Ind. Eng. Chem. Res.

2003, 42, 6619-6624 6619

SEPARATIONS

Removal of Zinc from Aqueous Solutions Using Bagasse Fly Ash -

a Low Cost Adsorbent
Vinod K. Gupta* and Saurabh Sharma
Department of Chemistry, Indian Institute of Technology, Roorkee, Roorkee 247 667 (U.A.) India

Bagasse fly ash, a sugar industry waste, has been converted into an inexpensive and efficient
adsorbent. The product obtained has been characterized and utilized for the removal of zinc
from aqueous solutions over a wide range of initial metal ion concentration (3.06 × 10-4 to 3.06
× 10-3 M), contact time (24 h), adsorbent dose (5-20 g L-1), and pH (1.0-6.0). The removal of
Zn2+ is 100% at low concentrations, whereas it is 60-65% at higher concentrations at an optimum
pH of 4.0, using 10 g L-1 of adsorbent in 6-8 h of equilibration time. The uptake decreases with
a rise in temperature indicating the process to be exothermic in nature. Kinetic studies have
been performed to understand the mechanism of adsorption. The removal takes place through
film diffusion mechanism at lower concentrations (e1.84 × 10-3 M) and by particle diffusion at
higher concentrations (g 3.06 × 10-3 M).

Introduction i.e., the disposal of these wastes and their usage as a

Environmental pollution by toxic metals is well
recognized and can be detrimental to human health and
the environment. Metals can be distinguished from
other toxic pollutants, because these are nonbiodegrad-
able, may undergo transformations, and can have a
large environmental, public health, and economic im-
pact.1 This has led to more stringent legislation and has
prompted industry to seek more effective methods of
pollution control as the permissible limits are reduced.2
Zinc is a toxic element that can be found in natural
water, as well as in various industrial effluents.3 The
average human body contains about 2 g of zinc, which
is essential for the normal activity of DNA polymeriza-
tion and for protein synthesis. However, the inhalation
of zinc fumes may produce “Zinc Fever”, which is
characterized by chills and fevers. Edema of the lungs
from fumes of zinc chloride (ZnCl2 smoke) is sometimes
fatal. Soluble and astringent acid salts, such as ZnSO4
in large doses (about 10 g), have caused internal organ
damage and death. Zinc has a secondary drinking water
standard of 5.0 mg L-1 principally because of its bitter
metallic taste.3
Among the methods examined for zinc removal from
water, adsorption on activated carbon has been shown
to be very efficient.4,5 But the use of commercially
available activated carbon is limited, especially in
developing countries, because of its high cost and
difficulties in its regeneration.6 Accordingly, current
research is focused on the development of inexpensive
materials having high affinity, selectivity, and capacity
toward metals. The potential of various agricultural and
industrial waste materials has received the most atten-
tion for this purpose, which results in 2-fold benefits,
* To whom correspondence should be addressed. Tel.: 0091-
1332-285801. Fax: 0091-1332-273560. E-mail: vinodfcy@
iitr.ernet.in.
10.1021/ie0303146 CCC: $25.00 © 2003 American Chemical Society
Published on Web 11/12/2003
low cost adsorbents for the treatment of wastewater.
Contributions in this regard have been made by many
researchers who have utilized a number of materials
such as fly ash,7 peat,8 bentonite,9 lignin,10 charcoal,11
straw,12 blast furnace slag,13,14 biomass,15,16 sludges,17-19
red mud,20,21 and so forth.
The sugar industry is one of the most important agro-
based industries in India. Bagasse fly ash, a waste
material of sugar industries, causes a disposal problem.
Currently this fly ash is being used as filler in building
materials, but to date no other proper application of this
waste has been found. Recently, in our laboratory,
bagasse fly ash has been converted into an effective
adsorbent and used for the removal of toxic sub-
stances.22,23 In continuation, the aim of the present
research is to utilize the bagasse fly ash for the removal
of zinc from aqueous solutions and the results are
discussed in this communication.
Materials and Methods
All the reagents used were of A. R. grade. Stock
solution of zinc (1 × 10-2 M) was prepared by dissolving
Zn(NO3)2 in doubly distilled water.
Equipment. Atomic absorption spectra were re-
corded using an atomic absorption/emission spectropho-
tometer (Perkin-Elmer model 3100) using light source
Hollow Cathode; lamp current, 15.00 mA; wavelength,
213.9 nm; slit width, 0.7 nm; sensitivity, 1.0 mg L-1.
X-ray measurements were done by a Phillips X-ray
diffractometer employing nickel filtered Cu KR radia-
tions. The surface area of the sample was measured by
a surface area analyzer (model QS-7; Quantasorb sur-
face area analyzer). pH measurements were made using
a pH meter (model CT No. CL 46; Toshniwal, India).
Scanning electron microscopy (SEM) was performed
using a Phillips SEM 501 electron microscope. The
6620 Ind. Eng. Chem. Res., Vol. 42, No. 25, 2003
