Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

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Colloids and Surfaces B: Biointerfaces

journal homepage: www.elsevier.com/locate/colsurfb

Characterization of banana peel by scanning electron microscopy and

FT-IR spectroscopy and its use for cadmium removal
Jamil R. Memon a, , Saima Q. Memon b , M.I. Bhanger a , G. Zuhra Memon c , A. El-Turki d , Geoffrey C. Allen d
a

National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, Sindh 76080, Pakistan
Hi Tech Central Resource Laboratories, Pakistan
c
M.A. Kazi, Institute of Chemistry, Pakistan
d
Interface Analysis Center, University of Bristol, Bristol, UK
b

a r t i c l e

i n f o

Article history:
Received 3 April 2008
Received in revised form 1 July 2008
Accepted 2 July 2008
Available online 10 July 2008
Keywords:
Sorption
Cadmium
Banana peel
SEMEDX
FT-IR
Wastewater

a b s t r a c t
This study describes the use of banana peel, a commonly produced fruit waste, for the removal of Cd(II)
from environmental and industrial wastewater. The banana peel was characterized by FT-IR and scanning
electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis. The parameters pH, contact time, initial metal ion concentration and temperature were investigated and found to be rapid (97%
within 10 min). The Langmuir adsorption isotherm was used to describe partitioning behavior for the
system at room temperature. The value of QL was found to be (35.52 mg g1 ) higher than the previously
reported materials. The binding of metal ions was found to be pH-dependent with the optimal sorption
occurring at pH 8. The retained species were eluted with 5 mL of 5 103 M HNO3 with the detection
limit of 1.7 103 mg L1 . Kinetics of sorption followed the pseudo-rst-order rate equation with the rate
constant k, equal to 0.13 0.01 min1 . Thermodynamic parameters such as Gibbs free energy at 303 K
(7.41 0.13 kJ mol1 ) and enthalpy (40.56 2.34 kJ mol1 ) indicated the spontaneous and endothermic
nature of the sorption process. The developed method was utilized for the removal of Cd(II) ions from
environmental and industrial wastewater samples using ame atomic absorption spectrophotometer
(FAAS).
2008 Elsevier B.V. All rights reserved.

1. Introduction
The increase in environmental pollution caused by toxic metals is of great concern because of their carcinogenic properties [1],
non-biodegradability and bio-accumulation. Ingestion of cadmium
causes various types of acute and chronic metabolic disorders such
as itai-itai disease, renal damage, emphysema, hypertension and
testicular atrophy [2]. The drinking water guideline recommended
by the World Health Organization (WHO) and American Water
Works Association (AWWA) is 0.005 mg Cd2+ L1 [3]. Cadmium may
be found in wastewater discharges from the electroplating industry,
the manufacture of nickelcadmium batteries, fertilizers, pesticides, pigments and dyes and textile operations [4,5]. Because of its
toxic effects, it is important to develop an effective, fast, precise and
accurate method for the removal of the cadmium in environmental
water samples.

During the past two decades, extensive research has been carried out to identify new adsorbents for cadmium removal which
are both effective and economical. The following materials have
been assessed for cadmium uptake including wood and bark [6],
kraft lignin [7], rice husk [8], marine algal biomass [9], tea industry waste [10], olive pomace [11], activated sludge Nocardia amarae
[12], sugar beet pulp [13], seafood processing waste sludge [14],
bone char [15], pine bark [16] and red mud [17].
In the present work, we describe the use of an effective and
inexpensive banana waste material for the removal of cadmium
from water. The cadmium enrichment capability of the adsorbent
is ascertained by applying the method to a commercial wastewater
treatment plant.

2. Materials and methods

2.1. Materials

Corresponding author. Tel.: +92 22 2771379; fax: +92 22 2771560.

E-mail address: memon.jamil@gmail.com (J.R. Memon).
0927-7765/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.colsurfb.2008.07.001

All chemicals were supplied by E. Merck, Darmstadt, Germany

and were of analytical grade. A stock standard solution of Cd(II)
was prepared by dissolving the appropriate amount of its nitrate in

J.R. Memon et al. / Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

Table 1
Composition of banana peel

261

carbon-coated using an Edwards Scancoat Six machine prior to

SEM-EDX analysis to reduce the charging effect.

Proximate analysis of BP

Percentage (%)

Dry matter
Moisture
Fat
Crude Fiber
Crude Protein
Ash

90.36
9.64
5.02
11.04
10.14
18.98

deionized water (conductivity 0.5 mS cm1 ), acidied with a small

amount of nitric acid. Buffer solutions of pH 13, 46 and 79 were
prepared by mixing appropriate ratios of 0.1 M HCl and KCl, 0.5 M
acetic acid and sodium acetate and 0.5 M ammonia and NH4 Cl solutions, respectively.

