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

low cost adsorbents for the treatment of wastewater.
Environmental pollution by toxic metals is well Contributions in this regard have been made by many
recognized and can be detrimental to human health and researchers who have utilized a number of materials
the environment. Metals can be distinguished from such as fly ash,7 peat,8 bentonite,9 lignin,10 charcoal,11
other toxic pollutants, because these are nonbiodegrad- straw,12 blast furnace slag,13,14 biomass,15,16 sludges,17-19
able, may undergo transformations, and can have a red mud,20,21 and so forth.
large environmental, public health, and economic im-
pact.1 This has led to more stringent legislation and has The sugar industry is one of the most important agro-
prompted industry to seek more effective methods of based industries in India. Bagasse fly ash, a waste
pollution control as the permissible limits are reduced.2 material of sugar industries, causes a disposal problem.
Zinc is a toxic element that can be found in natural Currently this fly ash is being used as filler in building
water, as well as in various industrial effluents.3 The materials, but to date no other proper application of this
average human body contains about 2 g of zinc, which waste has been found. Recently, in our laboratory,
is essential for the normal activity of DNA polymeriza- bagasse fly ash has been converted into an effective
tion and for protein synthesis. However, the inhalation adsorbent and used for the removal of toxic sub-
of zinc fumes may produce “Zinc Fever”, which is stances.22,23 In continuation, the aim of the present
characterized by chills and fevers. Edema of the lungs research is to utilize the bagasse fly ash for the removal
from fumes of zinc chloride (ZnCl2 smoke) is sometimes of zinc from aqueous solutions and the results are
fatal. Soluble and astringent acid salts, such as ZnSO4 discussed in this communication.
in large doses (about 10 g), have caused internal organ
damage and death. Zinc has a secondary drinking water Materials and Methods
standard of 5.0 mg L-1 principally because of its bitter
metallic taste.3 All the reagents used were of A. R. grade. Stock
Among the methods examined for zinc removal from solution of zinc (1 × 10-2 M) was prepared by dissolving
water, adsorption on activated carbon has been shown Zn(NO3)2 in doubly distilled water.
to be very efficient.4,5 But the use of commercially Equipment. Atomic absorption spectra were re-
available activated carbon is limited, especially in corded using an atomic absorption/emission spectropho-
developing countries, because of its high cost and tometer (Perkin-Elmer model 3100) using light source
difficulties in its regeneration.6 Accordingly, current Hollow Cathode; lamp current, 15.00 mA; wavelength,
research is focused on the development of inexpensive 213.9 nm; slit width, 0.7 nm; sensitivity, 1.0 mg L-1.
materials having high affinity, selectivity, and capacity X-ray measurements were done by a Phillips X-ray
toward metals. The potential of various agricultural and diffractometer employing nickel filtered Cu KR radia-
industrial waste materials has received the most atten- tions. The surface area of the sample was measured by
tion for this purpose, which results in 2-fold benefits, a surface area analyzer (model QS-7; Quantasorb sur-
face area analyzer). pH measurements were made using
* To whom correspondence should be addressed. Tel.: 0091- a pH meter (model CT No. CL 46; Toshniwal, India).
1332-285801. Fax: 0091-1332-273560. E-mail: vinodfcy@ Scanning electron microscopy (SEM) was performed
iitr.ernet.in. using a Phillips SEM 501 electron microscope. The
10.1021/ie0303146 CCC: $25.00 © 2003 American Chemical Society
Published on Web 11/12/2003
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 fixed concentration over a pH range of 1.0-6.0. pH
by using a quantitative method of chemical analysis.24 adjustment was made by dilute NaOH and dilute HNO3.
The density of the adsorbent was determined by use of The pH was monitored at the beginning and at the end
specific gravity bottles. of the run and no noticeable change in pH was observed.
