAC and lead loaded
HPAC are shown in Fig. 6. SEM micrographs of fresh HPAC (Fig. 6a)
reveal the nature of the biomass which is dark, rough, heterogeneous,
very few pores and lots of ups and down, and thus makes possible for
the adsorption of Pb(II) ions in different parts of the adsorbent. Fig. 6b
represents the micrograph of Pb(II) loaded HPAC. The micrograph
clearly shows the presence of shiny particles over the surface of Pb(II)
loaded biosorbent which are absent in the fresh biosorbent [25,26].
EDX analysis provides the elemental information for the fresh as well
as the Pb(II) loaded biosorbent. Fig. 6c indicates the presence of C, O,
N, Cr, Ca, and S in the fresh biosorbent. EDX spectra presented in
Fig. 6d.revealed the additional Pb signal, which confirms the binding
of the metal ion to the surface of the biomass.
Fig. 6. SEM micrographs of (a) fresh HPAC, (b) Pb(II) loaded HPAC; EDX spectra of (c) fresh HPAC and (d) Pb(II) loaded HPAC.
19
3.7. Adsorption kinetic studies
Adsorption kinetics, which describes the solute adsorption rate, is
an important characteristic in evaluating the efficiency of the
adsorption. In order to clarify the biosorption kinetics of Pb(II) ions
onto HPAC, the kinetic models, that are, Lagergren's pseudo-first order
[27] and pseudo-second order [28] models were applied to the
experimental data. The linearised form of the pseudo-first order rate
equation by Lagergren is given as;
K1 ⋅t
Logðqe −qt Þ = log qe −
2:303
where qe and qt are the amounts of metal ion sorbed (mg/g) at
equilibrium and at time t, respectively. K1 is the Lagergren rate
constant of the biosorbent (1/min). A plot of log (qe − qt) versus t
gives the result shown in Fig. 7. The values of K1 and qe, calculated
from the slope and intercept are presented in Table 1.
The pseudo-second order kinetic model of McKay and Ho [28] can
be expressed as;
t 1 1
= + t
qt K2 q2e qe
where the equilibrium biosorption capacity, qe and the pseudo-
second order rate constant K2 (g/mg min) were determined exper-
imentally from the slope and intercept of plot t / qt versus t (Fig. 7).
Calculated correlations are closer to unity for pseudo-second order
kinetic model; therefore, the biosorption kinetics could well be
approximated more favourably by the second-order kinetics model
rather than the pseudo-first order kinetics for Pb(II). The K2 and qe
values for the pseudo-second order kinetic, calculated from Fig. 8 are
listed in Table 1. By comparing the constants of the two kinetic
models, the pseudo-second order kinetic model seems to be best
fitted for the experiment.
20 P. Chakravarty et al. / Desalination 256 (2010) 16–21
Fig. 7. Pseudo-first order kinetic plot for the biosorption of Pb(II) by HPAC at 31 °C and
pH 5.0.
3.8. Biosorption equilibria studies
An adsorption isotherm is a graphical representation showing the
relationship between the amounts adsorbed by a unit weight of
adsorbent and the amount of adsorbate remaining in a test medium at
equilibrium. The lead(II) uptake capacity of HPAC was evaluated using
the Langmuir [16] and Freundlich [17] adsorption isotherms. The
Langmuir equation, which is valid for monolayer sorption onto a surface
with a finite number of identical sites, which are homogeneously
distributed over the adsorbent surface, is given by the equation:
qmax bCeq
qe =
1 + bCeq
where qe is the amount of metal ion bound to per gram of the biomass
at equilibrium and Ce is the residual (equilibrium) metal ion
concentration left in the solution after binding, respectively. qmax is
the maximum amount of metal ion per unit weight of sorbent to form a
complete monolayer on the surface and b is the constant related to the
affinity of the binding sites. qmax and b can be determined from Ce / qe
versus the Ce plot which gives a straight line of slope 1/qmax and
intercept 1/b∙qmax [29].
On the other hand, the Freundlich equation is an empirical
equation based on adsorption on a heterogeneous surface is given
by equation:
1
qe ¼Kf Ce n
where Ce is the equilibrium concentration (mg/L), qe is the amount of
metal ion bound to per gram of the biomass at equilibrium (mg/L) and
Kf and n are the Freundlich constants related to the sorption capacity
and sorption intensity of the sorbent, respectively. The equation can
be linearised in logarithmic form and Freundlich constants can be
evaluated.