Figure 1. X-ray diffraction pattern of bagasse fly ash.
chemical composition of bagasse fly ash was determined
by using a quantitative method of chemical analysis.24
The density of the adsorbent was determined by use of
specific gravity bottles.
Material Development. Bagasse fly ash, a solid
waste, was obtained from a sugar industry establish-
ment at Bijnor (U. P.) India. This material in its
untreated form showed poor adsorption properties.
Therefore, this material was first treated with hydrogen
peroxide 30% w/v (100 volume) at 60 °C for 24 h, till
the evolution of bubbles stopped. The pretreatment with
hydrogen peroxide perhaps removes heterogeneously
distributed organic matter from the bagasse fly ash.
Preliminary adsorption studies revealed that treating
the waste material with hydrogen peroxide (30% w/v)
imparts maximum adsorption characteristics, and, there-
fore, all investigations were carried out on samples after
providing this treatment. The resulting product was
then washed with distilled water, dried at 100 °C for
24 h, and sieved to desired particle sizes such as 100-
150, 150-200, and 200-250 BSS mesh. The finished
product exhibited the best adsorption capacity and high
surface area. The product obtained at temperatures
higher than 100 °C exhibits poor adsorption capacity,
probably due to collapse of surface functional groups on
adsorbent. Finally, the product was stored in vacuum
desiccators until used.
Adsorption Studies. Adsorption studies were car-
ried out in a routine manner by batch technique.23
Isotherms were run with zinc solutions of varying
concentration (3.06 × 10-4 to 3.06 × 10-3 M), main-
tained at the desired pH and temperature. Stoppered
glass tubes containing metal ion solutions (10 mL) and
known amounts of bagasse fly ash (0.1 g; particle size
150-200 mesh) were stirred intermittently for a maxi-
mum period of 24 h. The contact time and other
conditions were selected on the basis of preliminary
studies that showed that the equilibrium was attained
in 6-8 h, and beyond this time the adsorption of zinc
ions on the adsorbent material remained almost con-
stant. Equilibration for longer times, that is between 8
and 24 h, gave practically the same uptake. After this
period the solutions were separated from the adsorbent
(centrifuged at 4000 rpm for 15 min) and immediately
analyzed to determine the uptake of zinc by the adsor-
bent. Adsorption studies were carried out at 30, 40, and
50 °C to establish the effect of temperature. The effect
of pH was determined by studying the adsorption at a
fixed concentration over a pH range of 1.0-6.0. pH
adjustment was made by dilute NaOH and dilute HNO3.
The pH was monitored at the beginning and at the end
of the run and no noticeable change in pH was observed.
Kinetic Studies. The batch technique was selected
because of its simplicity and reliability. A number of 50-
mL stoppered glass tubes containing 10 mL of solution
of metal ion of known concentration (1.84 × 10-3 M)
were placed in a thermostat cum shaking assembly. At
the desired temperature, 0.1 g of bagasse fly ash was
added into each tube and the solutions were agitated
intermittently. At predecided intervals of time (30 min
for the first two tubes and 60 min for all subsequent
tubes) the test solutions in the specified tubes were
centrifuged at 4000 rpm for 15 min and separated from
the adsorbent material. The supernatant was analyzed
for aqueous metal. The kinetic studies were also per-
formed at different adsorbate (1.22 × 10-3 to 3.06 × 10-3
M) and adsorbent (5 g L-1 to 20 g L-1) concentrations.
Results and Discussion
Characterization of the Adsorbent Material. The
adsorbent developed from bagasse fly ash was found to
be of “L” type in nature as classified earlier,23 i.e., it
lowers the pH when kept in deionized water. It is quite
stable in water, salt solutions, acid, and bases. Chemical
composition of the bagasse fly ash as determined by
chemical analysis24 is SiO2, 61.44; Al2O3, 14.50; CaO,
2.82; Fe2O3, 4.86; MgO, 0.71, and loss on ignition, 17.12
wt %. It is necessary to mention that no leaching
measurements were done in this work to estimate
contamination of solution by solubilized oxides from
bagasse fly ash. Leaching studies are out of the scope
of the present paper and are now a part of our ongoing
and future research. The X-ray diffraction pattern
(Figure 1) of the product provided d spacing values
which reflect the presence of different minerals, such
as goethite, mullite, hematite, kaolinite, γ-alumina, and
R-quartz, indicating high chemical stability of the ba-
gasse fly ash.25 Bands observed at 1172, 1157, and 680
cm-1 in the IR spectrum (figure not shown) of bagasse
fly ash were attributed to Si-O stretching vibrations,
a characteristic of quartz.26 The adsorption bands at
3696 and 3670 cm-1 indicated the presence of kaolinite.
A very weak band at 358 cm-1 was due to the presence
of hematite. A strong band at 470 cm-1 suggested the
presence of calcium silicate. The surface area of the