Material Development. Bagasse fly ash, a solid Kinetic Studies. The batch technique was selected
waste, was obtained from a sugar industry establish- because of its simplicity and reliability. A number of 50-
ment at Bijnor (U. P.) India. This material in its mL stoppered glass tubes containing 10 mL of solution
untreated form showed poor adsorption properties. of metal ion of known concentration (1.84 × 10-3 M)
Therefore, this material was first treated with hydrogen were placed in a thermostat cum shaking assembly. At
peroxide 30% w/v (100 volume) at 60 °C for 24 h, till the desired temperature, 0.1 g of bagasse fly ash was
the evolution of bubbles stopped. The pretreatment with added into each tube and the solutions were agitated
hydrogen peroxide perhaps removes heterogeneously intermittently. At predecided intervals of time (30 min
distributed organic matter from the bagasse fly ash. for the first two tubes and 60 min for all subsequent
Preliminary adsorption studies revealed that treating tubes) the test solutions in the specified tubes were
the waste material with hydrogen peroxide (30% w/v) centrifuged at 4000 rpm for 15 min and separated from
imparts maximum adsorption characteristics, and, there- the adsorbent material. The supernatant was analyzed
fore, all investigations were carried out on samples after for aqueous metal. The kinetic studies were also per-
providing this treatment. The resulting product was formed at different adsorbate (1.22 × 10-3 to 3.06 × 10-3
then washed with distilled water, dried at 100 °C for M) and adsorbent (5 g L-1 to 20 g L-1) concentrations.
24 h, and sieved to desired particle sizes such as 100-
150, 150-200, and 200-250 BSS mesh. The finished Results and Discussion
product exhibited the best adsorption capacity and high
surface area. The product obtained at temperatures Characterization of the Adsorbent Material. The
higher than 100 °C exhibits poor adsorption capacity, adsorbent developed from bagasse fly ash was found to
probably due to collapse of surface functional groups on be of “L” type in nature as classified earlier,23 i.e., it
adsorbent. Finally, the product was stored in vacuum lowers the pH when kept in deionized water. It is quite
desiccators until used. stable in water, salt solutions, acid, and bases. Chemical
Adsorption Studies. Adsorption studies were car- composition of the bagasse fly ash as determined by
ried out in a routine manner by batch technique.23 chemical analysis24 is SiO2, 61.44; Al2O3, 14.50; CaO,
Isotherms were run with zinc solutions of varying 2.82; Fe2O3, 4.86; MgO, 0.71, and loss on ignition, 17.12
concentration (3.06 × 10-4 to 3.06 × 10-3 M), main- wt %. It is necessary to mention that no leaching
tained at the desired pH and temperature. Stoppered measurements were done in this work to estimate
glass tubes containing metal ion solutions (10 mL) and contamination of solution by solubilized oxides from
known amounts of bagasse fly ash (0.1 g; particle size bagasse fly ash. Leaching studies are out of the scope
150-200 mesh) were stirred intermittently for a maxi- of the present paper and are now a part of our ongoing
mum period of 24 h. The contact time and other and future research. The X-ray diffraction pattern
conditions were selected on the basis of preliminary (Figure 1) of the product provided d spacing values
studies that showed that the equilibrium was attained which reflect the presence of different minerals, such
in 6-8 h, and beyond this time the adsorption of zinc as goethite, mullite, hematite, kaolinite, γ-alumina, and
ions on the adsorbent material remained almost con- R-quartz, indicating high chemical stability of the ba-
stant. Equilibration for longer times, that is between 8 gasse fly ash.25 Bands observed at 1172, 1157, and 680
and 24 h, gave practically the same uptake. After this cm-1 in the IR spectrum (figure not shown) of bagasse
period the solutions were separated from the adsorbent fly ash were attributed to Si-O stretching vibrations,
(centrifuged at 4000 rpm for 15 min) and immediately a characteristic of quartz.26 The adsorption bands at
analyzed to determine the uptake of zinc by the adsor- 3696 and 3670 cm-1 indicated the presence of kaolinite.