2.2.4. Equilibrium metal adsorption experiments

The metal sorption behavior of banana peel was investigated
using batch equilibrium experiments. 0.1 g of banana peel was
equilibrated with 10 mL of Cd(II) solution (1.78 105 M) maintained at constant pH 8 at 30 1 C and shaken on an electrical
shaker (water bath) at 80 rpm for a designated time (060 min).
The mixture was ltered and adsorbed metal ions were desorbed
by shaking with 5 mL of 5 103 M HNO3 solution and analyzed by
ame atomic absorption spectrophotometer at 228.8 nm and a slit
width of 0.5 nm using an airacetylene ame. Experiments were
conducted in triplicate and the results are the average of triplicate
measurements. Precision in all cases is close to 1%.

2.2. Methods
2.2.1. Preparation of adsorbent
Slices of banana peel were cut into small pieces, dried, crushed
and passed through 120 mesh sieve (125 m). The banana peel was
then washed thoroughly with deionized water to remove physically adsorbed contamination and dried in an air oven at 100 C for
a period of 8 h. The surface area of the dried material was measured using the BET method [18] and was found to be 13 m2 g1 .
The analysis of banana peel for the determination of protein, ber,
dry matter and ash was carried out as per procedure reported in
the literature [19]. The results are presented in Table 1.
2.2.2. Esterication of banana peel
Modication of the carboxylic groups on the surface of the
banana peel using acidic methanol was performed as follows: 9 g
of dry-washed banana peel was suspended in 633 mL of 99.9%
methanol to which 5.4 mL of concentrated HCl was added (0.1 M
HCl nal concentration). The solution was continuously stirred and
heated at 60 C for 48 h. The banana peel was then washed three
times with cold deionized water in order to quench the esterication reaction [20].
2.2.3. Chemical analysis
A Varian AA-10 atomic absorption spectrophotometer was used
to determine cadmium concentrations in the solution. The pH measurements were made with a digital (InoLab pH level I) pH meter
equipped with a calibrated combined pH glass electrode. A Gallenkamp thermostated automatic shaker model BKS 305-010, UK
was used for the batch experiments.
The dried banana peel was analyzed by FT-IR using a ZnSe SBATR accessory. The infrared spectra were acquired using a Thermo
Nicolet Avatar 330 FT-IR spectrometer equipped with a deuterated
triglycine sulfate (DTGS) detector and KBr optics and controlled by
OMNIC software (Thermo Nicolet Analytical Instruments, Madison,
WI) with spectra collected by co-addition of 32 scans at a resolution of 8 cm1 . The spectrum of sample was ratioed against a fresh
background spectrum recorded from the bare ATR crystal cleaned
with propanol to remove any residues and the residual solvent
evaporated in a stream of nitrogen gas.
Scanning electron microscopy with energy dispersive X-ray
analysis (SEMEDX) is a near surface technique. The electrons produced by an electron gun strike the specimen being irradiated,
and the X-ray radiation from the specimen is then collected and
analyzed by means of EDX. The morphologies of the specimen surface areas were examined by a Hitachi S2300 Scanning Electron
Microscope with 25 kV of accelerating voltage. The microscope was
equipped with EDX analyzers, which enabled determination of the
elemental composition of specimen surfaces. The samples were

3. Results and discussion

3.1. FT-IR spectroscopy of banana peel
FT-IR spectra of banana peel were obtained in order to understand the nature of the functional groups present in banana peel.
FT-IR spectra (Fig. 1a) displayed a number of peaks, indicating
the complex nature of the adsorbent. Bands appearing at 3313.4,
2920.3, 2850.6, 1734, 1613.6, 1317.4, 1035.2 and 884.6 cm1 in
Fig. 1a were assigned to OH stretching, CH stretching of alkane,
CH and C O stretching of carboxylic acid or ester, COO anion
stretching, OH bending, CO stretching of ester or ether and NH
deformation of amines respectively [21]. Out of these, carboxylic
acid and hydroxyl groups played a major role in the removal of
Cd(II) ions. As expected, a signicant reduction in the intensity of
OH, CH and especially COOH peaks at 3336, 2906 and 1623 cm1
respectively were recorded in the spectra of esteried banana peel
(Fig. 1b).

Fig. 1. FT-IR spectra of (a) banana peel and (b) esteried banana peel.

262

J.R. Memon et al. / Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

3.3. Effect of pH

Fig. 2. Scanning electron microscopic (SEM) analysis of banana peel.