Figure 2. SEM photographs of bagasse fly ash at different
magnifications: (a) 1 × 5000; (b) 1 × 2500; and (c) 1 × 121.
adsorbent as calculated by BET method was found to
be 470 m2 g-1. The surface area was also worked out
theoretically, by methylene blue dye adsorption, taking
methylene blue dye molecule area as 197 Å2 and found
to be 440 m2 g-1. This value is slightly less than that
determined by N2 gas adsorption, and indicates that
some pores of bagasse fly ash are not accessible to
methylene blue. Scanning electron microscopic (SEM)
photographs of bagasse fly ash (Figure 2 (a-c)) clearly
reveal the surface texture and porosity of the sample.
The material was so porous that it could be crushed
easily by hand. The point of zero charge pHzpc (pH of
the suspension at which surface charge density σ ) zero)
and cation exchange capacity were determined by using
potentiometric titration method.27,28 The characteristics
Ind. Eng. Chem. Res., Vol. 42, No. 25, 2003 6621
Figure 3. Effect of pH on the adsorption of Zn2+ on bagasse fly
ash.
Figure 4. Effect of temperature on the adsorption of Zn2+ on
bagasse fly ash.
of the adsorbent are pHzpc, 3.8; density, 1.02 g cm3;
porosity, 0.36 (fraction); and ion exchange capacity, 1.43
meq g-1.
Adsorption Studies. The effect of pH on the uptake
of zinc (Figure 3) clearly indicates that the percentage
adsorption increases with pH to attain maximum at pH
4.0, and thereafter it decreases with any further in-
crease in pH. The increase in the removal could be
related to the surface charges that are strongly depend-
ent on the pH of the solution. The ZPC of the adsorbent
(pHzpc) is 3.8. Thus, below a pH of 3.8 the surface will
have high positive charge density and under these
conditions the uptake of zinc ions would be quite low
due to electrostatic repulsion. With increasing pH, i.e.,
beyond ZPC, the negative charge density on the surface
of adsorbent increases, thereby resulting in a sudden
enhancement in metal adsorption. A similar behavior
has been reported by Sen and De29 for Hg (II) and Gupta
et al.23 for lead adsorption on fly ash and bagasse fly
ash, respectively.
All the adsorption studies were carried out at a pH
of 4.0. The adsorption isotherms (Figure 4) are regular,
positive, and concave to the concentration axis. The
uptake is almost 100% at low concentrations (e 6.12 ×
10-4 M), and the adsorption decreases with concentra-
tion at 1.84 × 10-3 M and ultimately becomes constant.
This indicates the efficiency of the adsorbent for the
removal of zinc from wastewater in a wide range of
concentrations. Further, it is observed that the adsorp-
tion decreased with increase in temperature indicating
that the process is exothermic in nature. The adsorption
6622 Ind. Eng. Chem. Res., Vol. 42, No. 25, 2003
Table 1. Freundlich, Langmuir, and Thermodynamic Parameters for Zn2+ Removal by Bagasse Fly Ash
Freundlich constant Langmuir constant
n KF × 105 Q° × 104(mol g-1) b× 10-2(L
temp. ((0.02) ((0.005) ((0.01) ((0.02)
30 °C 0.36 3.10 2.02 9.45
40 °C 0.44 1.23 1.97 2.19
50 °C 0.46 0.132 1.85 1.41
data fitted well to Freundlich and Langmuir adsorption
isotherms, and the values of Freundlich and Langmuir
constants as calculated from these isotherms are listed
in Table 1. The adsorption capacity KF decreases as the
temperature increases. The slope 1/n, which reflects the
intensity of adsorption, presents the same trend. The
value of Q° (i.e., maximum uptake) decreases with
increase in temperature, thereby indicating exothermic
nature of the process. The adsorption capacity of ba-
gasse fly ash for zinc at pH 4.0 and 30 °C was found to
be 13.21 mg g-1. The adsorption capacity obtained for
bagasse fly ash is found to be comparable to, and in
some cases better than, the other adsorbents and
activated carbons as reported by Vishwanadham et al.3
for chitin (1.183 mg g-1); Weng and Huang7 for fly ash
(0.27-4.64 mg g-1), Nuchar-SN carbon (66 mg g-1), and
Filtrasorb-400 carbon (4.0 mg g-1); Gosset et al.8 for peat
(11.2 mg g-1); Larsen and Schierup for activated carbon
(6.2 mg g-1) and straw (5.3 mg g-1); Lopez et al.20 and
Gupta et al.13 for red mud (12.59 mg g-1) and blast
furnace slag (37.98 mg g-1), respectively.