bent. Adsorption studies were carried out at 30, 40, and A very weak band at 358 cm-1 was due to the presence
50 °C to establish the effect of temperature. The effect of hematite. A strong band at 470 cm-1 suggested the
of pH was determined by studying the adsorption at a presence of calcium silicate. The surface area of the
 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
Figure 2. SEM photographs of bagasse fly ash at different conditions the uptake of zinc ions would be quite low
magnifications: (a) 1 × 5000; (b) 1 × 2500; and (c) 1 × 121. due to electrostatic repulsion. With increasing pH, i.e.,
beyond ZPC, the negative charge density on the surface
adsorbent as calculated by BET method was found to of adsorbent increases, thereby resulting in a sudden
be 470 m2 g-1. The surface area was also worked out enhancement in metal adsorption. A similar behavior
theoretically, by methylene blue dye adsorption, taking has been reported by Sen and De29 for Hg (II) and Gupta
methylene blue dye molecule area as 197 Å2 and found et al.23 for lead adsorption on fly ash and bagasse fly
to be 440 m2 g-1. This value is slightly less than that ash, respectively.
determined by N2 gas adsorption, and indicates that All the adsorption studies were carried out at a pH
of 4.0. The adsorption isotherms (Figure 4) are regular,
some pores of bagasse fly ash are not accessible to
positive, and concave to the concentration axis. The
methylene blue. Scanning electron microscopic (SEM) uptake is almost 100% at low concentrations (e 6.12 ×
photographs of bagasse fly ash (Figure 2 (a-c)) clearly 10-4 M), and the adsorption decreases with concentra-
reveal the surface texture and porosity of the sample. tion at 1.84 × 10-3 M and ultimately becomes constant.
The material was so porous that it could be crushed This indicates the efficiency of the adsorbent for the
easily by hand. The point of zero charge pHzpc (pH of removal of zinc from wastewater in a wide range of
the suspension at which surface charge density σ ) zero) concentrations. Further, it is observed that the adsorp-
and cation exchange capacity were determined by using tion decreased with increase in temperature indicating
potentiometric titration method.27,28 The characteristics 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 thermodynamic parameters
n KF × 105 Q° × 104(mol g-1) b× 10-2(L mol-1) -∆G° (kJ mol-1) -∆H° (kJ mol-1) -∆S° (J mol-1 K-1)
temp. ((0.02) ((0.005) ((0.01) ((0.02) ((0.05) ((0.05) mean ((0.1) mean
30 °C 0.36 3.10 2.02 9.45 17.27 76.83 197.95
40 °C 0.44 1.23 1.97 2.19 14.03
50 °C 0.46 0.132 1.85 1.41 13.30

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 Figure 5. Effect of adsorbate concentration on the rate of uptake
Gupta et al.13 for red mud (12.59 mg g-1) and blast of Zn2+ on bagasse fly ash.
furnace slag (37.98 mg g-1), respectively.
The dimensionless factor RL as calculated from RL ) bate to the external surface of the adsorbent (film
1/1+bCo was found to be 0.37. This indicates a highly diffusion); (b) transport of the adsorbate within the
favorable adsorption (RL , 1).30 The thermodynamic pores of the adsorbent except for a small amount of
parameters obtained for this system using equations as adsorption that occurs on the external surface (particle
described earlier14 are also given in Table 1. The diffusion); and (c) adsorption of the adsorbate on the
negative free energy values indicate the feasibility of exterior surface of the adsorbent.
the process and its spontaneous nature without any It is generally accepted that process (a) is very rapid
induction period. The negative value of enthalpy change and does not represent the rate-determining step in the
(∆H°) for the processes further confirms the exothermic uptake of adsorbate.23 For the remaining two steps in
nature of the process. Negative entropy of adsorption the overall transport, three distinct cases may occur:
(∆S°) reflects the affinity of the adsorbent material case I, external transport > internal transport; case II,
toward zinc. external transport < internal transport; and case III,
Kinetic Studies. Preliminary studies on the rate of external transport ≈ internal transport.
removal of Zn2+ by bagasse fly ash (at optimum pH and In cases I and II, the transport of adsorbate to the
adsorbent concentration) indicated the process to be adsorbent is quite rapid and is governed by film diffu-
quite rapid. Nearly 50 to 60% of the adsorption capacity sion, whereas in case III, the transport of ions to the
was attained within the first hour of contact. The initial adsorbent surface does not occur at a significant rate,
rapid adsorption gives way to a very slow approach to thereby leading to the formation of a liquid film with a
equilibrium, and saturation is reached in 6-8 h (Figure concentration gradient surrounding the sorbent par-
5). It is also evident from Figure 5 that at low concen- ticles.