3.2. Scanning electron microscopy and energy dispersive X-ray

analysis
The surface morphology of banana peel was studied with the
use of SEM. A microporous structure (Fig. 2) was observed at a resolution of 1500 while the image of banana peel was taken with a
particle size of 10 m.
In order to know the composition of banana peel, elemental
analysis was done with the use of EDX analysis. The EDX analysis
of unadsorbed banana peel, shown in Fig. 3a, showed the presence
of various elements along with a high amount of potassium, while
EDX spectra of cadmium-adsorbed banana peel, shown in Fig. 3b,
showed an additional peak conrming the sorption of cadmium
onto the surface of the banana peel.

pH is one of the most important parameters while assessing the

sorption capacity of an adsorbent for metal ions sequestering from
aqueous solution. The pH of the system controls the sorption capacity due to its inuence on the surface properties of the adsorbent
and ionic forms of the cadmium in solution. Sorption experiments
were carried out in the pH range of 19 keeping all other parameters constant. The uptake of metal ions onto dried banana peel as
a function of pH is shown in Fig. 4. At pH < 3, low uptake and at
pH > 3, high uptake of metal ions was recorded as reported in Refs.
[7,9]. The sorption was increased slowly up to pH 8 and attained
a maximum value of 95%; at pH greater than 8, percent sorption
declined. Therefore, for further experiment pH 8 was employed.
Up to pH 8 the main species of Cd(II) is Cd2+ (100%) [22] consequently, precipitation is not the retention mechanism on banana
peels.
The dependence of metal uptake on pH is related to the surface functional groups in banana peel. The nal pH increased with
increasing initial pH, in acidic medium; the reverse was observed
in basic medium. Thus, neutralization and sorption processes were
occurring simultaneously. The H+ ions may also compete with
metal ions for binding with the surface groups of banana peel.
At lower pH, the higher concentration of the hydrogen ions effectively leads to fewer surface functional groups being available for
the binding of metal ions. Increased pH (i.e. fewer H+ ions) results
in more functional groups being available for metal ion binding and
hence sorption was enhanced.
The metal ion binding could be attributed to several mechanisms such as ion-exchange, complexation, electrostatic attraction
and precipitation. For banana peel, ion-exchange has been considered as a main mechanism responsible for metal sequestering [9].
The typical dependence of metal uptake on pH suggests that the
weak acidic carboxylic groups RCOO (apparent pKa in the range
3.55.0) of banana peel are the probable sorption sites. Hydroxyl
groups are also present in all polysaccharides but are less abundant.
These become negatively charged at high pH, thereby contributing
to metal sorption [9].
3.4. Sorption of Cd(II) on esteried banana peel
In an attempt to identify the nature of the functional groups
responsible for cadmium sorption, sorption experiments were
carried out on esteried banana peel. Results from the sorption
experiments showed that the amount of Cd(II) bound was reduced
from 99% to 0%. Reduction in percent sorption on esteried banana
peel suggested the involvement of COOH groups for the selective
sorption of Cd(II).

Fig. 3. Energy dispersive X-ray (EDX) analysis of (a) unadsorbed and (b) Cd adsorbed
banana peel.

Fig. 4. Sorption of Cd(II) ions onto banana peel as a function of pH.

J.R. Memon et al. / Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

263

Table 2
Reagent used for the elution of Cd(II) ions
Reagenta

Concentration (M)

%Recovery

NH3
NH3
NaOH
NaOH
HCl
HCl
H2 SO4
H2 SO4
HNO3
HNO3

0.01
0.1
0.01
0.1
0.005
0.01
0.005
0.01
0.001
0.005

7
25
6
100
38
100
75
100
25
100

Volume of each reagent used = 5 mL.

Fig. 5. MorrisWeber plot for the sorption of Cd(II) ions onto banana peel.

3.5. Recovery of cadmium

Desorption of cadmium from banana peel surface was studied
using 5 mL of different concentrations of HNO3 , H2 SO4 , HCl, NaOH
and NH3 . For this purpose, 0.1 g of Cd(II) adsorbed banana peel was
agitated at 150 rpm for 30 min with 5 mL of the desired concentration of each reagent mentioned. Percent recoveries are given in
Table 2. Elution was found to be quantitative (100%) with 5 mL of
5 103 M HNO3 .
3.6. Optimum shaking speed
Sorption of metal ions as a function of shaking speed was studied
in the range of 20140 rpm. It was found that sorption increases
with increasing shaking speed and attains a maximum sorption at
80 rpm. Therefore, for further studies 80 rpm shaking speed was
employed.
3.7. Optimum shaking time
The effect of shaking time on adsorption of Cd(II) ions onto
banana peel was studied over a range of 060 min, at pH 8 and
shaking speed 80 rpm, using 10 mL of 1.78 105 M Cd(II) ions solution and 0.1 g of adsorbent. For the equilibrium study, the pH of the
metal ion solution was maintained during the sorption experiment.
Sorption increased with increase of shaking time. Equilibrium was
established within 10 min and there was only a slight increase in
percent sorption up to 30 min but in order to avoid sorption error,
all further experiments were carried out for 30 min.
3.8. Limit of preconcentration and preconcentration factor