The dimensionless factor RL as calculated from RL )
1/1+bCo was found to be 0.37. This indicates a highly
favorable adsorption (RL , 1).30 The thermodynamic
parameters obtained for this system using equations as
described earlier14 are also given in Table 1. The
negative free energy values indicate the feasibility of
the process and its spontaneous nature without any
induction period. The negative value of enthalpy change
(∆H°) for the processes further confirms the exothermic
nature of the process. Negative entropy of adsorption
(∆S°) reflects the affinity of the adsorbent material
toward zinc.
Kinetic Studies. Preliminary studies on the rate of
removal of Zn2+ by bagasse fly ash (at optimum pH and
adsorbent concentration) indicated the process to be
quite rapid. Nearly 50 to 60% of the adsorption capacity
was attained within the first hour of contact. The initial
rapid adsorption gives way to a very slow approach to
equilibrium, and saturation is reached in 6-8 h (Figure
5). It is also evident from Figure 5 that at low concen-
tration (1.22 × 10-3 M), 96.72% zinc is removed,
whereas 92.93% removal was ascertained with the
concentration of 1.84 × 10-3 M using 10 g L-1 of the
adsorbent dose in 6-8 h. At higher concentration (3.06
× 10-3 M) nearly 62.75% of zinc is removed from the
solution under identical conditions of adsorbent dose
and contact time. It was also found that at fixed
concentration the rate of removal of zinc increases with
an increase in the amount of bagasse fly ash. There was
a significant increase in the adsorption when the
adsorbent amount was increased from 5 g L-1 to 10 g
L-1. Any additional amount of bagasse fly ash did not
cause any significant change. Thus, 10 g L-1 of bagasse
fly ash has been used in all subsequent studies.
The above observations can be explained on the basis
of the following three consecutive steps, which may be
involved in the adsorption of an organic/inorganic spe-
cies by a porous adsorbent: (a) transport of the adsor-
thermodynamic parameters
mol-1) -∆G° (kJ mol-1) -∆H° (kJ mol-1) -∆S° (J mol-1 K-1)
((0.05) ((0.05) mean ((0.1) mean
17.27 76.83 197.95
14.03
13.30
Figure 5. Effect of adsorbate concentration on the rate of uptake
of Zn2+ on bagasse fly ash.
bate to the external surface of the adsorbent (film
diffusion); (b) transport of the adsorbate within the
pores of the adsorbent except for a small amount of
adsorption that occurs on the external surface (particle
diffusion); and (c) adsorption of the adsorbate on the
exterior surface of the adsorbent.
It is generally accepted that process (a) is very rapid
and does not represent the rate-determining step in the
uptake of adsorbate.23 For the remaining two steps in
the overall transport, three distinct cases may occur:
case I, external transport > internal transport; case II,
external transport < internal transport; and case III,
external transport ≈ internal transport.
In cases I and II, the transport of adsorbate to the
adsorbent is quite rapid and is governed by film diffu-
sion, whereas in case III, the transport of ions to the
adsorbent surface does not occur at a significant rate,
thereby leading to the formation of a liquid film with a
concentration gradient surrounding the sorbent par-
ticles.
Usually, external transport is the rate-limiting step
in systems which have poor mixing, dilute concentration
of adsorbate, small particle size, etc. In contrast, the
intraparticle transport step (case III) governs the overall
transfer for those systems having high concentration of
adsorbate, good mixing, larger particle size, etc. Hence
the low removal of zinc at higher concentration at fixed
adsorbent concentration reflects the intraparticle dif-
fusion, whereas high removal of zinc at low concentra-
tion might be due to the rapid external transport
mechanism to be the rate controlling step in the overall
removal of zinc at varying concentration range.
Adsorption Dynamics. Lagergren’s rate equation
as cited by Ho and Mckay31 was employed for studying
the rate constant for the systems. The plot between log-
(qe - q) and t was found to be linear, which shows the
first-order nature of the processes. The value of the rate
constant, Kad, for the system was 8.73 × 10-3 min-1.