The Langmuir and Freundlich equations were used to describe
the data derived from the adsorption of Pb(II) by the biosorbent over
the entire concentration range studied (10 mg/L to 70 mg/L). The linear
Table 1
Kinetic model parameters for the biosorption of Cd (II) by the heartwood powder of
Areca catechu (HPAC).
Pseudo-first order Pseudo-second order
parameters parameters
qe (mg/g) K1 (1/min) R2 qe (mg/g) K2 (g/mg min) R2
3.85 0.143 0.9892 20.2 0.0572 0.9998 19.5
Fig. 8. Pseudo-second order kinetic plot for the biosorption of Pb(II) by HPAC at 31 °C
and pH 5.0.
plot of the Langmuir and Freundlich isotherm models for sorption of Pb
(II) on HPAC are presented in Figs. 9 and 10. The plot of Ce / qe versus Ce
(Fig. 9) showed that the experimental data fitted reasonably well to the
linearised equation of the Langmuir isotherm over the whole Pb(II)
concentration range studied. The correlation coefficient was 0.9993.
qmax and b were evaluated from the slope and intercept of the plot and
were found to be 11.7233 mg/g and 1.3023 L/mg respectively.
The essential characteristics of Langmuir can be explained in terms
of dimensionless constant separation factor (RL), defined by:
1
RL =
1 + bCo
where b is the Langmuir constant and Co is the initial concentration of
metal ion. The value of RL indicated the type of Langmuir isotherm to
be irreversible (RL = 0), favourable (0 b RL b 1), linear (RL = 1) or
unfavourable (RL N 1). The RL was found to be 0.0713 to 0.0108 for
concentrations of 10–70 mg/L Pb(II).
Linear plots of log qe versus log Ce showed that the Freundlich
isotherm was also representative for the Pb(II) by the biosorbent
tested. The correlation coefficient was 0.9728. Kf and n were calculated
from the slopes of the Freundlich plots (Fig. 10) and were found to be
0.1816 and 1.5562 respectively. The magnitude of Kf and n shows easy
separation of heavy metal ion from wastewater and high adsorption
capacity. The value of n, which is related to the distribution of bonded
ions on the sorbent surface, represents beneficial adsorption if it is
between 1 and 10 [30]. The n value for the biosorbent used found to be
greater than 1, indicating that adsorption of Pb(II) is favourable.
Experimental
value
qe (mg/g)
Fig. 9. Langmuir isotherm plot for Pb(II) adsorption onto HPAC.
 P. Chakravarty et al. / Desalination 256 (2010) 16–21
Fig. 10. Freundlich plot for Pb(II) adsorption onto HPAC.
Table 2
Isotherm parameters for Pb(II) adsorption on the heartwood of Areca catechu powder
(HACP).
Langmuir isotherm Freundlich isotherm
b (L/mg) qmax (mg/g) R2 Kf n R2
1.3023 11.7233 0.9993 0.1816 1.5562 0.9728
Table 2 gives the isotherm parameters for both Langmuir and
Freundlich isotherms. From linear correlation coefficients of the adsorp-
tion isotherm, it is noted that the Langmuir isotherm model exhibits a
better fit to the sorption data of Pb(II) than the Freundlich isotherm
model. This phenomenon suggests that monolayer sorption takes place on
the surface of the HPAC.
4. Conclusion
In this study the ability of the biomass of the heartwood powder of
A. catechu (HPAC) to remove the synthetic Pb(II) solution has been
demonstrated. In this batch mode of studies, the adsorption was
dependent on contact time, pH, initial metal ion concentration, and
biosorbent dosage. The biosorbent was successful in removing Pb(II)
with 97% sorption efficiency from the aqueous solution containing
20 mg/l Pb(II). The biosorption was rapid and equilibrium was
achieved within 25 min. It was also observed that the adsorption
was pH dependent and the maximum adsorption of 97% occurred at
pH 5.0. The results of the study revealed that the removal of Pb(II) from
aqueous solutions by using HPAC as an adsorbent seems to follow the
pseudo-second order kinetic model and the Langmuir isotherm better
than the Lagergren's pseudo-first order kinetic model and Freundlich
isotherm, respectively. FT-IR and SEM characterization of the biosor-
bent have shown a clear difference in the fresh and Pb(II) loaded
biosorbent. Based on all results, it can be concluded that since the
biosorbent, HPAC, is an easily available and low cost adsorbent and has
a considerable high biosorption capacity, it may be treated as an
alternative biosorbent for treatment of wastewater containing Pb(II)
ions.
Acknowledgement
The authors are thankful to the Regional Sophisticated Instrumen-
tation Centre (RSIC), Shillong, India, for providing instrumental help
during the research work.
21
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