tration (1.22 × 10-3 M), 96.72% zinc is removed, Usually, external transport is the rate-limiting step
whereas 92.93% removal was ascertained with the in systems which have poor mixing, dilute concentration
concentration of 1.84 × 10-3 M using 10 g L-1 of the of adsorbate, small particle size, etc. In contrast, the
adsorbent dose in 6-8 h. At higher concentration (3.06 intraparticle transport step (case III) governs the overall
× 10-3 M) nearly 62.75% of zinc is removed from the transfer for those systems having high concentration of
solution under identical conditions of adsorbent dose adsorbate, good mixing, larger particle size, etc. Hence
and contact time. It was also found that at fixed the low removal of zinc at higher concentration at fixed
concentration the rate of removal of zinc increases with adsorbent concentration reflects the intraparticle dif-
an increase in the amount of bagasse fly ash. There was fusion, whereas high removal of zinc at low concentra-
a significant increase in the adsorption when the tion might be due to the rapid external transport
adsorbent amount was increased from 5 g L-1 to 10 g mechanism to be the rate controlling step in the overall
L-1. Any additional amount of bagasse fly ash did not removal of zinc at varying concentration range.
cause any significant change. Thus, 10 g L-1 of bagasse Adsorption Dynamics. Lagergren’s rate equation
fly ash has been used in all subsequent studies. as cited by Ho and Mckay31 was employed for studying
The above observations can be explained on the basis the rate constant for the systems. The plot between log-
of the following three consecutive steps, which may be (qe - q) and t was found to be linear, which shows the
involved in the adsorption of an organic/inorganic spe- first-order nature of the processes. The value of the rate
cies by a porous adsorbent: (a) transport of the adsor- constant, Kad, for the system was 8.73 × 10-3 min-1.
 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)
Figure 6. McKay plots of Zn2+ on bagasse fly ash. KF)Freundlich constant of solute (mol g-1)
Kad)Rate constant (min-1)
Mckay and co-workers32 model (eq 1) has been em- Q∞)amount of adsorbate adsorbed per gram of adsorbent
ployed for the determination of the surface mass- (mol g-1) at equilibrium
transfer coefficient βL. Qt)amount of adsorbate adsorbed per gram of adsorbent
(mol g-1) at time t

ln [
Ct
-
1
Co 1 + mk ]
) ln
mk
1 + mk
-
1 + mk
mk
βL Ss t (1)
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)
The straight line plot between ln [Ct/Co - 1/(1 + mk)] ∆S0)entropy of adsorption (kJ K-1.mol-1)
and t proved the validity of the above model in the ZPC)zero point charge
present study. The value of βL for the system as b, b1, b2)Langmuir constants at 30, 40, and 50 °C (L/mol)
determined from the plot was 2.41 × 10-7 cm s-1.
k)constant obtained by multiplying the Langmuir con-
To know the rate controlling step of the process, stants Q° and b (L g-1)
McKay plots (Figure 6) at different adsorbate concen- m)mass of adsorbent per unit volume of particle free
trations have been drawn. The plots between log(1 -F) adsorbate solution (g L-1)
and t, where F is the fractional attainment of equilib- n)Freundlich constant of solute (dimensionless)
rium at time t and is obtained by F ) Qt/Q∞ where Qt is qe)amount adsorbed at equilibrium (mg g-1)
amount of uptake at time t and Q∞ is maximum q)amount adsorbed at time t (mg g-1)
equilibrium uptake for Zn2+ at lower concentrations (e t)predecided time interval at which adsorbent is separated
1.84 × 10-3 M) were found to be linear indicating a from the adsorbate solution (h)
purely film diffusion process. However, nonlinear plot βL)mass transfer coefficient (cm s-1)
at g 3.06 × 10-3 M concentration supports the assump-
tion that particle diffusion becomes the rate-limiting
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