after 30 min of contact time. The recorded kinetic data were tted to different equations namely, MorrisWeber, Lagergren and
Reichenberg. The adsorbed
concentration at time t, qt (mol g1 )

was plotted against t to test the MorrisWeber equation [23] in

the following form:

qt = Rd t
(1)
where Rd is the rate constant of intraparticle transport. Up to 30 min
Eq. (1) held well with a regression coefcient of 0.99 but deviated
as the agitation time increased. From the slope of the plot in the
initial stage (Fig. 5) the value of Rd , the rate constant for intraparticle transport, was estimated to be 0.64 0.02 mol g1 min1/2 for
Cd(II). The Lagergren equation [24]:
log(qe qt ) = log qe

kt
2.303

was tested by plotting log(qe qt ) versus time t (Fig. 6), where qe is

the adsorbed concentration of cadmium on banana peel (mol g1 )
at equilibrium. The overall value of rate constant (k) was estimated
to be 0.13 0.01 min1 from the slope of the plot with a regression
coefcient of 0.9898. The effectiveness of the diffusion of exchanging ions within the adsorbent particles of radius r and control of
lm diffusion in sorption may be deduced from the linear t of the
data to the Reichenberg equation [25]:
Q =1

6eBt
2

(3)

where Q = qt /qm , Bt = 2 Di /r2 and qt and qm are adsorbed concentration at time t and the maximum sorption capacity of the
adsorbent and Di is the effective diffusion coefcient of ions
exchanging inside the adsorbent particle. The value of Bt which

To explore the possibility of enriching low concentrations of analyte from large volumes, the maximum applicable sample volume
must be determined. For this purpose different volumes of sample solution, each containing 10 g of Cd(II) ions were equilibrated
with banana peel under the optimum conditions (0.1 g banana peel
and shaking speed 80 rpm) and recoveries were calculated after
desorbing the metal ion with 5 mL of 5 103 M HNO3 . Recovery was found to be quantitative using a 6000 mL sample volume.
As the adsorbed Cd(II) ions can be eluted with 5 mL of HNO3 , so
the enrichment factor achieved was 1200 (6000/5) with the detection limit of 1.7 103 mg L1 (10 g/6000 mL = 0.0017 g mL1 or
1.7 103 mg L1 ).
3.9. Kinetics of sorption
Kinetic studies were carried out under optimized conditions
from 0 to 30 min. The sorption was very fast as reported earlier
[13]. The removal was 97% with very little increase in sorption

(2)

Fig. 6. Lagergren plot for the sorption of Cd(II) ions onto banana peel.

264

J.R. Memon et al. / Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

Table 3
Comparison of sorption capacities of Cd(II) with previously reported adsorbents
Adsorbent

Adsorption capacity (mg g1 )

Reference

Oak wood char

Pine bark char
Oak bark char
Carbon F-400
Tea industry waste
Olive pomace
Activated sludge (Nocardia amarae)
Sugar beet pulp
Seafood processing waste sludge
Pine bark
Red mud
Banana peel

0.37
0.34
5.40
8.00
11.3
6.97
34.7
24.4
15.74
14.16
10.57
35.52

[6]

[10]
[11]
[12]
[13]
[14]
[16]
[17]
This work

Fig. 7. Reichenberg plot for the sorption of Cd(II) ions onto banana peel.

is a mathematical function of Q can be evaluated for each value of

Q, using the following equation:
Bt = 0.4977 ln(1 Q )

Table 4
Determination and removal of Cd(II) from environmental and industrial wastewater
samples
Sample

(4)

The plot of Bt versus time (Fig. 7) was linear from 0 to 15 min with a
regression coefcient of 0.9898 but the regression line plot did not
pass through origin indicating the formation of a thin lm of Cd(II)
on the surface.