Figure 6. McKay plots of Zn2+ on bagasse fly ash.
Mckay and co-workers32 model (eq 1) has been em-
ployed for the determination of the surface mass-
transfer coefficient βL.
ln [
Ct
-
1
Co 1 + mk ]
) ln
mk
1 + mk
-
1 + mk
mk
βL Ss t (1)
The straight line plot between ln [Ct/Co - 1/(1 + mk)]
and t proved the validity of the above model in the
present study. The value of βL for the system as
determined from the plot was 2.41 × 10-7 cm s-1.
To know the rate controlling step of the process,
McKay plots (Figure 6) at different adsorbate concen-
trations have been drawn. The plots between log(1 -F)
and t, where F is the fractional attainment of equilib-
rium at time t and is obtained by F ) Qt/Q∞ where Qt is
amount of uptake at time t and Q∞ is maximum
equilibrium uptake for Zn2+ at lower concentrations (e
1.84 × 10-3 M) were found to be linear indicating a
purely film diffusion process. However, nonlinear plot
at g 3.06 × 10-3 M concentration supports the assump-
tion that particle diffusion becomes the rate-limiting
step at this concentration. Thus, it is evident that the
rate of adsorption of zinc is limited by external transport
at low concentrations, whereas at concentrations higher
than 3.06 × 10-3 M the intraparticle diffusion mecha-
nism is of greater importance in determining the overall
rate of removal.
Cost Estimation. In India, the cheapest variety of
commercially available carbon costs (U.S. dollars) ap-
proximately $285 ton-1. Waste baggase fly ash is
available for $2 ton-1, and considering the cost of
transport, chemicals, electrical energy, etc., used in the
process, the finished product would cost approximately
$15 ton-1. Hence, the developed adsorbent would be a
good replacement for commercially available carbon
based on its comparatively low cost and good efficiency.
Conclusions
Bagasse fly ash, a waste residue generated in a
substantial amount in the sugar refining industry, was
converted into a suitable adsorbent. Bagasse fly ash
exhibits promising adsorption characteristics for the
removal of zinc and can be used for the treatment of
metal bearing wastewater. The material under consid-
eration is not only economical, but is a waste product.
Hence, its use as an adsorbent, would on one hand solve
Ind. Eng. Chem. Res., Vol. 42, No. 25, 2003 6623
the problem of its disposal and on other hand provide
an effective adsorbent for the treatment of metal-
bearing wastewaters.
Acknowledgment
We are very thankful to the Council of Scientific and
Industrial Research (CSIR), New Delhi, India for award-
ing a Research Associateship to undertake this work.
Nomenclature
BSS)British Standard Sieve
Ct)concentration of adsorbate at time t (mg g-1)
C0)initial concentration of adsorbate (mg g-1)
F)fractional attainment of equilibrium
∆G0)Gibbs free energy (kJ mol-1)
∆H0)enthalpy change of the process (kJ mol-1)
KF)Freundlich constant of solute (mol g-1)
Kad)Rate constant (min-1)
Q∞)amount of adsorbate adsorbed per gram of adsorbent
(mol g-1) at equilibrium
Qt)amount of adsorbate adsorbed per gram of adsorbent
(mol g-1) at time t
Q0)Langmuir monolayer capacity (mol g-1)
RL)separation factor (dimensionless)
Ss)outer surface of the adsorbent per unit volume of
particle-free slurry (cm-1)
∆S0)entropy of adsorption (kJ K-1.mol-1)
ZPC)zero point charge
b, b1, b2)Langmuir constants at 30, 40, and 50 °C (L/mol)
k)constant obtained by multiplying the Langmuir con-
stants Q° and b (L g-1)
m)mass of adsorbent per unit volume of particle free
adsorbate solution (g L-1)
n)Freundlich constant of solute (dimensionless)
qe)amount adsorbed at equilibrium (mg g-1)
q)amount adsorbed at time t (mg g-1)
t)predecided time interval at which adsorbent is separated
from the adsorbate solution (h)
βL)mass transfer coefficient (cm s-1)
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Received for review April 14, 2003
Revised manuscript received July 28, 2003
Accepted August 11, 2003
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