National Electroplating Industry, Karachi

Tap Water, Hala (new)
Tap Water, Jamshoro
Phulleli Canal, Hyderabad

3.10. Thermodynamics of adsorption

Different thermodynamic parameters such as H, S and
G were also calculated from the data obtained by temperature variations (293313 K) using equations reported in the
literature [26,27]. The values of H = 40.56 2.34 kJ mol1 and
S = 0.11 0.01 J mol1 K1 were estimated with a regression
coefcient of 0.9899. The positive value of H and negative value
of G indicated the endothermic and spontaneous nature of reaction respectively. The Gibbs free energy was estimated to be
G303 K = 7.41 0.13 kJ mol1 .
3.11. Sorption isotherms
The sorption of Cd(II) ions was also investigated as a function of
concentration at room temperature in the range of 0.1500 mg L1
using 0.1 g of adsorbent and 10 mL of adsorbate solution, and 30 min
shaking time at a shaking speed of 80 rpm. The uptake of metal ion
increased with increasing concentration up to 50 mg L1 , where
95% adsorption of Cd(II) was recorded. At higher concentration
a decreasing trend was observed; the decrease was slight up to
100 mg L1 and 7% uptake of Cd(II) was observed at 500 mg L1 .
These results reected the efciency of the adsorbent for the
removal of cadmium ions from aqueous solution in the concentration range of 0.1100 mg L1 . The effect of the tested metal
ion concentration on banana peel was analyzed in terms of the
Freundlich, Langmuir and DubininRadushkevich (DR) isotherms
[28] but the sorption data followed only the Langmuir isotherm.
Therefore, the Langmuir isotherm was used to evaluate the sorption
capacity of banana peel for Cd(II) ions.
Ce
1
Ce
=
+
Cads
Q
Qb

(5)

where Cads is the amount of metal ions adsorbed per unit mass of
adsorbent and Ce is the amount of metal ions in the liquid phase
at equilibrium. Q and b are the Langmuir constants. The values
of Q = 316 7 mol g1 and b = 2.3 1.4 L g1 were calculated from
the slope and intercept of the linear plot at room temperature.
The sorption capacity value obtained from the Langmuir isotherm
was found to be higher than other previously reported methods

Cd(II) (g mL1 )
Added

Found

Removal (%)

0.0
0.0
2.0
0.0
2.0
0.0
2.0
0.0
2.0

2.2
0.2
2.18
0.1
2.1
0.04
2.02
0.01
2.00

100

99.09

100

99.02

99.50

as shown in Table 3. An essential characteristic of the Langmuir

isotherm can be explained in terms of a dimensionless constant
separation factor (RL ), calculated using the equation RL = 1/(1 + bCi )
where, Ci is the initial concentration of metal ions. RL describes the
type of Langmuir isotherm [29] to be irreversible (RL = 0), favorable
(0 < RL > 1), linear (RL = 1) or unfavorable. The values of RL calculated
were between 0.009 and 0.97 indicating highly favorable sorption
of Cd(II) ions onto banana peel.
3.12. Reusability of banana peel
In order to check the reusability of adsorbent, banana peel was
subjected to several loading and elution experiments. The capacity
of the adsorbent was found to be practically constant (variation
of 13%) after 10 times of repeated use; thus multiple use of the
adsorbent was seen to be feasible.
3.13. Analytical applications
The analytical applicability of banana peel was tested for environmental and industrial wastewater samples obtained from Sindh,
Pakistan. A 50-mL aliquot of water sample was ltered and adjusted
to pH 8. Another 50 mL aliquot of water sample was spiked with
Cd(II) at pH 8. The solutions were then agitated with 0.1 g of banana
peel at the shaking speed of 80 rpm for 30 min. The metal ions
were then eluted with 5 mL of 5 103 M HNO3 and determined by
ame atomic absorption spectrophotometer. The results are given
in Table 4. The R.S.D. was always within 2% which clearly shows
the efciency of banana peel for the removal of Cd(II) ions from
industrial and environmental wastewater samples.
4. Conclusion
The present work explores a new cheaper, economical and selective adsorbent as an alternative to costly adsorbents for the removal

J.R. Memon et al. / Colloids and Surfaces B: Biointerfaces 66 (2008) 260265

of Cd(II) ions. The main advantages include its low cost, rapid attainment of phase equilibration and high sorption capacity values. FT-IR
analysis of banana peel showed the presence of various functional
groups indicating the complex nature of the banana peel. Scanning electron microscopic analysis demonstrated the microporous
structure of the material while energy dispersive X-ray analysis
conrmed the sorption of Cd(II) on banana peel. The kinetics of
sorption of cadmium follows a pseudo rst order rate equation.
Sorption of Cd(II) onto banana peel follows only the Langmuir
model. Banana peel can effectively be used to remove Cd(II) ions
from environmental and industrial wastewater samples.

[10]
[11]
[12]
[13]

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